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(11) | EP 2 712 936 B1 |
| (12) | EUROPEAN PATENT SPECIFICATION |
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SUGAR PRODUCTS AND FABRICATION METHOD THEREOF ZUCKERPRODUKTE UND HERSTELLUNGSVERFAHREN DAFÜR PRODUITS DE SUCRE ET SON PROCÉDÉ DE FABRICATION |
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| Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention). |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This Application claims priority of China Patent Application No. 2013104350048, filed on Sep 23, 2013. This application claims the benefit of U.S. Application No. 13/973,072, filed on Aug 22, 2013, which claims the benefit of provisional Application No. 61/707,576, filed on Sep 28, 2012, the entireties of which are incorporated by reference herein.
TECHNICAL FIELD
BACKGROUND
[0003] The world is facing problems such as the gradual extraction and depletion of petroleum reserves, and changes to the earth's atmosphere due to the greenhouse effect. In order to ensure the sustainability of human life, it has become a world trend to gradually decrease the use of petrochemical energy and petroleum feedstock and to develop new sources of renewable energy and materials.
[0004] Lignocellulose is the main ingredient of biomass, which is the most abundant organic substance in the world. Lignocellulose mainly consists of 38-50% cellulose, 23-32% hemicellulose and 15-25% lignin. Cellulose generates glucose through hydrolysis. However, it is difficult for chemicals to enter the interior of cellulose molecules for depolymerization due to strong intermolecular and intramolecular hydrogen bonding and Van de Waal forces and the complex aggregate structure of cellulose with high-degree crystallinity. The main methods of hydrolyzing cellulose are enzyme hydrolysis and acid hydrolysis. However, there is significant imperfection in these two technologies, therefore, it is difficult to apply widely.
[0005] Generally speaking, enzyme hydrolysis can be carried out at room temperature, which is an environmentally friendly method due to the rarity of byproducts, no production of anti-sugar fermentation substances, and integration with the fermentation process. However, a complicated pretreatment process is required, hydrolytic activity is low, the reaction rate is slow, and cellulose hydrolysis enzyme is expensive.
[0006] Dilute acid hydrolysis generally uses comparatively cheap sulfuric acid as a catalyst, but it must operate in a corrosion-resistant pressure vessel at more than 200°C, requiring high-level equipment; simultaneously, the temperature of the dilute acid hydrolysis is high, the byproduct thereof is plentiful, and the sugar yield is low. Concentrated acid hydrolysis can operate at lower temperature and normal pressure. However, there are problems of strong corrosivity of concentrated acid, complications in the post-treatment process of the hydrolyzed solution, large consumption of acid, and difficulties with recycling, among other drawbacks.
[0007] WO 2006/007691 A1 discloses a sugar product which comprises glucose and a sugar monomer selected from the group consisting of xylose, arabinose, mannose, galactose and a combination thereof and acetic acid and also comprises an inorganic salt and acetate salt.
SUMMARY
[0008] One embodiment of the disclosure provides a sugar product, comprising: a sugar mixture comprising glucose, xylose, mannose, arabinose and oligosaccharides thereof with a weight ratio of 2-15wt%; an acid compound with a weight ratio of 48-97wt%; and a salt compound with a weight ratio of 1-50wt%, wherein the salt compound comprises lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide or iron bromide.
[0009] One embodiment of the disclosure provides a method for fabricating a sugar product, comprising: mixing formic acid or acetic acid and lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide, iron bromide, or heteropoly acid to form a mixing solution; adding a cellulosic biomass to the mixing solution for a dissolution reaction; and adding water to the mixing solution for a hydrolysis reaction to obtain a sugar product.
DETAILED DESCRIPTION
[0011] In the following detailed description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the disclosed embodiments. It will be apparent, however, that one or more embodiments may be practiced without these specific details. In other instances, well-known structures and devices are schematically shown in order to simplify the drawing.
[0012] In one embodiment of the disclosure, a sugar product is provided. The sugar product comprises a sugar mixture, an acid compound, and a salt compound. The sugar mixture comprises glucose, xylose, mannose, arabinose and oligosaccharides thereof with a weight ratio of about 2-15wt% in the sugar product. The acid compound may comprise formic acid or acetic acid with a weight ratio of about 48-97wt% in the sugar product. The salt compound may comprise lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide, or iron bromide with a weight ratio of about 1-50wt% in the sugar product.
[0013] In one embodiment of the disclosure, a method for fabricating a sugar product is provided, comprising the following steps. First, formic acid or acetic acid and lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide, iron bromide, or heteropoly acid are mixed to form a mixing solution. A cellulosic biomass is added to the mixing solution for a dissolution reaction. Water is added to the mixing solution for a hydrolysis reaction to obtain a sugar product.
[0015] The lithium chloride or lithium bromide has a weight ratio of about 5-20wt% or 10-20wt% in the mixing solution.
[0016] The magnesium chloride or magnesium bromide has a weight ratio of about 10-30wt% or 15-20wt% in the mixing solution.
[0017] The calcium chloride or calcium bromide has a weight ratio of about 12-40wt% or 12-30wt% in the mixing solution.
[0018] The zinc chloride or zinc bromide has a weight ratio of about 5-45wt% or 20-30wt% in the mixing solution.
[0019] The iron chloride or iron bromide has a weight ratio of about 1-50wt% or 5-10wt% in the mixing solution.
[0020] The heteropoly acid may comprise H3PW12O40, H4SiWi2O40, H3PMo12O40 or H4SiMo12O40 with a weight ratio of about 1-5wt% or 2-5wt% in the mixing solution.
[0021] The cellulosic biomass may be derived from wood, grass, leaves, algae, waste paper, corn stalks, corn cobs, rice straw, rice husk, wheat straw, bagasse, bamboo, or crop stems. The cellulosic biomass may comprise cellulose, hemicellulose, or lignin with a weight ratio of about 1-20wt% or 5-15wt% in the mixing solution.
[0022] The dissolution reaction has a reaction temperature of about 40-90 or 50-70 and a reaction time of about 20-360 minutes or 30-120 minutes.
