CN119332030A - A method for preparing bamboo biomass sugar - Google Patents
A method for preparing bamboo biomass sugar Download PDFInfo
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- CN119332030A CN119332030A CN202411367692.3A CN202411367692A CN119332030A CN 119332030 A CN119332030 A CN 119332030A CN 202411367692 A CN202411367692 A CN 202411367692A CN 119332030 A CN119332030 A CN 119332030A
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- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 131
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 131
- 241001330002 Bambuseae Species 0.000 title claims abstract description 131
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 131
- 239000011425 bamboo Substances 0.000 title claims abstract description 131
- 235000000346 sugar Nutrition 0.000 title claims abstract description 96
- 239000002028 Biomass Substances 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 18
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims abstract description 62
- 239000002994 raw material Substances 0.000 claims abstract description 36
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims abstract description 31
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 31
- 238000002360 preparation method Methods 0.000 claims abstract description 24
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 17
- 238000013375 chromatographic separation Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 145
- 239000000243 solution Substances 0.000 claims description 54
- 238000006460 hydrolysis reaction Methods 0.000 claims description 53
- 230000007062 hydrolysis Effects 0.000 claims description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 36
- 239000012528 membrane Substances 0.000 claims description 35
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 claims description 33
- 238000005086 pumping Methods 0.000 claims description 29
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000006188 syrup Substances 0.000 claims description 22
- 235000020357 syrup Nutrition 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000011084 recovery Methods 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 17
- 238000005342 ion exchange Methods 0.000 claims description 16
- 239000000413 hydrolysate Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005341 cation exchange Methods 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 8
- 238000001728 nano-filtration Methods 0.000 claims description 8
- 239000012466 permeate Substances 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 238000005349 anion exchange Methods 0.000 claims description 7
- 235000008504 concentrate Nutrition 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 238000010612 desalination reaction Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000011033 desalting Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229920000875 Dissolving pulp Polymers 0.000 abstract description 3
- 230000004888 barrier function Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 150000008163 sugars Chemical class 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- -1 salt ions Chemical class 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
- B01D15/1814—Recycling of the fraction to be distributed
- B01D15/1821—Simulated moving beds
- B01D15/1828—Simulated moving beds characterised by process features
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/02—Column or bed processes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Biochemistry (AREA)
- Saccharide Compounds (AREA)
Abstract
本申请涉及一种竹材生物质糖的制备方法，所述竹材生物质糖的制备方法，克服了现有技术中竹材半纤维素未能得到充分利用的缺陷，以竹材为原料，经过备料、预处理后，经糖份提取步骤水解竹原料中半纤维素，后依次经过中和、浓缩净化、再浓缩和色谱分离七个步骤，高效制备得到竹材生物质糖液，其包含5%‑50%的低聚木糖和30%‑70%的木糖，且两组分的纯度均在90%以上。此外，所述竹材生物质糖的制备方法，提取生物质糖后的竹材可用于溶解浆和绒毛浆的生产，能产生更多附加值，对提升竹资源综合价值更有意义，为生物质糖开辟出一条全新的制备路径，同时打破了竹材低价值利用的壁垒。The present application relates to a method for preparing bamboo biomass sugar, which overcomes the defect that bamboo hemicellulose has not been fully utilized in the prior art. Bamboo is used as raw material. After material preparation and pretreatment, the hemicellulose in the bamboo raw material is hydrolyzed through a sugar extraction step, and then the bamboo biomass sugar solution is efficiently prepared through seven steps of neutralization, concentration and purification, reconcentration and chromatographic separation. It contains 5%-50% of oligoxylose and 30%-70% of xylose, and the purity of the two components is above 90%. In addition, the method for preparing bamboo biomass sugar, the bamboo after extracting biomass sugar can be used for the production of dissolving pulp and fluff pulp, which can generate more added value, is more meaningful for improving the comprehensive value of bamboo resources, and opens up a new preparation path for biomass sugar, while breaking the barrier of low-value utilization of bamboo.
Description
Technical Field
The application relates to the field of biomass sugar preparation, in particular to a preparation method of bamboo biomass sugar.
Background
Biomass is the only renewable carbon resource in nature, biomass sugar is an inexpensive and easily available chemical raw material, and comprises cellulose and hemicellulose in woody biomass, derived sugars such as starch, xylose, fructose, glucose and sucrose, and the derived sugars are further converted into energy sources (fuel ethanol, biodiesel, hydrogen and the like) and chemical platform chemicals (organic acids, organic alcohols, esters and the like), so that the biomass resource is an ideal way for high-efficiency utilization.
