CN103382512B - Glucose preparation method by hydrolyzing cellulose through microwave heating - Google Patents
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Abstract
The invention discloses a glucose preparation method by hydrolyzing cellulose through microwave heating. The glucose preparation method by hydrolyzing the cellulose through the microwave heating comprises steps of (1) dissolving cellulose raw materials into phosphoric acid of 81 wt % to 85 wt % to obtain a solution with the mass percent of 5% to 30 %, preprocessing for 10 to 180 minutes at the temperature of 40 to 60 DEG C, adding organic reagents and filtering and washing to obtain processed cellulose; (2) performing microwave heating of 800 to 1200 watts on the processed cellulose and performing diluted acid catalytic hydrolyzing at the temperature of 120 to 160 DEG C; (3) neutralizing, desalting, decoloring and precipitating a sugar solution obtained from the step (2) to obtain glucose solid. According to the glucose preparation method by hydrolyzing the cellulose through the microwave heating, the glucose is prepared by efficiently and high selectively hydrolyzing the cellulose through the microwave heating, the reaction temperature is low, the time is short, the energy consumption is low, the conversion rate of the cellulose achieves 80% to 95 %, the selectivity of the glucose is from 80% to 95 %, the glucose separation process is simple, and the purity is high.
Description
Technical field
The present invention relates to cellulosic hydrolysis field, relate in particular to a kind of method that microwave heating hydrocellulose is prepared glucose.
Background technology
Along with petering out of petrochemical industry resource becomes increasingly conspicuous with problem of environmental pollution, people more and more pay close attention to the development and utilization of green renewable resources, and wherein the utilization of biomass is study hotspots of people in recent years.Utilize biomass to produce fuel and chemical, not only can break away from the dependence of people to oil, reduce petrochemical industry resource simultaneously and use the carbonic acid gas producing.The organism that biomass refer to directly or indirect utilization green plants photosynthesis forms, is mainly starch and Mierocrystalline cellulose.Compared with starch, Mierocrystalline cellulose is as non-food crop, wide material sources, and reserves reach 1,000 hundred million tons/year, considerably beyond existing prospective oil, and cheap, environmental friendliness, is a kind of desirable biological material.
Mierocrystalline cellulose passes through β-1 by glucose unit, the linear natural polymer of 4 glycosidic link link compositions, its component units---glucose, as important hardware and software platform compound, can be used for producing various chemical (5 hydroxymethyl furfural (HMF), levulinic acid, polyvalent alcohol etc.), for fields such as chemical industry, fuel, therefore, it is effectively to utilize one of cellulosic important channel that cellulose hydrolysis is prepared glucose.But cellulosic molecule interchain, the strong hydrogen bond action of interior existence, have the chemical structure of quite stable, thereby the solution that feeds water is brought very large difficulty.At present, cellulosic method for hydrolysis mainly contains enzyme hydrolysis method and acid catalyzed hydrolysis.Enzymic hydrolysis selectivity is high, mild condition, but the hydrolysis cycle is long, and cellulase preparation is difficult, cost is high.Acid-catalyzed hydrolysis technical maturity, mainly contains concentrated acid and diluted acid catalytic hydrolysis.
Concentrated acid catalytic hydrolysis refers to the method that exceedes catalysis biomass in 30% sulfuric acid or hydrochloric acid and be hydrolyzed into monose in concentration.In concentrated acid catalyzing cellulose hydrolysis technology, product sugar is insoluble problem with separating of catalyst acid.
Chinese patent CN101157445A discloses the also method of reclaim(ed) sulfuric acid of organic solvent deposit sugar in vitriol oil hydrocellulose.In this patent working example 1, point out, the oligosaccharides being settled out from principal hydrolysis solution by organic reagent, need through in the further catalytic hydrolysis of 10% sulfuric acid, calcium carbonate and after just can obtain glucose solution.The a large amount of sulfuric acid of this process need consumption and calcium carbonate reclaim the residual sugar in solution, and need further to process purifying collection glucose.The implementation Process difficulties such as in addition, sulfuric acid has strong oxidizing property and strongly-acid, concentrated, purification.