[0023] In the hydrolysis reaction, the amount of water added is larger than the total molar equivalent of monosaccharides hydrolyzed from the cellulosic biomass.
[0024] The hydrolysis reaction has a reaction temperature of about 50-150°C or 60-105 °C and a reaction time of about 30-180 minutes or 30-120 minutes.
[0025] The sugar product fabricated by the method may comprise a sugar mixture, an acid compound, and a salt compound. The sugar mixture may comprise glucose, xylose, mannose, arabinose and oligosaccharides thereof with a weight ratio of about 2-15wt% in the sugar product. The acid compound may comprise formic acid or acetic acid with a weight ratio of about 48-97wt% in the sugar product. The salt compound may comprise lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide, or iron bromide with a weight ratio of about 1-50wt% in the sugar product.
[0026] In one embodiment, the method further comprises adding inorganic acid to the mixing solution before, during or after the dissolution reaction. The inorganic acid may comprise sulfuric acid or hydrochloric acid. The inorganic acid has a weight ratio of about 1-2wt% in the mixing solution. When the inorganic acid is added, the adding amount of the chloride salt or the bromide salt may be reduced, for example, the weight ratio of the magnesium chloride, the magnesium bromide, the calcium chloride or the calcium bromide in the mixing solution may be reduced to about 1-10wt%, and the weight ratio of the lithium chloride, the lithium bromide, the zinc chloride, the zinc bromide, the iron chloride or the iron bromide in the mixing solution may be reduced to about 1-5wt%.
[0027] In the disclosure, formic acid or acetic acid (weak acid) is mixed with lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide, or iron bromide to be utilized as a solvent with the characteristic of dissolving cellulose under low temperature (<90°C) and rapid reaction time (<6 hours) to generate a homogeneous liquid. In the disclosed method, cellulose is dissolved in the solvent formed by chloride salt or bromide salt and formic acid or acetic acid to generate a homogeneous liquid at 40-150°C, and a sugar product is further obtained through hydrolysis. This method achieves the technical goals of low temperature, normal pressure, rapid reaction time and high sugar yield and without use of a strong acid corrosion-resistant reactor.
Examples
Example 1-1
[0028] Formic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (60wt% of formic acid, 40wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (15wt% of Avicel®cellulose) for a dissolution reaction (50 , 20 minutes) to form a yellow, homogeneous, and transparent liquid, as recorded in Table 1.
Example 1-2
[0029] Formic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (60wt% of formic acid, 40wt% of zinc chloride). α-cellulose (Sigma Corporation, C8002) was added to the mixing solution (15wt% of α-cellulose) for a dissolution reaction (50°C, 20 minutes) to form an amber, homogeneous, and transparent liquid, as recorded in Table 1.
Example 1-3
[0030] Formic acid and calcium chloride (CaCl2) were mixed and heated to form a mixing solution (75wt% of formic acid, 25wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (6wt% of Avicel®cellulose) for a dissolution reaction (65 °C , 90 minutes) to form a yellow, homogeneous, and transparent liquid, as recorded in Table 1.
Example 1-4
[0031] Formic acid and calcium chloride (CaCl2) were mixed and heated to form a mixing solution (75wt% of formic acid, 25wt% of calcium chloride). α-cellulose (Sigma Corporation, C8002) was added to the mixing solution (6wt% of α-cellulose) for a dissolution reaction (65°C, 90 minutes) to form an amber, homogeneous, and transparent liquid, as recorded in Table 1.
Example 1-5
[0032] Formic acid and magnesium chloride (MgCl2) were mixed and heated to form a mixing solution (80wt% of formic acid, 20wt% of magnesium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (65 °C , 120 minutes) to form an amber, homogeneous, and transparent liquid, as recorded in Table 1.
Example 1-6
[0033] Formic acid and magnesium chloride (MgCl2) were mixed and heated to form a mixing solution (80wt% of formic acid, 20wt% of magnesium chloride). α-cellulose (Sigma Corporation, C8002) was added to the mixing solution (5wt% of α-cellulose) for a dissolution reaction (65°C, 120 minutes) to form an amber, homogeneous, and transparent liquid, as recorded in Table 1.
Table 1
| Examples | Salt (wt%) | Cellulose (wt%) | Dissolution temp. (°C) | Dissolution time (min) | Solution appearance |
| 1-1 | zinc chloride (40) | Avicel®cellulose (15) | 50 | 20 | yellow, homogeneous and transparent liquid |
| 1-2 | zinc chloride (40) | α-cellulose (15) | 50 | 20 | amber, homogeneous and transparent liquid |
| 1-3 | calcium chloride (25) | Avicel®cellulose (6) | 65 | 90 | yellow, homogeneous and transparent liquid |
| 1-4 | calcium chloride (25) | α-cellulose (6) | 65 | 90 | amber, homogeneous and transparent liquid |
| 1-5 | magnesium chloride (20) | Avicel®cellulose (5) | 65 | 120 | amber, homogeneous and transparent liquid |
| 1-6 | magnesium chloride (20) | α-cellulose (5) | 65 | 120 | amber, homogeneous and transparent liquid |
Example 2-1
[0034] Formic acid and lithium chloride (LiCl) were mixed and heated to form a mixing solution (90wt% of formic acid, 10wt% of lithium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-2
[0035] Formic acid and lithium chloride (LiCl) were mixed and heated to form a mixing solution (95wt% of formic acid, 5wt% of lithium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 12 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-3
[0036] Formic acid and sodium chloride (NaCl) were mixed and heated to form a mixing solution (90wt% of formic acid, 10wt% of sodium chloride (saturated solution)). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 19 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-4
[0037] Formic acid and lithium bromide (LiBr) were mixed and heated to form a mixing solution (90wt% of formic acid, 10wt% of lithium bromide). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 0.5 hour). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-5
[0038] Formic acid and sodium bromide (NaBr) were mixed and heated to form a mixing solution (82wt% of formic acid, 18wt% of sodium bromide). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 9 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-6
[0039] Formic acid and calcium bromide (CaBr2) were mixed and heated to form a mixing solution (88wt% of formic acid, 12wt% of calcium bromide). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-7
[0040] Formic acid and barium bromide (BaBr2) were mixed and heated to form a mixing solution (80wt% of formic acid, 20wt% of barium bromide). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-8