The plant hemicellulose extract in the market is basically used for producing xylose, xylitol or xylooligosaccharide, mainly takes corncob and bagasse as raw materials, and has mature industrial production technology and market. The bamboo resource is used as an important raw material in the pulping and papermaking field, cellulose and lignin in the bamboo resource are well applied, but hemicellulose is not well applied, and basically is burnt along with black liquor, so that good economic value cannot be generated.
Hemicellulose hydrolysate in bamboo wood contains xylose and xylooligosaccharide, and is a high-added-value product, and is an important component of biomass sugar in bamboo wood, so that development of a method for preparing biomass sugar by adopting hemicellulose in bamboo wood is imperative.
Disclosure of Invention
In view of the defects in the prior art, the application provides a method for preparing biomass sugar by taking bamboo as a raw material, which develops a new way for obtaining biomass sugar and improves the comprehensive utilization value of bamboo resources.
The application provides a preparation method of bamboo biomass sugar, which comprises the following steps:
(1) Preparing materials, namely slicing or/and preparing bamboo chips and bamboo powder, and washing the bamboo chips and the bamboo powder to obtain bamboo raw materials;
(2) Pretreatment, namely adding a pretreatment medium into the bamboo raw material for pretreatment;
The pretreatment medium contains 0.05 to 0.12 percent of sulfuric acid, and is pretreated for 0.5 to 2 hours;
(3) Sugar extraction:
3a, adding a hydrolysis medium into the pretreated bamboo raw material to enable hemicellulose in the bamboo raw material to undergo hydrolysis reaction, and cooling and discharging hydrolysis liquid after the reaction;
the hydrolysis medium is sulfuric acid with the concentration of 0.5% -3%, the hydrolysis temperature is 100-120 ℃, and the hydrolysis is carried out for 1-4 hours;
3b, adding water to circularly wash reaction residues to obtain sugar recovery liquid;
3c, mixing the hydrolysate with the sugar recovery liquid according to the ratio of 1:1-1:2 to obtain a mixed liquid;
(4) And (3) neutralization:
Slowly adding calcium carbonate slurry into the mixed solution under the stirring condition for neutralization reaction, wherein the reaction temperature is 75-85 ℃ and the reaction time is 0.5-1 hour, so as to obtain a neutralization solution;
4b, carrying out solid-liquid separation on the neutralization solution, and filtering out calcium sulfate crystal salt to obtain clear liquid;
(5) Concentrating and purifying:
pumping the clear liquid into a filter membrane device for desalination and concentration to obtain concentrated liquid;
5b, adding active carbon into the concentrated solution under the stirring condition for decoloring, heating to 70-80 ℃, and preserving heat for 0.5-1 hour;
5c, carrying out solid-liquid separation on the decolored concentrated solution, and filtering out activated carbon mud powder to obtain decolored solution;
pumping the decolorized liquid into an ion exchange column for ion exchange purification to obtain bamboo biomass sugar liquor;
(6) Concentrating the bamboo biomass sugar solution to 55% -65% to obtain concentrated syrup;
(7) Separating the concentrated syrup by adopting continuous chromatographic separation equipment to obtain xylooligosaccharide liquid with the concentration of 30-50 percent and xylose liquid.
As a further improvement to the scheme, the preparation method further comprises the steps of respectively concentrating the xylooligosaccharide liquid and the xylose liquid, and respectively pumping the concentrated xylooligosaccharide liquid and xylose liquid into a spray dryer for drying by a high-pressure pump to obtain powdery xylooligosaccharide and powdery xylose.
As a further improvement to the above scheme, the hydrolysate vapors resulting from the hydrolysis reaction in step 3a are sent to a spray condenser for condensation, and the resulting condensate is used for the recycle washing of the reaction residues in step 3 b.
As a further improvement to the above scheme, in step 4a, the pH of the neutralization solution is controlled to be 3.5-4;
Or in the step 5b, the dosage of the activated carbon is controlled to be 10% -30% of the total solid content.
As a further improvement to the above scheme, after step 5c, the decolorized liquid is pumped into a filtration membrane device for desalting and concentrating.
As a further improvement on the scheme, the filter membrane equipment adopts a ceramic nanofiltration membrane, and the molecular weight cut-off value of the filter membrane is 150-200Da.
As a further improvement to the above, in step 5d, the ion exchange column comprises at least one cation exchange column and at least one anion exchange column.
