CN109867732B - Method for improving hemicellulose extraction yield - Google Patents
Method for improving hemicellulose extraction yield Download PDFInfo
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- CN109867732B CN109867732B CN201910162965.3A CN201910162965A CN109867732B CN 109867732 B CN109867732 B CN 109867732B CN 201910162965 A CN201910162965 A CN 201910162965A CN 109867732 B CN109867732 B CN 109867732B
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- biomass material
- hemicellulose
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- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000000605 extraction Methods 0.000 title claims abstract description 24
- 239000002028 Biomass Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000002791 soaking Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010411 cooking Methods 0.000 claims abstract description 18
- 238000010257 thawing Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000007605 air drying Methods 0.000 claims abstract description 3
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 239000002023 wood Substances 0.000 claims description 47
- 241000219000 Populus Species 0.000 claims description 23
- 238000007710 freezing Methods 0.000 claims description 9
- 230000008014 freezing Effects 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 7
- 235000013312 flour Nutrition 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 14
- 238000004255 ion exchange chromatography Methods 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- 239000000835 fiber Substances 0.000 description 6
- 238000004537 pulping Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 240000003433 Miscanthus floridulus Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention belongs to the field of improving the comprehensive utilization efficiency of biomass materials, and particularly relates to a method for improving the extraction yield of hemicellulose. The method comprises the following steps: cleaning and air-drying the biomass material, then fully soaking the biomass material in water, and performing freeze thawing treatment on the soaked biomass material; adding soaking liquid (water after soaking the biomass material) into the biomass material subjected to freeze thawing treatment for cooking, and collecting the cooking liquid after the reaction is finished to obtain pre-extracted sugar liquid. The reagent used in the invention is deionized water, and no chemical reagent is added in the whole process, so that the method is green and environment-friendly; the extraction process is simple and easy to operate; is expected to improve the dissolution rate of the hemicellulose and reduce the production cost at the same time.
Description
Technical Field
The invention belongs to the field of improving the comprehensive utilization efficiency of biomass materials, and particularly relates to a method for improving the extraction yield of hemicellulose.
Background
Plant fiber raw materials are the most abundant renewable resources in nature, the paper industry is the major household using plant resources, and about one hundred million tons of plant fiber raw materials are used for pulping and papermaking in the world every year. However, pulping and papermaking only uses cellulose which is one of three major components of plant raw materials, and hemicellulose and lignin which are also used as the three major components are relatively rarely used, so how to effectively utilize plant fiber resources becomes one of important fields of research in many countries in the world. The method has the advantages that the hemicellulose in the plant fiber resources is efficiently and environmentally extracted, and the method has important significance for plant resource utilization, environmental protection and sustainable development.
The traditional chemical pulping method is generally used for directly treating raw materials, most of biomass, especially hemicellulose in the raw materials enter pulping waste liquid to be wasted, and the potential value of the hemicellulose as a biomass resource is ignored. Therefore, before the pulping working section, a pretreatment method with mild conditions is adopted to separate part of hemicellulose in the fiber raw material, and the hemicellulose is converted and fermented or chemicals such as acetic acid and the like are directly extracted to realize high value-added utilization of the hemicellulose. At present, many researchers research and develop various pretreatment methods, which can be classified into physical methods, chemical methods, biological methods, comprehensive methods and the like. But the physical pretreatment can damage the fiber structure, so the operation cost is higher; the requirements of dilute acid pretreatment production equipment are high, the requirements of process control conditions are very strict, certain pollution can be caused to the environment, and more importantly, the dilute acid pretreatment can hydrolyze part of cellulose, so that the method is unfavorable for the pulping process; in the alkaline pretreatment production process, alkali is added in the pre-extraction process, so that part of lignin is dissolved out, the purification of hemicellulose becomes more difficult, and the production cost is increased. The hot water pre-extraction method does not need to use acid, and the pretreated slurry does not need to use chemicals for buffering and neutralizing treatment, so that the cost is reduced, and the aim of no pollution to the environment is fulfilled.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide a method for extracting hemicellulose yield by two-step green treatment.
The purpose of the invention is realized by the following technical scheme:
a method for improving the extraction yield of hemicellulose comprises the following steps:
(1) cleaning and air-drying the biomass material, then fully soaking the biomass material in water, and performing freeze thawing treatment on the soaked biomass material;
(2) and (2) adding a soaking solution (namely the water obtained after soaking the biomass material in the step (1)) into the biomass material subjected to freeze thawing treatment for cooking, and collecting the cooking solution after the reaction is finished to obtain a pre-extracted sugar solution.
Preferably, the biomass material comprises one or more of wood chips, wood flour, and non-wood biomass materials (e.g., wheat straw, rice straw, reed, bagasse, miscanthus, bamboo, devil's rush, etc.).