[0041] Formic acid and magnesium chloride (MgCl2) were mixed and heated to form a mixing solution (80wt% of formic acid, 20wt% of magnesium chloride (saturated solution)). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (65 °C , 2 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-9
[0042] Formic acid and magnesium chloride (MgCl2) were mixed and heated to form a mixing solution (90wt% of formic acid, 10wt% of magnesium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 12 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-10
[0043] Formic acid and calcium chloride (CaCl2) were mixed and heated to form a mixing solution (75wt% of formic acid, 25wt% of calcium chloride (saturated solution)). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (65°C, 1.5 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-11
[0044] Formic acid and calcium chloride (CaCl2) were mixed and heated to form a mixing solution (82.5wt% of formic acid, 17.5wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 2 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-12
[0045] Formic acid and calcium chloride (CaCl2) were mixed and heated to form a mixing solution (88wt% of formic acid, 12wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-13
[0046] Formic acid and calcium chloride (CaCl2) were mixed and heated to form a mixing solution (90wt% of formic acid, 10wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 12 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-14
[0047] Formic acid and barium chloride (BaCl2) were mixed and heated to form a mixing solution (85wt% of formic acid, 15wt% of barium chloride (saturated solution)). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, >6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-15
[0048] Formic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (60wt% of formic acid, 40wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (50°C, 0.25 hour). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-16
[0049] Formic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (80wt% of formic acid, 20wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (65°C, 0.25 hour). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-17
[0050] Formic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (95wt% of formic acid, 5wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-18
[0051] Formic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (98wt% of formic acid, 2wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C , >6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-19
[0052] Formic acid and iron chloride (FeCl3) were mixed and heated to form a mixing solution (95wt% of formic acid, 5wt% of iron chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 1 hour). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-20
[0053] Formic acid and iron chloride (FeCl3) were mixed and heated to form a mixing solution (98wt% of formic acid, 2wt% of iron chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 3 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-21
[0054] Formic acid and iron chloride (FeCl3) were mixed and heated to form a mixing solution (99wt% of formic acid, 1wt% of iron chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example2-22
[0055] Formic acid and ammonium chloride (NH4Cl) were mixed and heated to form a mixing solution (90wt% of formic acid, 10wt% of ammonium chloride (saturated solution)). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, >12 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-23
[0056] Formic acid and aluminum chloride (AlCl3) were mixed and heated to form a mixing solution (98wt% of formic acid, 2wt% of aluminum chloride (saturated solution)). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70 °C , 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-24
[0057] Formic acid and tin chloride (SnCl3) were mixed and heated to form a mixing solution (95wt% of formic acid, 5wt% of tin chloride (saturated solution)). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70 °C , 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-25
[0058] Formic acid and calcium sulfate (CaSO4) were mixed and heated to form a mixing solution (80wt% of formic acid, 20wt% of calcium sulfate). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Example 2-26
[0059] Formic acid and heteropoly acid (H3PW12O40) were mixed and heated to form a mixing solution (99wt% of formic acid, 1wt% of heteropoly acid). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). The dissolution of cellulose was observed using a polarizing microscope, as recorded in Table 2.
Table 2
| Examples | Salt | wt% | Dissolution temp. (°C) | Dissolution time (hour) | Dissolution of cellulose |
| 2-1 | lithium chloride | 10 | 70 | 6 | complete dissolution |
| 2-2 | 5 | 70 | 12 | no dissolution | |
| 2-3 | sodium chloride | 10, saturated | 70 | 19 | no dissolution |
| 2-4 | lithium bromide | 10 | 70 | 0.5 | complete dissolution |
| 2-5 | sodium bromide | 18 | 70 | 9 | no dissolution |
| 2-6 | calcium bromide | 12 | 70 | 6 | complete dissolution |
| 2-7 | barium bromide | 20 | 70 | 6 | no dissolution |
| 2-8 | magnesium chloride | 20, saturated | 65 | 2 | complete dissolution |
| 2-9 | 10 | 70 | 12 | no dissolution | |
| 2-10 | calcium chloride | 25, saturated | 65 | 1.5 | complete dissolution |
| 2-11 | 17.5 | 70 | 2 | complete dissolution | |
| 2-12 | 12 | 70 | 6 | complete dissolution | |
| 2-13 | 10 | 70 | 12 | no dissolution | |
| 2-14 | barium chloride | 15, saturated | 70 | >6 | no dissolution |
| 2-15 | zinc chloride | 40 | 50 | 0.25 | complete dissolution |
| 2-16 | 20 | 65 | 0.25 | complete dissolution | |
| 2-17 | 5 | 70 | 6 | complete dissolution | |
| 2-18 | 2 | 70 | >6 | no dissolution | |
| 2-19 | iron chloride | 5 | 70 | 1 | complete dissolution |
| 2-20 | 2 | 70 | 3 | complete dissolution | |
| 2-21 | 1 | 70 | 6 | complete dissolution | |
| 2-22 | ammonium chloride | 10, saturated | 70 | >12 | no dissolution |
| 2-23 | aluminum chloride | 2, saturated | 70 | 6 | no dissolution |
| 2-24 | tin chloride | 5, saturated | 70 | 6 | no dissolution < |
| 2-25 | calcium sulfate | 20 | 70 | 6 | no dissolution |
| 2-26 | heteropoly acid (H3PW12O40) | 1 | 70 | 6 | complete dissolution |
Example 3-1
[0060] Formic acid and magnesium chloride (MgCl2) were mixed by stirring and heated to 70°C under 1 atm to form a mixing solution (80wt% of formic acid, 20wt% of magnesium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 2 hours). After the complete dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (120 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Magnesium carbonate (MgCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 3.
Example 3-2
[0061] Formic acid and magnesium chloride (MgCl2) were mixed by stirring and heated to 70°C under 1 atm to form a mixing solution (90wt% of formic acid, 10wt% of magnesium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 6 hours). After the complete dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (120 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Magnesium carbonate (MgCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 3.