As a further improvement to the above, step (6) includes:
6a, pumping the bamboo biomass sugar liquid into a filter membrane device for concentration to obtain bamboo biomass sugar concentrated liquid with the concentration of 20% -22%;
And 6b, pumping the bamboo biomass sugar concentrate into a plate evaporator for concentrating to 55% -65% to obtain the concentrated syrup.
As a further improvement to the scheme, the permeate liquid in the step 5a and the permeate liquid in the step 6a and the evaporated condensate water in the step 6b are sent into a pretreatment medium tank for pretreatment of the bamboo raw material in the step (2).
As a further improvement to the above scheme, in step (7), the concentrated syrup is separated by using an SSMB sequential simulated moving bed.
Compared with the prior art, the preparation method of the bamboo biomass sugar overcomes the defect that bamboo hemicellulose cannot be fully utilized in the prior art, takes bamboo as a raw material, hydrolyzes the hemicellulose in the bamboo raw material through sugar extraction steps after material preparation and pretreatment, and then sequentially carries out seven steps of neutralization, concentration purification, re-concentration and chromatographic separation to efficiently prepare the bamboo biomass sugar solution, wherein the bamboo biomass sugar solution contains 5% -50% of xylooligosaccharide and 30% -70% of xylose, and the purity of the two components is more than 90%.
Detailed Description
The present application is described in detail below so that advantages and features of the present application can be more easily understood by those skilled in the art, thereby making clear and unambiguous the scope of the present application.
The application provides a preparation method of bamboo biomass sugar, which aims to solve the problem that bamboo hemicellulose cannot be fully utilized in the prior art, improve the comprehensive utilization value of bamboo resources and open up a brand-new preparation path for biomass sugar.
The preparation method of the bamboo biomass sugar comprises the following steps:
(1) Preparing bamboo chips and powder, and washing with water to obtain bamboo material.
Specifically, bamboo is processed into bamboo chips with the length of 3-5cm and the width of 1-2cm from raw bamboo or into bamboo scraps and bamboo powder with smaller sizes, and the bamboo scraps and the bamboo powder are washed by at least two serially connected washing machines to remove impurities.
The cleaning water for washing the bamboo raw materials is recovered, purified and reused.
(2) Pretreatment, namely conveying the bamboo raw materials cleaned by the washing machine into a hydrolysis reaction tank through spiral conveying, and adding a pretreatment medium into the bamboo raw materials for pretreatment.
Wherein the pretreatment medium contains 0.05% -0.12% sulfuric acid, so that the pretreatment medium completely infiltrates the bamboo raw material, and the pretreatment is performed for 0.5-2 hours.
After pretreatment is finished, pumping the pretreatment liquid to a pretreatment liquid tank, and adjusting pH value, and then, entering middle-section water for purification and reuse.
Furthermore, the hydrolysis reaction tank can be provided with 1 group or more than 2 groups. And a plurality of groups of hydrolysis reaction tanks are used for hydrolysis simultaneously, so that the productivity is improved, and the production efficiency is improved.
(3) Sugar extraction:
and 3a, adding a hydrolysis medium into the bamboo raw material pretreated in the hydrolysis reaction tank, so that the bamboo raw material is completely soaked by the hydrolysis medium, and hemicellulose in the bamboo raw material undergoes hydrolysis reaction.
Wherein the solid-liquid volume ratio is 1:2-1:4, the hydrolysis medium is 0.5% -3% sulfuric acid, the hydrolysis temperature is 100-120 ℃, and the hydrolysis is carried out for 1-4 hours.
And cooling the reacted hydrolysate, and then discharging the cooled hydrolysate to a hydrolysate tank, specifically, cooling the hydrolysate to 70-80 ℃ through heat exchange, and then discharging the hydrolysate to the hydrolysate tank.
And 3b, adding water to circularly wash the reaction residues to obtain a sugar recovery liquid, and pumping the sugar recovery liquid into a sugar recovery liquid tank.
In this step, the volume of the circulating washing water is controlled to be 4-8 times the volume of the solid matter.
In the step 3a, the hydrolysate vapor generated by the hydrolysis reaction is introduced into a spray condenser to be condensed, and the generated condensate is introduced into a sugar recovery medium tank for circularly washing reaction residues in the step so as to collect as much sugar generated by the hydrolysis reaction as possible.
And 3c, mixing the hydrolysate with the sugar recovery liquid in a mass ratio of 1:1-1:2 in a combined hydrolysate tank to obtain a mixed liquid.
In the pretreatment step and the sugar extraction step, the pretreatment liquid, the hydrolysis liquid and the sugar recovery liquid are respectively recovered/collected, and all the liquid sections do not cross, so that the stable quality of products in all the subsequent steps is ensured.