Chinese patent CN102690899A discloses the method that strong phosphoric acid hydrolysis of lignocellulose is refined sugar and reclaimed phosphoric acid.First Mierocrystalline cellulose becomes soluble sugar through strong phosphoric acid catalytic hydrolysis, adds subsequently organic reagent by sugared precipitate and separate.The technology implementation condition that this patent is reported for work is harsher, requires sepn process to adopt to be slightly soluble in the organic reagent of water and control phosphorus acid content in solution to be greater than 65%.In addition, in soluble sugar molecular structure, contain great amount of hydroxy group, in water and phosphoric acid, solubleness is large, and the method also comprises the concentrated removal process of follow-up sugar.
In addition, in the soluble sugar that phosphoric acid catalyzed cellulose hydrolysis obtains, polysaccharide is main, and monose is less.Sun Xiaofeng seminar has reported that Mierocrystalline cellulose strong phosphoric acid fast hydrolyzing under microwave action prepares the experimental technique of reducing sugar [Wang Guangzheng, Sun Xiaofeng etc., the fast hydrolyzing of Mierocrystalline cellulose in phosphoric acid under microwave condition, Chinese sizing agent, 2012,7(21) 19-23.].Although concentrated acid is hydrocellulose effectively, do not provide the separation method of strong phosphoric acid and reducing sugar.Because reducing sugar solubleness in strong phosphoric acid is large, in prior art, be difficult to carry out sugar and separate with the effective of acid, the report of the isolation technique of not also being correlated with, the acid recovery process of bringing is thus also very complicated.Therefore, this reports that disclosed technology is not suitable for following large-scale production, does not possess the feature of creative invention technology yet.
Dilute acid hydrolysis refers generally to working concentration, and to be less than 10% mineral acid or organic acid be that catalyzer is by the method for cellulose hydrolysis saccharogenesis.Due to Mierocrystalline cellulose highly crystalline, steady chemical structure often need to (>200 ° of C) could realize when dilute acid hydrolysis under hot conditions.The research of having reported explicitly points out, and side reaction easily occurs the glucose that under hot conditions, rare catalytic hydrolysis obtains in hydrolytic process simultaneously, causes the productive rate of glucose low and poor selectivity (Jeong et al.Renew.Energ.2012,42,207-211; Xiang et al.2004, Appl.Biochem.Biotech.115 (1-3), 1127-1138.).
To sum up, the technical bottleneck that cellulose hydrolysis is prepared glucose is how economical, hydrocellulose and simple and effective separation and purification glucose efficiently, key technical problem is wherein the decomposition that how suppresses glucose when catalyse cellulose effectively hydrolyzing, ensures productive rate and the selectivity of glucose.
Summary of the invention
The object of the present invention is to provide a kind of, method that highly selective hydrocellulose prepare high purity glucose efficient through gentle simple and convenient process.
For achieving the above object, first the present invention improves its hydrolysis reaction activity by phosphoric acid pretreatment of fiber element, then under microwave heating, make Mierocrystalline cellulose under low temperature, low acid concentration condition fast, highly selective is converted into glucose, and obtains high purity glucose by simple separation.Specifically take following technical scheme:
Microwave heating hydrocellulose is prepared a method for glucose, comprises the steps:
(1) it is 5～30% solution that the phosphoric acid that cellulosic material is dissolved in to 81wt%～85wt% obtains quality percentage composition, under 40～60 ° of C, after pre-treatment 10～180min, adds organic reagent, filters, washing obtains Mierocrystalline cellulose after treatment;
(2) Mierocrystalline cellulose after treatment, through 800～1200W microwave heating, carries out diluted acid catalytic hydrolysis at 120～160 ° of C;
(3) sugar soln that step (2) obtains obtains glucose solids through neutralization, desalination, decolouring, sedimentation.