Table 3
| Examples | Cellulose (wt%) | Mixing solution (magnesium chloride: formic acid) (wt%) | Dissolution temp. (°C) | Dissolution time (hour) | Hydrolysis temp. (°C) | Hydrolysis time (min) | Yield of reducing sugar (%) |
| 3-1 | 5 | 20: 80 | 70 | 2 | 100 | 120 | 97.9 |
| 3-2 | 5 | 10: 90 | 70 | 6 | 100 | 120 | 75.3 |
Example 4-1
[0062] Formic acid and calcium chloride (CaCl2) were mixed by stirring and heated to 50°C under 1 atm to form a mixing solution (85wt% of formic acid, 15wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (50°C, 4 hours). After the complete dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (60 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Calcium carbonate (CaCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 4.
Example 4-2
[0063] Formic acid and calcium chloride (CaCl2) were mixed by stirring and heated to 70°C under 1 atm to form a mixing solution (88wt% of formic acid, 12wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (70°C, 4 hours). After the complete dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (60 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Calcium carbonate (CaCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 4.
Example 4-3
[0064] Formic acid and calcium chloride (CaCl2) were mixed by stirring and heated to 90°C under 1 atm to form a mixing solution (90wt% of formic acid, 10wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (90°C, 4 hours). After the complete dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (60 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Calcium carbonate (CaCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 4.
Table 4
| Examples | Cellulose (wt%) | Mixing solution (calcium chloride: formic acid) (wt%) | Dissolution temp. (°C) | Dissolution time (hour) | Hydrolysis temp. (°C) | Hydrolysis time (min) | Yield of reducing sugar (%) |
| 4-1 | 5 | 15: 85 | 50 | 4 | 100 | 60 | 78.4 |
| 4-2 | 5 | 12: 88 | 70 | 4 | 100 | 60 | 70.6 |
| 4-3 | 5 | 10: 90 | 90 | 4 | 100 | 60 | 67.3 |
Example 5-1
[0065] Formic acid and zinc chloride (ZnCl2) were mixed by stirring and heated to 50°C under 1 atm to form a mixing solution (60wt% of formic acid, 40wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (50°C). After the complete dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (30 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Zinc carbonate (ZnCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 5.
Example 5-2
[0066] Formic acid and zinc chloride (ZnCl2) were mixed by stirring and heated to 50°C under 1 atm to form a mixing solution (60wt% of formic acid, 40wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (50°C). After the complete dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (45 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Zinc carbonate (ZnCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 5.
Table 5
| Examples | Cellulose (wt%) | Adding amount of water (wt%) | Hydrolysis time (min) | Yield of reducing sugar (%) |
| 5-1 | 5 | 50 | 30 | 65 |
| 5-2 | 5 | 50 | 45 | 89 |
Example 6
[0067] Formic acid and zinc chloride (ZnCl2) were mixed by stirring and heated to 55 °C under 1 atm to form a mixing solution (60wt% of formic acid, 40wt% of zinc chloride). Dried bagasse (comprising 43.58wt% of glucan, 24.02wt% of xylan, 12.45wt% of acid-soluble lignin, 18.12wt% of acid-insoluble lignin and 1.71wt% of ash) was added to the mixing solution (5wt% of bagasse) for a dissolution reaction (55 °C). After the dissolution of the bagasse, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (120 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Zinc carbonate (ZnCO3) precipitate was then removed from the mixing solution. Next, the yields of glucose and xylose were analyzed using high performance liquid chromatography (HPLC) and the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the glucose is the ratio of the moles of the produced glucose and the moles of the glucose monomers contained in the cellulose in the bagasse. The yield of the xylose is the ratio of the moles of the produced xylose and the moles of the xylose monomers contained in the hemicellulose in the bagasse. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the total weight of the cellulose and hemicellulose in the bagasse. The result is shown in Table 6. After the hydrolysis reaction, a hydrolyzed solution comprising 25.3wt% of zinc chloride, 33.2wt% of water, 38.2wt% of formic acid, 2.3wt% of reducing sugar (comprising 43.2wt% of glucose and 30.4wt% of xylose), 0.4wt% of acid-soluble lignin and 0.6wt% of acid-insoluble lignin was formed.
Table 6
| Examples | Bagasse (wt%) | Amount of water added (wt%) | Hydrolysis time (min) | Yield of glucose (%) | Yield of xylose (%) | Yield of reducing sugar (%) |
| 6-1 | 5 | 50 | 30 | 36.3 | 88.5 | 93.3 |
| 6-2 | 5 | 50 | 60 | 53.3 | 94.2 | 97.9 |
| 6-3 | 5 | 50 | 120 | 70.4 | 89.9 | 105.2 |
Example 7
[0068] Formic acid and magnesium chloride (MgCl2) were mixed by stirring and heated to 50°C under 1 atm to form a mixing solution (80wt% of formic acid, 20wt% of magnesium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (50°C, 2.5 hours). After the dissolution of the cellulose, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (90 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Magnesium carbonate (MgCO3) precipitate was then removed from the mixing solution. Next, the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the weight of the cellulose. The result is shown in Table 7.
Table 7
| Examples | Cellulose (wt%) | Mixing solution (magnesium chloride: formic acid) (wt%) | Dissolution temp. (°C) | Dissolution time (hour) | Hydrolysis temp. (°C) | Hydrolysis time (min) | Yield of reducing sugar (%) |
| 7 | 5 | 20: 80 | 50 | 2.5 | 100 | 0th | 46 |
| 100 | 90th | 89 |
Example 8
[0069] Formic acid and zinc chloride (ZnCl2) were mixed by stirring and heated to 55 °C under 1 atm to form a mixing solution (60wt% of formic acid, 40wt% of zinc chloride). Dried corn stalks (comprising 44.5wt% of glucan, 12.4wt% of xylan, 4.6wt% of acid-soluble lignin, 24.4wt% of acid-insoluble lignin, 2.7wt% of water and 3.8wt% of ash) was added to the mixing solution (5wt% of corn stalks) for a dissolution reaction (55°C). After the dissolution of the corn stalks, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction (90 minutes). Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Zinc carbonate (ZnCO3) precipitate was then removed from the mixing solution. Next, the yields of glucose and xylose were analyzed using high performance liquid chromatography (HPLC) and the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the glucose is the ratio of the moles of the produced glucose and the moles of the glucose monomers contained in the cellulose in the corn stalks. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the total weight of the cellulose and hemicellulose in the corn stalks. The result is shown in Table 8.