(4) And (3) neutralization:
Pumping the mixed solution in the combined hydrolysis liquid tank to a neutralization tank, slowly adding calcium carbonate slurry into the mixed solution under the stirring condition for neutralization reaction, wherein the reaction temperature is 75-85 ℃ and the reaction time is 0.5-1 hour, and obtaining the neutralization solution.
Further, in the step, steam is introduced into the neutralization tank to raise the temperature to 75-85 ℃.
In this step, the pH of the neutralization solution is controlled to 3.5 to 4.
And 4b, pumping the neutralization liquid into a plate-frame filter for solid-liquid separation, filtering out calcium sulfate crystal salt to obtain clear liquid, and delivering the clear liquid into a first-stage neutralization liquid tank.
Furthermore, the plate-and-frame filter is a closed plate-and-frame filter, so that vapor emission in the solid-liquid separation process is prevented, clear liquid is protected from being polluted, and the production cleanliness is improved.
(5) Concentrating and purifying:
and 5a, pumping the clear liquid from the first-stage neutralization liquid tank into a filter membrane device for desalination and concentration to obtain concentrated liquid, and sending the concentrated liquid into a second-stage neutralization liquid tank and sending the permeate liquid into a pretreatment medium tank.
Wherein the pretreatment medium tank is used for storing the pretreatment medium and is used in the pretreatment working section of the bamboo raw materials.
Furthermore, the filter membrane equipment adopts a ceramic nanofiltration membrane so as to overcome the defect that the clear liquid needs to be cooled to below 50 ℃ when a conventional synthetic material membrane is adopted, and improve the concentration efficiency of the clear liquid.
Further, the molecular weight cut-off value of the filter membrane is 150-200Da, so that impurities such as salts with molecular weight below the range in the clear liquid are discharged along with the permeate.
Wherein, the molecular weight cut-off value refers to the lower limit of molecular weight of molecules which can be completely cut off in the filtration process of the filter membrane, and the molecular weight cut-off value is usually expressed in Da (Dalton).
Pumping the concentrated solution from the two-stage neutralization liquid tank into a decoloring tank, adding active carbon into the concentrated solution under the stirring condition for decoloring, introducing steam, heating to 70-80 ℃, and preserving heat for 0.5-1 hour;
Further, in the step, steam is introduced into the decoloring tank to raise the temperature to 70-80 ℃.
Furthermore, the activated carbon is wet powdery activated carbon or slurry activated carbon, and compared with solid activated carbon, the contact area of the activated carbon with the concentrated solution is increased, so that the decoloring efficiency and the decoloring effect are improved.
Further, the dosage of the activated carbon is controlled to be 10% -30% of the total solid content.
And 5c, pumping the decolored mixture into a plate-and-frame filter for solid-liquid separation, filtering out activated carbon mud powder, and delivering the decolored liquid into a decolored liquid tank.
Furthermore, the plate-and-frame filter is a closed plate-and-frame filter, so that vapor emission in the solid-liquid separation process is prevented, decolorized liquid is prevented from being polluted, and the production cleanliness is improved.
Further, the transmissivity of the decolorized solution after solid-liquid separation is controlled to be more than 80%, and the activated carbon mud powder is reused for secondary recycling and then sent to a boiler for combustion and recycling.
In one embodiment, the preparation method of the bamboo biomass sugar further comprises the step of pumping the decolorized solution from the decolorized solution tank into a filter membrane device for desalting and concentrating, so as to further reduce the load for the subsequent stage of ion exchange purification process.
In this embodiment, the permeate of the decolorized solution after desalting and concentrating is fed to the pretreatment medium tank.
Furthermore, the filter membrane equipment adopts a ceramic nanofiltration membrane with a molecular weight cutoff value of 150-200Da, so that salt impurities in the decolorized solution are further filtered, the concentration of the decolorized solution is improved, the defect that the decolorized solution needs to be cooled to be below 50 ℃ by adopting a conventional synthetic material membrane is overcome by the ceramic nanofiltration membrane, and the concentration efficiency of the decolorized solution is improved.
And 5d, pumping the decolorized liquid into an ion exchange column for ion exchange purification to obtain bamboo biomass sugar liquid, and sending the bamboo biomass sugar liquid into a sugar liquid storage tank.
The residual gray salt plasma in the decolorized solution is removed again, and the small molecular pigment is adsorbed, so that the decolorized solution is further decolorized, and the transmittance of the bamboo biomass sugar solution reaches more than 90%.
Further, the ion exchange column includes at least one cation exchange column and at least one anion exchange column to ensure adequate removal of the different types of ions.