More preferably, the wood chips are poplar chips.
More preferably, the specification of the wood chips is (15-25) mm x (10-20) mm x (3-5) mm. Preferably, the moisture content of the biomass material is 7-15%.
Preferably, the number of cycles of the freeze-thaw treatment is 1-6.
Preferably, the freezing temperature of the freeze-thaw treatment is-4 ℃ to-70 ℃, and the thawing temperature is 16 ℃ to 30 ℃.
Preferably, the freezing time of the freeze-thaw treatment is 6-24 h, and the thawing time is 3-10 h.
Preferably, the solid-to-liquid ratio of the biomass material to the soaking solution is 1: (4-10) g/mL, wherein the mass of the biomass material is calculated by absolute dry mass.
Preferably, the cooking temperature is 120 ℃ to 185 ℃.
Preferably, the heating time of the cooking is 30-90 min, and the heat preservation time is 30-90 min.
The preparation method of the invention has the following advantages and beneficial effects:
(1) the reagent used in the invention is water, and no chemical reagent is added in the whole process, so that the method is green and environment-friendly;
(2) the method for improving the extraction yield of the hemicellulose has the advantages of simple process, easy operation and lower cost;
(3) compared with the simple hot water pre-extraction, the content of hemicellulose in the pre-extraction solution is obviously improved.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The sizes of the wood chips selected in the examples were (20. + -. 5) mm X (15. + -. 5) mm X (4. + -.1) mm.
Example 1
(1) Taking 30g of air-dried poplar chips (absolutely dry), fully soaking the wood chips with 178mL of deionized water until the wood chips are completely soaked, freezing the soaked wood chips in a refrigerator at the temperature of-20 ℃ for 6 hours, then taking out the wood chips, unfreezing the wood chips at room temperature for 5 hours until the wood chips are completely unfrozen, and carrying out freeze-thaw cycling for 1 time;
(2) and (3) after the freeze-thaw treatment is finished, adding the wood chips subjected to the freeze-thaw treatment and a soaking solution (namely water obtained after soaking the wood chips in the step (1)) into a rotary multi-tank digester, heating to 170 ℃ to cook the wood chips, wherein the heating time is 1h, the heat preservation time is 1h, the stewing solution is collected after the reaction is finished, and the extraction amount of hemicellulose of the wood chips is 88.43mg/g through ion chromatography detection.
Control group 1: taking 30g of air-dried poplar chips (completely dried), adding 178mL of deionized water into a rotary multi-tank digester, heating to 170 ℃ for digesting the wood chips, wherein the heating time is 1h, the heat preservation time is 1h, after the reaction is finished, collecting digestion liquid, and detecting the extraction amount of hemicellulose of the wood chips by ion chromatography to be 81.23 mg/g.
Example 2
(1) Taking 30g of air-dried poplar chips (absolutely dry), fully soaking the wood chips with 178mL of deionized water until the wood chips are completely soaked, freezing the soaked wood chips in a refrigerator at the temperature of-20 ℃ for 6 hours, then taking out the wood chips, unfreezing the wood chips at room temperature for 5 hours until the wood chips are completely unfrozen, and carrying out freeze-thaw cycling for 4 times;
(2) and (3) after the freeze-thaw treatment is finished, adding the wood chips subjected to the freeze-thaw treatment and a soaking solution (namely water obtained after soaking the wood chips in the step (1)) into a rotary multi-tank digester, heating to 170 ℃ to cook the wood chips, wherein the heating time is 1h, the heat preservation time is 1h, the stewing solution is collected after the reaction is finished, and the extraction amount of hemicellulose of the wood chips is 100.72mg/g through ion chromatography detection.
Control group 2: taking 30g of air-dried poplar chips (completely dried), adding 178mL of deionized water into a rotary multi-tank digester, cooking the poplar chips at 170 ℃, heating for 1h, keeping the temperature for 1h, collecting cooking liquor after the reaction is finished, and detecting the extraction amount of hemicellulose of the poplar chips by ion chromatography to be 81.23 mg/g.
Example 3
(1) Taking 30g of air-dried poplar chips (absolutely dry), fully soaking the wood chips with 178mL of deionized water until the wood chips are completely soaked, freezing the soaked wood chips in a refrigerator at the temperature of-20 ℃ for 6 hours, then taking out the wood chips, unfreezing the wood chips at room temperature for 5 hours until the wood chips are completely unfrozen, and carrying out freeze-thaw cycling for 1 time;
(2) and (3) after the freeze-thaw treatment is finished, adding the wood chips subjected to the freeze-thaw treatment and a soaking solution (namely water obtained after soaking the wood chips in the step (1)) into a rotary multi-tank digester, heating to 160 ℃ for cooking the wood chips, wherein the heating time is 1h, the heat preservation time is 1h, the cooking solution is collected after the reaction is finished, and the extraction amount of hemicellulose of the wood chips is 60.79mg/g through ion chromatography detection.