Table 8
| Examples | Corn stalks (wt%) | Amount of water added (wt%) | Hydrolysis time (min) | Yield of glucose (%) | Yield of reducing sugar (%) |
| 8 | 5 | 50 | 90 | 85 | 96 |
Example 9-1
[0070] 37wt% of HCl, zinc chloride (ZnCl2) and formic acid were mixed by stirring and heated to 55°C under 1 atm to form a mixing solution (1wt% of HCl, 5wt% of zinc chloride, 94wt% of formic acid). Dried bagasse (comprising 40.7wt% of glucan, 20.5wt% of xylan, 2.9wt% of Arab polysaccharides, 27.4wt% of lignin, 3.3wt% of ash and 5.2wt% of other ingredients) was added to the mixing solution (10wt% of bagasse) for a dissolution reaction (65°C). After the dissolution of the bagasse, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction. Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Zinc carbonate (ZnCO3) precipitate was then removed from the mixing solution. Next, the yields of glucose and xylose were analyzed using high performance liquid chromatography (HPLC) and the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the glucose is the ratio of the moles of the produced glucose and the moles of the glucose monomers contained in the cellulose in the bagasse. The yield of the xylose is the ratio of the moles of the produced xylose and the moles of the xylose monomers contained in the hemicellulose in the bagasse. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the total weight of the cellulose and hemicellulose in the bagasse. The result is shown in Table 9.
Example 9-2
[0071] 37wt% of HCl, iron chloride (FeCl3) and formic acid were mixed by stirring and heated to 55°C under 1 atm to form a mixing solution (1wt% of HCl, 2wt% of iron chloride, 97wt% of formic acid). Dried bagasse (comprising 40.7wt% of glucan, 20.5wt% of xylan, 2.9wt% of Arab polysaccharides, 27.4wt% of lignin, 3.3wt% of ash and 5.2wt% of other ingredients) was added to the mixing solution (10wt% of bagasse) for a dissolution reaction (65°C). After the dissolution of the bagasse, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction. Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Iron carbonate (Fe2(CO3)3) precipitate was then removed from the mixing solution. Next, the yields of glucose and xylose were analyzed using high performance liquid chromatography (HPLC) and the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the glucose is the ratio of the moles of the produced glucose and the moles of the glucose monomers contained in the cellulose in the bagasse. The yield of the xylose is the ratio of the moles of the produced xylose and the moles of the xylose monomers contained in the hemicellulose in the bagasse. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the total weight of the cellulose and hemicellulose in the bagasse. The result is shown in Table 9.
Example 9-3
[0072] 98wt% of H2SO4, iron chloride (FeCl3) and formic acid were mixed by stirring and heated to 55°C under 1 atm to form a mixing solution (1wt% of H2SO4, 2wt% of iron chloride, 97wt% of formic acid). Dried bagasse (comprising 40.7wt% of glucan, 20.5wt% of xylan, 2.9wt% of Arab polysaccharides, 27.4wt% of lignin, 3.3wt% of ash and 5.2wt% of other ingredients) was added to the mixing solution (10wt% of bagasse) for a dissolution reaction (65°C). After the dissolution of the bagasse, water was added to the mixing solution (50wt% of water) and the mixing solution was heated to 100°C for a hydrolysis reaction. Next, saturated sodium carbonate (Na2CO3) aqueous solution was added to neutralize the mixing solution. Iron carbonate (Fe2(CO3)3) precipitate was then removed from the mixing solution. Next, the yields of glucose and xylose were analyzed using high performance liquid chromatography (HPLC) and the total weight of the reducing sugar was measured using 3,5-dinitro-salicylic acid (DNS) method. The yield of the reducing sugar was then calculated. The reducing sugar comprised glucose, xylose, mannose, arabinose and oligosaccharides thereof. The yield of the glucose is the ratio of the moles of the produced glucose and the moles of the glucose monomers contained in the cellulose in the bagasse. The yield of the xylose is the ratio of the moles of the produced xylose and the moles of the xylose monomers contained in the hemicellulose in the bagasse. The yield of the reducing sugar is the ratio of the total weight of the reducing sugar and the total weight of the cellulose and hemicellulose in the bagasse. The result is shown in Table 9.
Table 9
| Examples | Hydrolysis time (min) | Yield of glucose (%) | Yield of xylose (%) | Yield of reducing sugar (%) |
| 9-1 | 90 | 67.5 | 82.7 | 94.5 |
| 9-2 | 90 | 57.5 | 78.3 | 76.6 |
| 9-3 | 90 | 50.5 | 85.3 | 75.1 |
Example 10-1
[0073] Formic acid, acetic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (54wt% of formic acid, 6wt% of acetic acid and 40wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (60°C, 60 minutes), forming an amber transparent liquid with an uniform phase. The dissolution of cellulose was observed using a polarizing microscope. The cellulose was completely dissolved.
Example 10-2
[0074] Formic acid, acetic acid and calcium chloride (CaCl2) were mixed and heated to form a mixing solution (72wt% of formic acid, 8wt% of acetic acid and 20wt% of calcium chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (60°C, 180 minutes), forming an amber transparent liquid with an uniform phase. The dissolution of cellulose was observed using a polarizing microscope. The cellulose was completely dissolved.
Example 10-3
[0075] Formic acid, acetic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (50wt% of formic acid, 10wt% of acetic acid and 40wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (65°C, 60 minutes), forming an amber transparent liquid with an uniform phase. The dissolution of cellulose was observed using a polarizing microscope. The cellulose was completely dissolved.