Further, the cation exchange column and the anion exchange column are arranged at intervals.
(6) Concentrating the bamboo biomass sugar solution to 55% -65% to obtain concentrated syrup.
Further, the re-concentration step comprises the steps of ① pumping the bamboo biomass sugar liquid into a filter membrane device for concentration to obtain bamboo biomass sugar concentrated liquid with the concentration of 20% -22%, and sending the bamboo biomass sugar concentrated liquid into a bamboo biomass sugar concentrated liquid tank.
② Pumping the bamboo biomass sugar concentrate into a plate evaporator for concentrating to 55% -65% to obtain the concentrated syrup.
Furthermore, in step ①, the permeate from the concentration step of the filter membrane device and the evaporated condensate from the plate evaporator in step ② are both fed into the pretreatment medium tank, and the bamboo raw material in step (2) is pretreated.
The filter membrane device is preferably a ceramic nanofiltration membrane, and the plate evaporator is heated by steam.
(7) Separating the concentrated syrup by adopting continuous chromatographic separation equipment to obtain xylooligosaccharide liquid with the concentration of 30-50 percent and xylose liquid.
Chromatographic separation is based on the fact that different substances have different partition coefficients in a system consisting of a stationary phase and a mobile phase, exhibiting different retention times during elution with the mobile phase, thus achieving separation.
The traditional chromatographic separation technology adopts a fixed chromatographic column to carry out, a certain amount of materials are firstly introduced, then the eluent is adopted to continuously elute, different product components can be received at the same outlet in different time periods, and the process is time-consuming and labor-consuming.
In the application, the SSMB sequential simulated moving bed is adopted to separate the concentrated syrup, so that the multi-component high-efficiency separation of biomass sugar preparation is realized, the purity of each component is high, and the preparation cost is low.
Further, the concentrated syrup obtained in the step (6) is required to be cooled to 60-70 ℃ and then is sent to an SSMB sequential simulated moving bed for chromatographic separation.
The preparation method of the bamboo biomass sugar overcomes the defect that hemicellulose of bamboo is not fully utilized in the prior art, and bamboo is used as a raw material to prepare the bamboo biomass sugar liquid with high efficiency, wherein the bamboo biomass sugar liquid contains 5-50% of xylooligosaccharide and 30-70% of xylose, and the purities of the two components are over 90%.
Wherein xylose is the main product of bamboo hemicellulose after hydrolysis, and xylooligosaccharide is the product of polymerization of 2-7 xylose molecules, both belong to white to colorless saccharides which are easily dissolved in water.
In the preparation method of the bamboo biomass sugar, the liquid concentration working procedures adopt membrane concentration, so that the steam consumption can be greatly reduced, salt ions in the liquid can be better removed, and the resin consumption is saved.
In some embodiments of the present application, the preparation method of bamboo biomass sugar further includes a step of concentrating the xylooligosaccharide liquid and the xylose liquid respectively, and a step of pumping the concentrated xylooligosaccharide liquid and xylose liquid into a spray dryer to dry respectively by a high pressure pump, so as to obtain powdery xylooligosaccharide and powdery xylose.
Further, evaporating and concentrating the xylooligosaccharide liquid and the xylose liquid by adopting a two-effect plate type evaporator to obtain xylooligosaccharide liquid and xylose liquid with the concentration of more than 85%, and respectively pumping the xylooligosaccharide liquid and the xylose liquid with the concentration of more than 85% into a spray dryer for drying by a high-pressure pump to obtain powdery xylooligosaccharide and powdery xylose.
Wherein, the plate evaporator is heated by steam.
Further, the hot air inlet temperature of the spray dryer is not more than 140 ℃ and the outlet temperature is not more than 110 ℃.
Further, the hot air fed into the spray dryer is subjected to dust and sterilization treatment through filtration treatment.
In the embodiment, the powdery xylooligosaccharide and powdery xylose are obtained by adopting a spray dryer drying method, so that the problems of low crystallization speed and difficult mother liquor treatment in a crystallization method are avoided, and the powdery bamboo biomass sugar product is directly prepared, thereby being beneficial to storage and transportation.
In some embodiments of the application, the preparation method of bamboo biomass sugar further comprises the step of injecting clean water into the hydrolysis reaction tank to continuously wash residual acid in reaction residues after the sugar recovery liquid is pumped to the sugar recovery liquid tank, and pumping the washing water to the washing liquid tank for standby, wherein the washing water can be sent to the hydrolysis medium tank for sugar recovery procedures.