Mierocrystalline cellulose is a kind of polyhydroxylated polymer, has stronger polarity, only exceedes in the phosphoric acid of 80wt% and can occur significantly interact and fully dissolve with the polar functional group of phosphoric acid in concentration.The Mierocrystalline cellulose that is dissolved in phosphoric acid can, by partially catalyzed generation chain rupture under 40～60 ° of C, form the Mierocrystalline cellulose oligopolymer similar to cellulosic structure.In this process, must reduce the concentration of phosphoric acid as far as possible, in order to avoid cellulose chain fracture is excessively, cause Precipitation separation difficulty, through preferably determining that phosphoric acid concentration is 81wt%～85wt%.After phosphoric acid is processed, add polar organic solvent at Mierocrystalline cellulose, because the effect of polar solvent and phosphoric acid is better than the effect of Mierocrystalline cellulose oligopolymer and phosphoric acid, make Mierocrystalline cellulose oligopolymer be easy to from phosphoric acid, precipitate and separate.In addition, the Mierocrystalline cellulose oligopolymer being obtained by precipitate and separate, in its crystalline texture and settling process, the viscosity of solution is closely related: when low viscosity that and if only if, in solution, the extension degree of cellulose molecular chain is high, interchain entanglement is few, form unbodied Mierocrystalline cellulose oligopolymer, therefore, in preferred solution, Mierocrystalline cellulose percentage composition is 5～30%, both can avoid excessive being unfavorable for of Mierocrystalline cellulose phosphoric acid dissolution process viscosity to decrystallize, can avoid again processing rear cellulose solution viscosity too low and affect productive rate.
For ensureing effective precipitate and separate of Mierocrystalline cellulose oligopolymer and the efficient recovery of phosphoric acid, as preferably, the organic solvent in step (1) is C1～C8 alcohol, and the volume ratio of organic solvent and phosphoric acid is 1～5:1.
Further preferably, described organic solvent is methyl alcohol, ethanol, propyl alcohol, propyl carbinol or isopropylcarbinol.
Linked the linear natural high moleculer eompound forming by β-Isosorbide-5-Nitrae glycosidic link by glucose unit due to Mierocrystalline cellulose oligopolymer, and glycosidic link hydrogen ion (H in solution
+) effect under rupture, finally form glucose.In this process, too much hydrogen ion will be induced glucose generation side reaction, also just reduce productive rate and the selectivity of glucose.Therefore, as preferably, in step (2), the concentration of diluted acid is 0.005～0.05mol/L, and the quality of dilute acid soln is 1～100 times of Mierocrystalline cellulose quality after treatment.
As preferably, described diluted acid is made into by one or more mixing in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, formic acid, toxilic acid, tosic acid, citric acid.Preferred several acid is all strong protonic acid, has the very strong hydrogen ion ability of dissociating, and only needs lower acid concentration can meet the requirement of required hydrogen ion concentration, is also conducive to separating of product glucose and acid catalyst in solution.
Cellulosic acid-catalyzed hydrolysis is the fracture that proton attack glycosidic link causes glycosidic link, and hydrolysis rate and protonic acid concentration are closely related.Because general fibre element material crystal degree is high, the effective collision probability of protonic acid and cellulose sugar glycosidic bond is too low, conventionally the carrying out that dilute acid hydrolysis Mierocrystalline cellulose often carrys out intensified response by high temperature or high acid concentration can not be realized effectively hydrolysis and be produced glucose under low temperature, low acid concentration.Though but use high temperature, high acid concentration can realize cellulosic effective hydrolysis, and inevitably cause the decomposition of product glucose, greatly reduce productive rate and the selectivity of glucose.
The fiber method for hydrolysis that the present invention builds, obtain unbodied Mierocrystalline cellulose oligopolymer by phosphoric acid pretreatment of fiber element, greatly promote infiltration and the motion of proton in cellulosic matrix, improve the effective collision probability between hydrogen ion and glycosidic link, having reduced the difficulty of follow-up hydrolysis, is the steps necessary that realizes glucose high yield, highly selective conversion.And step (2), by microwave heating technique, has realized the utilization to hydrogen ion catalysis efficiency in the short period of time, when having reduced sour consumption, avoid the side reaction of glucose to decompose.
Microwave is as a kind of heating technique, and its heating is highly sensitive, and heating finishes rear without thermal hysteresis; And rate of heating is fast, homogeneous heating, whole reaction system is heating simultaneously under microwave action, does not have thermograde, thereby has suppressed to a certain extent the generation of side reaction.Due to the type of heating of microwave uniqueness, in reaction, can greatly improve speed of reaction, reduce the time of hydrolysis, as preferably, in step (2), the time of diluted acid catalytic hydrolysis is 1～15min.