Example 10-4
[0076] Formic acid, acetic acid and zinc chloride (ZnCl2) were mixed and heated to form a mixing solution (40wt% of formic acid, 20wt% of acetic acid and 40wt% of zinc chloride). Avicel®cellulose (Sigma Corporation, Avicel-pH-105-27NI) was added to the mixing solution (5wt% of Avicel®cellulose) for a dissolution reaction (65°C, 60 minutes), forming an amber transparent liquid with an uniform phase. The dissolution of cellulose was observed using a polarizing microscope. The cellulose was completely dissolved.
[0077] It will be apparent to those skilled in the art that various modifications and variations can be made to the disclosed embodiments. It is intended that the specification and examples be considered as exemplary only, with the true scope of the disclosure being indicated by the following claims and their equivalents.
1. A sugar product, comprising:
a sugar mixture comprising glucose, xylose, mannose, arabinose and oligosaccharides thereof with a weight ratio of 2-15wt%;
an acid compound with a weight ratio of 48-97wt%; and
a salt compound with a weight ratio of 1-50wt%, wherein the salt compound comprises lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide or iron bromide.
2. The sugar product as claimed in claim 1, wherein the acid compound comprises organic
acid compounds or inorganic acid compounds.
3. The sugar product as claimed in claim 1, wherein acid compound comprises formic acid,
acetic acid or a mixture thereof.
4. A method for fabricating a sugar product, comprising:
mixing an acid compound and lithium chloride, magnesium chloride, calcium chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium bromide, zinc bromide, iron bromide or heteropoly acid to form a mixing solution;
adding a cellulosic biomass to the mixing solution for a dissolution reaction; and
adding water to the mixing solution for a hydrolysis reaction to obtain a sugar product.
5. The method for fabricating a sugar product as claimed in claim 4, wherein the acid compound comprises formic acid, acetic acid or a mixture thereof.
6. The method for fabricating a sugar product as claimed in claim 5, wherein the formic
acid or acetic acid has a weight ratio of 50-97wt% in the mixing solution.
7. The method for fabricating a sugar product as claimed in claim 4, wherein the lithium chloride or lithium bromide has a weight ratio of 5-20wt% in
the mixing solution.
8. The method for fabricating a sugar product as claimed in claim 4, wherein the magnesium chloride or magnesium bromide has a weight ratio of 10-30wt%
in the mixing solution.
9. The method for fabricating a sugar product as claimed in claim 4, wherein the calcium chloride or calcium bromide has a weight ratio of 12-40wt% in
the mixing solution.
10. The method for fabricating a sugar product as claimed in claim 4, wherein the zinc chloride or zinc bromide has a weight ratio of 5-45wt% in the mixing
solution.
11. The method for fabricating a sugar product as claimed in claim 4, wherein the iron chloride or iron bromide has a weight ratio of 1-50wt% in the mixing
solution.
12. The method for fabricating a sugar product as claimed in claim 4, wherein the heteropoly acid comprises H3PW12O40, H4SiW12O40, H3PMo12O40 or H4SiMo12O40.
13. The method for fabricating a sugar product as claimed in claim 4, wherein the heteropoly acid has a weight ratio of 1-5wt% in the mixing solution.
14. The method for fabricating a sugar product as claimed in claim 4, wherein the cellulosic biomass comprises cellulose, hemicellulose or lignin.
15. The method for fabricating a sugar product as claimed in claim 4, wherein the cellulosic biomass is derived from wood, grass, leaves, algae, waste
paper, corn stalks, corn cobs, rice straw, rice husk, wheat straw, bagasse, bamboo
or crop stems.
16. The method for fabricating a sugar product as claimed in claim 4, wherein the dissolution reaction has a reaction temperature of 40-90°C.
17. The method for fabricating a sugar product as claimed in claim 4, wherein the dissolution reaction has a reaction time of 20-360 minutes.
18. The method for fabricating a sugar product as claimed in claim 4, wherein the amount of water added is larger than the total molar equivalent of monosaccharides
hydrolyzed from the cellulosic biomass.
19. The method for fabricating a sugar product as claimed in claim 4, wherein the hydrolysis reaction has a reaction temperature of 50-150°C .
20. The method for fabricating a sugar product as claimed in claim 4, wherein the hydrolysis reaction has a reaction time of 30-180 minutes.
21. The method for fabricating a sugar product as claimed in claim 4, wherein the sugar product comprises a sugar mixture, an acid compound and a salt
compound.
22. The method for fabricating a sugar product as claimed in claim 21, wherein the sugar mixture comprises glucose, xylose, mannose, arabinose and oligosaccharides
thereof.
23. The method for fabricating a sugar product as claimed in claim 21, wherein the sugar mixture has a weight ratio of 2-15wt% in the sugar product.
24. The method for fabricating a sugar product as claimed in claim 21, wherein the salt compound comprises lithium chloride, magnesium chloride, calcium
chloride, zinc chloride, iron chloride, lithium bromide, magnesium bromide, calcium
bromide, zinc bromide or iron bromide.
25. The method for fabricating a sugar product as claimed in claim 21, wherein the salt compound has a weight ratio of 1-50wt% in the sugar product.
26. The method for fabricating a sugar product as claimed in claim 4, further comprising adding inorganic acid to the mixing solution.
27. The method for fabricating a sugar product as claimed in claim 26, wherein the inorganic acid comprises sulfuric acid or hydrochloric acid.
28. The method for fabricating a sugar product as claimed in claim 26, wherein the inorganic acid has a weight ratio of 1-2wt% in the mixing solution.
29. The method for fabricating a sugar product as claimed in claim 26, wherein the magnesium chloride, the magnesium bromide, the calcium chloride or the
calcium bromide has a weight ratio of 1-10wt% in the mixing solution.
30. The method for fabricating a sugar product as claimed in claim 26, wherein the lithium chloride, lithium bromide, the zinc chloride, the zinc bromide,
the iron chloride or iron bromide has a weight ratio of 1-5wt% in the mixing solution.