The hydrolysis medium tank is used for storing hydrolysis medium, and clean water and sulfuric acid are added into the hydrolysis medium tank according to the requirement, so that the concentration of sulfuric acid in the hydrolysis medium is 0.5% -3%.
In the step, the washing water, the pretreatment liquid, the hydrolysate, the sugar recovery liquid, the permeate liquid of each concentration section and the condensed water are independently recovered/collected, and the liquids of each section are not crossed, so that the quality stability of the products of each working procedure is ensured.
Further, the pH of the reaction residue after washing is controlled to be 5-7, so that the subsequent piling and use are facilitated.
Further, after the reaction residue is washed, spraying dilution water on the peripheral wall of the hydrolysis reaction tank is started, the reaction residue is pumped to a residue bin through a special pump, and meanwhile, the filtrate is recycled as the spraying dilution water.
According to the preparation method of the bamboo biomass sugar, the total water recycling rate reaches 70%.
Yu Liaocang, the reaction residue is dehydrated and then is conveyed to a pulping workshop in a spiral way to be used as a special pulp raw material, flaky residue can be used as a production raw material of dissolving pulp and fluff pulp, and scraps or powdery residue can be dried and then is mixed with coal to be used as fuel.
In the prior art, residues after xylose or oligosaccharide is extracted by using a jade core are usually burnt by a biomass boiler, and no additional value is generated. The bamboo material after biomass sugar extraction can be used for producing dissolving pulp and fluff pulp, can generate more added values, is more significant in improving the comprehensive value of bamboo resources, and breaks the barrier of low-value utilization of the bamboo material.
The present application will be described in further detail with reference to examples. It is specifically noted that the following examples are only for illustrating the present application, but do not limit the scope of the present application. Likewise, the following examples are only some, but not all, of the examples of the present application, and all other examples, which a person of ordinary skill in the art would obtain without making any inventive effort, are within the scope of the present application.
Embodiment one:
The embodiment provides a preparation method of bamboo biomass sugar, which comprises the following steps:
s11, preparing materials, namely processing raw bamboo into bamboo chips with the length of 3-5cm and the width of 1-2cm from raw bamboo, and washing the bamboo chips with two serially connected washing machines to obtain bamboo raw materials.
S12, pretreatment is carried out by adding a pretreatment medium into the bamboo raw material.
The pretreatment medium contained 0.08% sulfuric acid, pretreated for 1 hour.
S13, extracting sugar:
Adding a hydrolysis medium into the pretreated bamboo raw material, wherein the solid-liquid volume ratio is 1:2, so that hemicellulose in the bamboo raw material undergoes hydrolysis reaction, and after 3 hours of reaction, the hydrolysis liquid is cooled to 70 ℃ through heat exchange and is discharged to a hydrolysis liquid tank.
Wherein the hydrolysis medium is 2% sulfuric acid, and the hydrolysis temperature is 110 ℃.
And sending the hydrolysate steam generated by the hydrolysis reaction into a jet condenser for condensation, and circularly washing reaction residues by the generated condensate to obtain sugar recovery liquid. In this step, the volume of the circulating washing water was controlled to be 8 times the volume of the solid matter.
Mixing the hydrolysate with the sugar recovery liquid according to the mass ratio of 1:1 to obtain a mixed liquid.
S14, neutralization:
And slowly adding calcium carbonate slurry into the mixed solution under the stirring condition to perform a neutralization reaction, wherein the reaction temperature is 80 ℃, and the reaction time is 1 hour, so as to obtain a neutralization solution.
And (3) carrying out solid-liquid separation on the neutralization solution by adopting a closed plate-and-frame filter, and filtering out calcium sulfate crystal salt to obtain clear liquid.
S15, concentrating and purifying:
a. Pumping the clear liquid into a filter membrane device for desalination and concentration to obtain concentrated solution.
The filter membrane equipment adopts a ceramic nanofiltration membrane with a molecular weight cutoff value of 200 Da.
B. Activated carbon is added into the concentrated solution under stirring for decolorization, and the temperature is raised to 80 ℃ and kept for 1 hour.
And (3) carrying out solid-liquid separation on the decolored concentrated solution by adopting a closed plate-frame filter, filtering out activated carbon mud powder to obtain decolored solution, and controlling the transmittance of the decolored solution after solid-liquid separation to be more than 80%.
C. And pumping the decolorized liquid into an ion exchange column for ion exchange purification to obtain bamboo biomass sugar liquid, wherein the transmittance of the bamboo biomass sugar liquid is more than 90%.
The ion exchange columns are provided with three groups, and the arrangement sequence is cation exchange columns, anion exchange columns and cation exchange columns.