The sugar soln obtaining through catalytic hydrolysis can obtain high purity glucose solids through purge processes such as neutralization, desalination, decolouring, sedimentations.As: gained sugar soln is neutralized and is removed acid catalyst by calcium carbonate, after drying with dissolve with ethanol glucose and remove by filter due to the not dissolved salt that adds calcium carbonate to produce, ethanol liquid glucose reclaims ethanol by underpressure distillation after activated carbon decolorizing, and gained solid obtains high purity glucose solids through water/acetone precipitation again.As preferably, after neutralization, drying temperature is 55～70 ° of C; Activated carbon decolorizing temperature is 65～80 ° of C, and activated carbon dosage is 1～3wt% of ethanol liquid glucose, and bleaching time is 5～10min; In water/acetone settling process of glucose, the consumption of water is glucose solids 1～1.5 times, acetone consumption is water 15～30 times, can obtain highly purified glucose through above-mentioned subsequent disposal.
Cellulosic dilute acid hydrolysis process is an out-phase reaction system, and hydrolysis efficiency and mass transfer process are closely related.In the time of microwave electric field polarization reactant molecule, the electric field energy of microwave is absorbed and is converted into interior energy by system, when microwave frequency is 2450MHz, and molecular polarization → be converted into the direction of an electric field arrangement → system configurational entropy decline → electric field process generation 2.45 × 10 per second of interior energy
9inferior, system temperature rises rapidly, and the reaction entropy of activation in this process increases, and it is large that effective collision probability becomes, and makes reaction rate accelerates.In addition, under microwave electric field effect, electric field exerts an influence to cellulose sugar glycosidic bond, promotes the fracture of glycosidic link, thereby realize, Mierocrystalline cellulose is efficient, highly selective is converted into glucose.
The invention has the advantages that, under microwave heating condition, realize under the catalysis of Mierocrystalline cellulose diluted acid efficient, highly selective hydrolysis and prepare glucose, this technology has the advantages such as speed of reaction is fast, selectivity is high, reaction conditions is gentle; And operating process is simple, energy consumption is low, sour consumption is few, glucose productive rate and selectivity high, can obtain high purity glucose solids by simple separation.
Brief description of the drawings
Fig. 1 is the schema that microwave heating hydrocellulose of the present invention is prepared glucose;
Fig. 2 is the glucose shape appearance figure that the present invention prepares;
Fig. 3 is the infrared spectrum of the glucose for preparing of the present invention;
Fig. 4 is the nuclear magnetic spectrogram (hydrogen spectrum) of the glucose for preparing of the present invention;
Fig. 5 is the nuclear magnetic spectrogram (charcoal spectrum) of the glucose for preparing of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, it is pointed out that following examples are intended to be convenient to the understanding of the present invention, and it is not played to any restriction effect.
Embodiment 1
Utilize microwave heating effectively hydrolyzing Mierocrystalline cellulose to prepare high purity glucose according to the flow process shown in Fig. 1, concrete steps are:
2.0g Mierocrystalline cellulose is dissolved in after 18g85wt% phosphoric acid, under 50 ° of C, after stir process 60min, adds 40mL ethanol, after filtration, washing, obtain cellulose solids after treatment after dry.Get 0.5g Mierocrystalline cellulose after treatment and mix with 10g0.04mol/L sulfuric acid, select microwave heating to the 160 ° C of 800W, insulation 5min.After temperature is down to room temperature, centrifugation obtains sugar aqueous solution.Calculating transformation efficiency according to quality change before and after fibrin reaction is 90.5%, and detecting glucose productive rate by high-efficient liquid phase chromatogram HPLC is 72.6%, and its selectivity is 80.2%.Gained sugar aqueous solution is neutralized and is removed sulfuric acid by calcium carbonate, and under 65 ° of C, evaporation obtains solid, by dissolve with ethanol glucose separated salt; Ethanol sugar soln adds 2wt% gac subsequently, and 70 ° of C decolouring 5min, repeat 1～2 time; Underpressure distillation ethanol and glucose under 40 ° of C, add water dissolution sugar by solid-to-liquid ratio 1:1, adds subsequently 20 times of volume acetone by the sedimentation of glucose sugar, filters, dryly obtains glucose solids, as shown in Figure 2.