1. Zuckerprodukt, umfassend:
ein Zuckergemisch, umfassend Glucose, Xylose, Mannose, Arabinose und Oligosaccharide davon, mit einem Gewichtsverhältnis von 2-15 Gew.-%;
eine Säureverbindung mit einem Gewichtsverhältnis von 48-97 Gew.-%; und
eine Salzverbindung mit einem Gewichtsverhältnis von 1-50 Gew.-%, wobei die Salzverbindung Lithiumchlorid, Magnesiumchlorid, Calciumchlorid, Zinkchlorid, Eisenchlorid, Lithiumbromid, Magnesiumbromid, Calciumbromid, Zinkbromid oder Eisenbromid umfasst.
2. Zuckerprodukt wie in Anspruch 1 beansprucht, wobei die Säureverbindung organische
Säureverbindungen oder anorganische Säureverbindungen umfasst.
3. Zuckerprodukt wie in Anspruch 1 beansprucht, wobei die Säureverbindung Ameisensäure,
Essigsäure oder ein Gemisch davon umfasst.
4. Verfahren zur Herstellung eines Zuckerprodukts, umfassend:
Mischen von einer Säureverbindung und Lithiumchlorid, Magnesiumchlorid, Calciumchlorid, Zinkchlorid, Eisenchlorid, Lithiumbromid, Magnesiumbromid, Calciumbromid, Zinkbromid, Eisenbromid oder Heteropolysäure, um ein Lösungsgemisch zu bilden;
Geben einer Cellulosebiomasse zu dem Lösungsgemisch für eine Lösungsreaktion; und
Geben von Wasser zu dem Lösungsgemisch für eine Hydrolysereaktion, wobei ein Zuckerprodukt erhalten wird.
5. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Säureverbindung Ameisensäure, Essigsäure oder ein Gemisch davon umfasst.
6. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 5 beansprucht, wobei
die Ameisensäure oder Essigsäure ein Gewichtsverhältnis von 50-97 Gew.-% in dem Lösungsgemisch
aufweist.
7. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
das Lithiumchlorid oder Lithiumbromid ein Gewichtsverhältnis von 5-20 Gew.-% in dem
Lösungsgemisch aufweist.
8. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
das Magnesiumchlorid oder Magnesiumbromid, ein Gewichtsverhältnis von 10-30 Gew.-%
in dem Lösungsgemisch aufweist.
9. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
das Calciumchlorid oder Calciuxnbromid ein Gewichtsverhältnis von 12-40 Gew.-% in
dem Lösungsgemisch aufweist.
10. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
das Zinkchlorid oder Zinkbromid ein Gewichtsverhältnis von 5-45 Gew.-% in dem Lösungsgemisch
aufweist.
11. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
das Eisenchlorid oder Eisenbromid ein Gewichtsverhältnis von 1-50 Gew.-% in dem Lösungsgemisch
aufweist.
12. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Heteropolysäure H3PW12O40, H4SiW12O40, H3PMo12O40 oder H4SiMo12O40 umfasst.
13. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Heteropolysäure ein Gewichtsverhältnis von 1-5 Gew.-% in dem Lösungsgemisch aufweist.
14. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Cellulosebiomasse Cellulose, Hemicellulose oder Lignin umfasst.
15. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Cellulosebiomasse von Holz, Gras, Laub, Algen, Papierabfall, Getreidehalmen bzw.
Maisstängeln, Maiskolben, Reisstroh, Reisspelze, Weizenstroh, Bagasse, Bambus oder
Feldfruchthalmen bzw. -stängeln abgeleitet ist.
16. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Lösungsreaktion eine Reaktionstemperatur von 40-90°C aufweist.
17. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Lösungsreaktion eine Reaktionszeit von 20-360 Minuten aufweist.
18. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Menge an Wasser, die zugegeben wird, größer ist als das Gesamtmoläquivalent von
aus der Cellulosebiomasse hydrolysierten Monosacchariden.
19. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Hydrolysereaktion eine Reaktionstemperatur von 50-150°C aufweist.
20. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
die Hydrolysereaktion eine Reaktionszeit von 30-180 Minuten aufweist.
21. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, wobei
das Zuckerprodukt ein Zuckergemisch, eine Säureverbindung und eine Salzverbindung
umfasst.
22. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 21 beansprucht, wobei
das Zuckergemisch Glucose, Xylose, Mannose, Arabinose oder Oligosaccharide davon umfasst.
23. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 21 beansprucht, wobei
das Zuckergemisch ein Gewichtsverhältnis von 2-15 Gew.-% in dem Zuckerprodukt aufweist.
24. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 21 beansprucht, wobei
die Salzverbindung Lithiumchlorid, Magnesiumchlorid, Calciumchlorid, Zinkchlorid,
Eisenchlorid, Lithiumbromid, Magnesimnbromid, Calciumbromid, Zinkbromid oder Eisenbromid
umfasst.
25. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 21 beansprucht, wobei
die Salzverbindung ein Gewichtsverhältnis von 1-50 Gew.-% in dem Zuckerprodukt aufweist.
26. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 4 beansprucht, ferner
umfassend Geben einer anorganischen Säure zu dem Lösungsgemisch.
27. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 26 beansprucht, wobei
die anorganische Säure Schwefelsäure oder Chlorwasserstoffsäure umfasst.
28. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 26 beansprucht, wobei
die anorganische Säure ein Gewichtsverhältnis von 1-2 Gew.-% in dem Lösungsgemisch
aufweist.
29. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 26 beansprucht, wobei
das Magnesiumchlorid, das Magnesiumbromid, das Calciumchlorid oder das Calciumbromid
ein Gewichtsverhältnis von 1-10 Gew.-% in dem Lösungsgemisch aufweist.
30. Verfahren zur Herstellung eines Zuckerprodukts wie in Anspruch 26 beansprucht, wobei
das Lithiumchlorid, Lithiumbromid, das Zinkchlorid, das Zinkbromid, das Eisenchlorid
oder Eisenbromid ein Gewichtsverhältnis von 1-5 Gew.-% in dem Lösungsgemisch aufweist.