S16, re-concentrating, namely concentrating the bamboo biomass sugar solution to 60% to obtain concentrated syrup.
Specifically, the bamboo biomass sugar solution is pumped into a filter membrane device for concentration to obtain bamboo biomass sugar concentrate with the concentration of 20% -22%, and then the bamboo biomass sugar concentrate is pumped into a plate evaporator for concentration to 60%, so that the concentrated syrup is obtained.
S17, chromatographic separation, namely cooling the concentrated syrup to 60 ℃, and then sending the cooled concentrated syrup into an SSMB sequential simulated moving bed for chromatographic separation to obtain xylooligosaccharide solution with the concentration of 50% and xylose solution with the concentration of 46%.
S18, adopting two-effect plate steaming to concentrate the xylooligosaccharide liquid and the xylose liquid to more than 85%, and respectively pumping the concentrated xylooligosaccharide liquid and xylose liquid into a spray dryer for drying by a high-pressure pump to obtain powdery xylooligosaccharide and powdery xylose.
The purity of the powdery xylo-oligosaccharide is 93 percent, and the purity of the powdery xylo-oligosaccharide is 95 percent.
Embodiment two:
The embodiment provides a preparation method of bamboo biomass sugar, which comprises the following steps:
S21, preparing materials, namely processing raw bamboo into bamboo chips with the length of 3-5cm and the width of 1-2cm from raw bamboo, and washing the bamboo chips with two serially connected washing machines to obtain bamboo raw materials.
S22, pretreatment, namely adding a pretreatment medium into the bamboo raw material for pretreatment.
The pretreatment medium contained 0.12% sulfuric acid, and was pretreated for 2 hours.
S23, extracting sugar:
Adding a hydrolysis medium into the pretreated bamboo raw material, wherein the solid-liquid volume ratio is 1:4, so that hemicellulose in the bamboo raw material undergoes hydrolysis reaction, after the reaction is carried out for 4 hours, the hydrolysis liquid after the cooling reaction is cooled to 80 ℃ through heat exchange, and then the hydrolysis liquid is discharged to a hydrolysis liquid tank to discharge the hydrolysis liquid after the reaction.
Wherein the hydrolysis medium is 1.5% sulfuric acid, and the hydrolysis temperature is 120 ℃.
And adding water to circularly wash the reaction residue to obtain sugar recovery liquid. In this step, the volume of the circulating washing water was controlled to be 4 times the volume of the solid matter.
Mixing the hydrolysate with the sugar recovery liquid according to the mass ratio of 1:1.5 to obtain a mixed liquid.
S24, neutralization:
And slowly adding calcium carbonate slurry into the mixed solution under the stirring condition to perform neutralization reaction, wherein the reaction temperature is 75 ℃, and the reaction time is 0.5 hour, so as to obtain a neutralization solution.
And (3) carrying out solid-liquid separation on the neutralization solution, and filtering out calcium sulfate crystal salt to obtain clear liquid.
S25, concentrating and purifying:
a. Pumping the clear liquid into a filter membrane device for desalination and concentration to obtain concentrated solution.
The filter membrane equipment adopts a ceramic nanofiltration membrane with a molecular weight cutoff value of 150 Da.
B. activated carbon is added into the concentrated solution under stirring for decolorization, the temperature is raised to 70 ℃, and the temperature is kept for 0.5 hour.
And (3) carrying out solid-liquid separation on the decolored concentrated solution, filtering out activated carbon mud powder to obtain decolored solution, and controlling the transmittance of the decolored solution after solid-liquid separation to be more than 80%.
C. And pumping the decolorized liquid into an ion exchange column for ion exchange purification to obtain bamboo biomass sugar liquid, wherein the transmittance of the bamboo biomass sugar liquid is more than 90%.
The ion exchange columns are provided with four groups, and the arrangement sequence is cation exchange column-anion exchange column-cation exchange column-anion exchange column.
S26, re-concentrating, namely concentrating the bamboo biomass sugar solution to 65% to obtain concentrated syrup.
Specifically, the bamboo biomass sugar solution is pumped into a filter membrane device for concentration to obtain bamboo biomass sugar concentrate with the concentration of 20% -22%, and then the bamboo biomass sugar concentrate is pumped into a plate evaporator for concentration to 65%, so that the concentrated syrup is obtained.
S27, chromatographic separation, namely, cooling the concentrated syrup to 65 ℃, then sending the cooled concentrated syrup into an SSMB sequential simulated moving bed for chromatographic separation, and separating the concentrated syrup by adopting continuous chromatographic separation equipment to obtain xylooligosaccharide liquid with the concentration of 45% and xylose liquid with the concentration of 39%.