Embodiment 2
Utilize microwave heating effectively hydrolyzing Mierocrystalline cellulose to prepare high purity glucose according to the flow process shown in Fig. 1, concrete steps are:
2.0g Mierocrystalline cellulose is dissolved in after 18g83.5wt% phosphoric acid, under 50 ° of C, after stir process 120min, adds 40mL ethanol, after filtration, washing, obtain cellulose solids after treatment after dry.Get 0.5g Mierocrystalline cellulose after treatment and mix with 10g0.04mol/L sulfuric acid, select microwave heating to the 160 ° C of 1200W, insulation 5min.After temperature is down to room temperature, centrifugation obtains sugar aqueous solution.Calculating transformation efficiency according to quality change before and after fibrin reaction is 93.5%, and detecting glucose productive rate by high-efficient liquid phase chromatogram HPLC is 78.9%, and its selectivity is 84.4%.Gained sugar aqueous solution is neutralized and is removed sulfuric acid by calcium carbonate, and under 65 ° of C, evaporation obtains solid, by dissolve with ethanol glucose separated salt; Ethanol sugar soln adds 2wt% gac subsequently, and 70 ° of C decolouring 5min, repeat 1～2 time; Underpressure distillation ethanol and glucose under 40 ° of C, add water dissolution sugar by solid-to-liquid ratio 1:1, adds subsequently 20 times of volume acetone by the sedimentation of glucose sugar, filtration, the dry high purity glucose solids that obtains.
Embodiment 3
Utilize microwave heating effectively hydrolyzing Mierocrystalline cellulose to prepare high purity glucose according to the flow process shown in Fig. 1, concrete steps are:
1.0g Mierocrystalline cellulose is dissolved in after 19g85wt% phosphoric acid, under 50 ° of C, after stir process 30min, adds 40mL ethanol, after filtration, washing, obtain cellulose solids after treatment after dry.Get 0.5g Mierocrystalline cellulose after treatment and mix with 10g0.04mol/L sulfuric acid, select microwave heating to the 140 ° C of 1200W, insulation 5min.After temperature is down to room temperature, centrifugation obtains sugar aqueous solution.Calculating transformation efficiency according to quality change before and after fibrin reaction is 91.3%, and detecting glucose productive rate by high-efficient liquid phase chromatogram HPLC is 74.2%, and its selectivity is 81.3%.Gained sugar aqueous solution is neutralized and is removed sulfuric acid by calcium carbonate, and under 65 ° of C, evaporation obtains solid, by dissolve with ethanol glucose separated salt; Ethanol sugar soln adds 2wt% gac subsequently, and 70 ° of C decolouring 5min, repeat 1～2 time; Underpressure distillation ethanol and glucose under 40 ° of C, add water dissolution sugar by solid-to-liquid ratio 1:1, adds subsequently 20 times of volume acetone by the sedimentation of glucose sugar, filtration, the dry high purity glucose solids that obtains.
Embodiment 4
Utilize microwave heating effectively hydrolyzing Mierocrystalline cellulose to prepare high purity glucose according to the flow process shown in Fig. 1, concrete steps are:
2.0g Mierocrystalline cellulose is dissolved in after 18g85wt% phosphoric acid, under 50 ° of C, after stir process 180min, adds 40mL ethanol, after filtration, washing, obtain cellulose solids after treatment after dry.Get 0.5g Mierocrystalline cellulose after treatment and mix with 10g0.02mol/L sulfuric acid, select microwave heating to the 160 ° C of 1200W, insulation 10min.After temperature is down to room temperature, centrifugation obtains sugar aqueous solution.Calculating transformation efficiency according to quality change before and after fibrin reaction is 92.6%, and detecting glucose productive rate by high-efficient liquid phase chromatogram HPLC is 77.8%, and its selectivity is 84.2%.Gained sugar aqueous solution is neutralized and is removed sulfuric acid by calcium carbonate, and under 65 ° of C, evaporation obtains solid, by dissolve with ethanol glucose separated salt; Ethanol sugar soln adds 2wt% gac subsequently, and 70 ° of C decolouring 5min, repeat 1～2 time; Underpressure distillation ethanol and glucose under 40 ° of C, add water dissolution sugar by solid-to-liquid ratio 1:1, adds subsequently 20 times of volume acetone by the sedimentation of glucose sugar, filtration, the dry high purity glucose solids that obtains.