1. Produit formant sucre, comprenant :
un mélange de sucre comprenant du glucose, du xylose, du mannose, de l'arabinose et des oligosaccharides de ceux-ci avec un rapport massique de 2 à 15 % en poids ;
un composé acide avec un rapport massique de 48 à 97 % en poids ; et
un composé salin avec un rapport massique de 1 à 50 % en poids, dans lequel le composé salin comprend du chlorure de lithium, du chlorure de magnésium, du chlorure de calcium, du chlorure de zinc, de chlorure de fer, du bromure de lithium, du bromure de magnésium, du bromure de calcium, du bromure de zinc ou du bromure de fer.
2. Produit formant sucre selon la revendication 1, dans lequel le composé acide comprend
des composés d'acide organique ou des composés d'acide inorganique.
3. Produit formant sucre selon la revendication 1, dans lequel le composé acide comprend
de l'acide formique, de l'acide acétique ou un mélange de ceux-ci.
4. Procédé de fabrication d'un produit formant sucre, comprenant :
le mélange d'un composé acide et de chlorure lithium, de chlorure de magnésium, de chlorure de calcium, de chlorure de zinc, de chlorure de fer, de bromure de lithium, de bromure de magnésium, de bromure de calcium, de bromure de zinc, de bromure de fer ou d'un hétéropolyacide de manière à former une solution de mélange ;
l'ajout d'une biomasse de cellulose à la solution de mélange afin d'assurer une réaction de dissolution ; et
l'ajout d'eau à la solution de mélange afin d'assurer une réaction d'hydrolyse de manière à obtenir un produit formant sucre.
5. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
le composé acide comprend de l'acide formique, de l'acide acétique ou un mélange de
ceux-ci.
6. Procédé de fabrication d'un produit formant sucre selon la revendication 5, dans lequel
l'acide formique ou l'acide acétique présente un rapport massique de 50 à 97 % en
poids dans la solution de mélange.
7. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
le chlorure de lithium ou le bromure de lithium présente un rapport massique de 5
à 20 % en poids dans la solution de mélange.
8. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
le chlorure de magnésium ou le bromure de magnésium présente un rapport massique de
10 à 30 % en poids dans la solution de mélange.
9. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
le chlorure de calcium ou le bromure de calcium présente un rapport massique de 12
à 40 % en poids dans la solution de mélange.
10. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
le chlorure de zinc ou le bromure de zinc présente un rapport massique de 5 à 45 %
en poids dans la solution de mélange.
11. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
le chlorure de fer ou le bromure de fer présente un rapport massique de 1 à 50 % en
poids dans la solution de mélange.
12. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
l'hétéropolyacide comprend le H3PW12O40, le H4SiW12O40, le H3PMo12O40 ou le H4SiMo12O40.
13. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
l'hétéropolyacide présente un rapport massique de 1 à 5 % en poids dans la solution
de mélange.
14. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
la biomasse cellulosique comprend de la cellulose, de l'hémicellulose ou de la lignine.
15. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
la biomasse de cellulose est un dérivé de bois, d'herbe, de feuilles, d'algues, de
déchet de papier, de maïs en grain, d'épis de maïs, de paille de riz, de cosse de
riz, de tiges de paille de blé, de bagasse, de bambou ou de tiges de plantes.
16. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
la réaction de dissolution présente une température de réaction de 40 à 90°C.
17. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
la réaction de dissolution présente un temps de réaction de 20 à 360 mn.
18. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
la quantité d'eau ajoutée est supérieure à l'équivalent molaire total des monosaccharides
hydrolysés à partir de la biomasse cellulosique.
19. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
la réaction d'hydrolyse présente une température de réaction de 50 à 150°C.
20. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
la réaction d'hydrolyse présente un temps de réaction de 30 à 180 minutes.
21. Procédé de fabrication d'un produit formant sucre selon la revendication 4, dans lequel
le produit formant sucre comprend un mélange de sucre, un composé d'acide et un composé
salin.
22. Procédé de fabrication d'un produit formant sucre selon la revendication 21, dans
lequel le mélange de sucre comprend du glucose, du xylose, du mannose, de l'arabinose
et des oligosaccharides de ceux-ci.
23. Procédé de fabrication d'un produit formant sucre selon la revendication 21, dans
lequel le mélange de sucre présente un rapport massique de 2 à 15 % en poids dans
le produit formant sucre.
24. Procédé de fabrication d'un produit formant sucre selon la revendication 21, dans
lequel le composé salin comprend du chlorure de lithium, du chlorure de magnésium,
du chlorure de calcium, du chlorure de zinc, du chlorure de fer, du bromure de lithium,
du bromure de magnésium, du bromure de calcium, du bromure de zinc ou du bromure de
fer.
25. Procédé de fabrication d'un produit formant sucre selon la revendication 21, dans
lequel le composé salin présente un rapport massique de 1 à 50 % en poids dans le
produit formant sucre.
26. Procédé de fabrication d'un produit formant sucre selon la revendication 4 comprenant,
en outre, l'ajout d'acide inorganique à la solution de mélange.
27. Procédé de fabrication d'un produit formant sucre selon la revendication 26, dans
lequel l'acide inorganique comprend de l'acide sulfurique ou de l'acide chlorhydrique.
28. Procédé de fabrication d'un produit formant sucre selon la revendication 26, dans
lequel l'acide inorganique présente un rapport massique de 1 à 2 % en poids dans la
solution de mélange.
29. Procédé de fabrication d'un produit formant sucre selon la revendication 26, dans
lequel le chlorure de magnésium, le bromure de magnésium, le chlorure de calcium ou
le bromure de calcium présente un rapport massique de 1 à 10 % en poids dans la solution
de mélange.
30. Procédé de fabrication d'un produit formant sucre selon la revendication 26, dans
lequel le chlorure de lithium, le bromure de lithium, le chlorure de zinc, le bromure
de zinc, le chlorure de fer ou le bromure de fer présente un rapport massique de 1
à 5 % en poids dans la solution de mélange.
REFERENCES CITED IN THE DESCRIPTION
This list of references cited by the applicant is for the reader's convenience only. It does not form part of the European patent document. Even though great care has been taken in compiling the references, errors or omissions cannot be excluded and the EPO disclaims all liability in this regard.
Patent documents cited in the description