The purity of the xylo-oligosaccharide in the xylo-oligosaccharide liquid is 95%, and the purity of the xylo-oligosaccharide in the xylo-oligosaccharide liquid is 92%. The foregoing description is only of embodiments of the present invention, and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes using the content of the present invention, or direct or indirect application in other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The preparation method of the bamboo biomass sugar is characterized by comprising the following steps of:
(1) Preparing materials, namely slicing or/and preparing bamboo chips and bamboo powder, and washing the bamboo chips and the bamboo powder to obtain bamboo raw materials;
(2) Pretreatment, namely adding a pretreatment medium into the bamboo raw material for pretreatment;
The pretreatment medium contains 0.05 to 0.12 percent of sulfuric acid, and is pretreated for 0.5 to 2 hours;
(3) Sugar extraction:
3a, adding a hydrolysis medium into the pretreated bamboo raw material to enable hemicellulose in the bamboo raw material to undergo hydrolysis reaction, and cooling and discharging hydrolysis liquid after the reaction;
the hydrolysis medium is sulfuric acid with the concentration of 0.5% -3%, the hydrolysis temperature is 100-120 ℃, and the hydrolysis is carried out for 1-4 hours;
3b, adding water to circularly wash reaction residues to obtain sugar recovery liquid;
3c, mixing the hydrolysate with the sugar recovery liquid according to the ratio of 1:1-1:2 to obtain a mixed liquid;
(4) And (3) neutralization:
Slowly adding calcium carbonate slurry into the mixed solution under the stirring condition for neutralization reaction, wherein the reaction temperature is 75-85 ℃ and the reaction time is 0.5-1 hour, so as to obtain a neutralization solution;
4b, carrying out solid-liquid separation on the neutralization solution, and filtering out calcium sulfate crystal salt to obtain clear liquid;
(5) Concentrating and purifying:
pumping the clear liquid into a filter membrane device for desalination and concentration to obtain concentrated liquid;
5b, adding active carbon into the concentrated solution under the stirring condition for decoloring, heating to 70-80 ℃, and preserving heat for 0.5-1 hour;
5c, carrying out solid-liquid separation on the decolored concentrated solution, and filtering out activated carbon mud powder to obtain decolored solution;
pumping the decolorized liquid into an ion exchange column for ion exchange purification to obtain bamboo biomass sugar liquor;
(6) Concentrating the bamboo biomass sugar solution to 55% -65% to obtain concentrated syrup;
(7) Separating the concentrated syrup by adopting continuous chromatographic separation equipment to obtain xylooligosaccharide liquid with the concentration of 30-50 percent and xylose liquid.
2. The preparation method of claim 1, further comprising the steps of concentrating the xylooligosaccharide liquid and the xylose liquid respectively, and drying the concentrated xylooligosaccharide liquid and xylose liquid respectively by high-pressure pumping into a spray dryer to obtain powdery xylooligosaccharide and powdery xylose.
3. The process according to claim 1, wherein the hydrolysis vapors from the hydrolysis in step 3a are condensed in a spray condenser, and the condensate produced is used for the cyclic washing of the reaction residues in step 3 b.
4. The method according to claim 1, wherein in step 4a, the pH of the neutralization solution is controlled to 3.5 to 4;
Or in the step 5b, the dosage of the activated carbon is controlled to be 10% -30% of the total solid content.
5. The method according to claim 1, wherein after step 5c, the decolorized solution is pumped to a filtration membrane device for desalting and concentrating.
6. The method according to claim 1 or 5, wherein the filter device is a ceramic nanofiltration membrane, and the molecular weight cut-off of the membrane is 150-200Da.
7. The method of claim 1, wherein in step 5d, the ion exchange column comprises at least one cation exchange column and at least one anion exchange column.
8. The method of claim 1, wherein step (6) comprises:
6a, pumping the bamboo biomass sugar liquid into a filter membrane device for concentration to obtain bamboo biomass sugar concentrated liquid with the concentration of 20% -22%;
And 6b, pumping the bamboo biomass sugar concentrate into a plate evaporator for concentrating to 55% -65% to obtain the concentrated syrup.
9. The method according to claim 1 or 8, wherein the permeate liquid in step 5a and the evaporated condensate water in step 6b are fed into a pretreatment medium tank for pretreatment of the bamboo material in step (2).
10. The process of claim 1, wherein in step (7), the concentrated syrup is separated using an SSMB-sequential simulated moving bed.
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