Embodiment 5
Utilize microwave heating effectively hydrolyzing Mierocrystalline cellulose to prepare high purity glucose according to the flow process shown in Fig. 1, concrete steps are:
1.5g Mierocrystalline cellulose is dissolved in after 18.5g81wt% phosphoric acid, under 50 ° of C, after stir process 150min, adds 40mL ethanol, after filtration, washing, obtain cellulose solids after treatment after dry.Get 0.5g Mierocrystalline cellulose after treatment and 10g0.02mol/L mixed in hydrochloric acid, select microwave heating to the 160 ° C of 1000W, insulation 2min.After temperature is down to room temperature, centrifugation obtains sugar aqueous solution.Calculating transformation efficiency according to quality change before and after fibrin reaction is 91.3%, and detecting glucose productive rate by high-efficient liquid phase chromatogram HPLC is 80.2%, and its selectivity is 87.8%.Gained sugar aqueous solution is neutralized and is removed sulfuric acid by calcium carbonate, and under 65 ° of C, evaporation obtains solid, by dissolve with ethanol glucose separated salt; Ethanol sugar soln adds 2wt% gac subsequently, and 70 ° of C decolouring 5min, repeat 1～2 time; Underpressure distillation ethanol and glucose under 40 ° of C, add water dissolution sugar by solid-to-liquid ratio 1:1, adds subsequently 20 times of volume acetone by the sedimentation of glucose sugar, filtration, the dry high purity glucose solids that obtains.
Fig. 2 is the glucose that separation and purification obtains, and the Infrared Characterization of Fig. 3 shows that spectrogram absorption peak is consistent with glucose standard specimen, does not find 1740cm
-1the ester bond structure at place, illustrates acidic impurities such as not finding formic acid, levulinic acid, gluconic acid.The nuclear magnetic spectrum of Fig. 4 and Fig. 5 further confirmed that gained glucose structure is the mixture of α and two kinds of configurations of β, and there is no obvious impurity peaks.
Claims (2)
1. microwave heating hydrocellulose is prepared a method for glucose, it is characterized in that, comprises the steps:
(1) it is 5～30% solution that the phosphoric acid that cellulosic material is dissolved in to 81wt%～85wt% obtains quality percentage composition, at 40～60 DEG C, after pre-treatment 10～180min, adds organic solvent, filters, washing obtains Mierocrystalline cellulose after treatment;
Described organic solvent is C1～C8 alcohol, and the volume ratio of organic solvent and phosphoric acid is 1～5:1;
(2) Mierocrystalline cellulose after treatment, through 800～1200W microwave heating, carries out diluted acid catalytic hydrolysis at 120～160 DEG C;
Described diluted acid is made into by one or more mixing in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, formic acid, toxilic acid, tosic acid, citric acid;
The concentration of described diluted acid is 0.005～0.05mol/L, and the quality of dilute acid soln is 1～100 times of Mierocrystalline cellulose quality after treatment;
The time of described diluted acid catalytic hydrolysis is 1～15min;
(3) sugar soln that step (2) obtains obtains glucose solids through neutralization, desalination, decolouring, sedimentation.
2. microwave heating hydrocellulose according to claim 1 is prepared the method for glucose, it is characterized in that, described organic solvent is methyl alcohol, ethanol, propyl alcohol, propyl carbinol or isopropylcarbinol.
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| CN104141016B (en) * | 2013-05-09 | 2016-04-13 | 中国科学院宁波材料技术与工程研究所 | A kind of cellulosic photochemical catalysis free radical cracking method |
| CN103981295B (en) * | 2014-06-06 | 2017-03-08 | 台州学院 | A kind of method preparing xylose and glucose using Caulis Zizaniae caduciflorae garbage |
| CN108251568A (en) * | 2018-01-10 | 2018-07-06 | 中国科学院宁波材料技术与工程研究所 | A kind of method of the microwave-driven effectively hydrolyzing cellulose with synchronous cooling |
| CN110346457A (en) * | 2018-04-04 | 2019-10-18 | 青岛大学附属医院 | A kind of detection method using monosaccharide composition in acid hydrolysis of microwave and anion-exchange chromatography-pulsed amperometric method analysis polysaccharide |
| CN109321688B (en) * | 2018-09-28 | 2022-05-17 | 中国科学院宁波材料技术与工程研究所 | Process for preparing water-soluble sugar |
| CN109289871A (en) * | 2018-10-31 | 2019-02-01 | 湖南师范大学 | A kind of preparation method of the carbon-based solid super-strong acid of biomass with classification duct |
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