Control group 3: taking 30g of air-dried poplar chips (completely dried), adding 178mL of deionized water into the poplar chips by a rotary multi-tank digester, cooking the poplar chips at 160 ℃, heating for 1h, keeping the temperature for 1h, collecting cooking liquor after the reaction is finished, and detecting the extraction amount of hemicellulose of the poplar chips by ion chromatography to be 31.23 mg/g.
Example 4
(1) Taking 30g of air-dried poplar chips (absolutely dry), fully soaking the poplar chips with 182mL of deionized water until the poplar chips are completely soaked, freezing the soaked poplar chips in a refrigerator at the temperature of-20 ℃ for 6 hours, taking out the poplar chips, thawing the poplar chips for 5 hours at room temperature until the poplar chips are completely thawed, and circulating for 1 time of freezing and thawing;
(2) and (3) after the freeze-thaw treatment is finished, adding the wood chips subjected to the freeze-thaw treatment and a soaking solution (namely water obtained after soaking the wood chips in the step (1)) into a rotary multi-tank digester, heating to 170 ℃ to cook the wood chips, wherein the heating time is 1h, the heat preservation time is 1h, the stewing solution is collected after the reaction is finished, and the extraction amount of hemicellulose of the wood chips is 92.77mg/g through ion chromatography detection.
Control group 4: taking 30g of air-dried poplar chips (completely dried), adding 182mL of deionized water into the poplar chips for cooking at 170 ℃ by using a rotary multi-tank cooker, heating for 1h, keeping the temperature for 1h, collecting cooking liquor after the reaction is finished, and detecting the extraction amount of hemicellulose of the wood chips by ion chromatography to be 81.23 mg/g.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. The method for improving the extraction yield of hemicellulose is characterized by comprising the following steps of:
(1) cleaning and air-drying the biomass material, then fully soaking the biomass material in water, and performing freeze thawing treatment on the soaked biomass material; the freezing temperature of the freeze-thaw treatment is-4 ℃ to-70 ℃, and the unfreezing temperature is 16 ℃ to 30 ℃; the number of times of the freeze-thaw treatment is 1-6; the freezing time of the freeze thawing treatment is 6-24 h, and the thawing time is 3-10 h;
(2) adding the soaking solution into the biomass material subjected to freeze thawing treatment for cooking, and collecting the cooking solution after the reaction is finished to obtain the pre-extracted sugar solution.
2. The method of claim 1, wherein the biomass material comprises one or more of wood chips, wood flour, and non-wood biomass material.
3. The method of claim 2, wherein the wood chips are poplar chips.
4. The method for improving the hemicellulose extraction yield according to claim 3, wherein the poplar chips are (15-25) mmX (10-20) mmX (3-5) mm in size.
5. The method for improving the extraction yield of hemicellulose according to claim 1, wherein the solid-to-liquid ratio of the biomass material to the soaking solution is 1: (4-10) g/mL, wherein the mass of the biomass material is calculated by absolute dry mass.
6. The method for improving hemicellulose extraction yield according to claim 1, wherein the cooking temperature is 120-185 ℃.
7. The method for improving the hemicellulose extraction yield according to claim 1, wherein the cooking temperature rise time is 30-90 min, and the heat preservation time is 30-90 min.
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| CN110924206A (en) * | 2019-12-11 | 2020-03-27 | 国际竹藤中心 | Method for cleanly separating bamboo raw material components |
| CN113444187A (en) * | 2021-08-04 | 2021-09-28 | 广西大学 | Method for efficiently separating bagasse from high-yield high-purity hemicellulose by aid of ultralow-temperature quick-freezing and p-toluenesulfonic acid |
| CN113527542A (en) * | 2021-08-04 | 2021-10-22 | 广西大学 | Method for efficiently separating bagasse high-yield high-purity high-molecular-weight hemicellulose by freeze thawing assisted with p-toluenesulfonic acid |
Citations (3)
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|---|---|---|---|---|
| CN102226317A (en) * | 2011-05-06 | 2011-10-26 | 华南理工大学 | Co-production preparation method of bamboo biomass fuel and bamboo pulp |
| CN102561082A (en) * | 2012-03-01 | 2012-07-11 | 北京林业大学 | Method of extracting hemicellulose, cellulose and lignin from wood fiber raw materials |
| CN108178837A (en) * | 2017-12-28 | 2018-06-19 | 盐城工业职业技术学院 | A kind of Ramulus Mori biomass cellulose full constituent aeroge and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226317A (en) * | 2011-05-06 | 2011-10-26 | 华南理工大学 | Co-production preparation method of bamboo biomass fuel and bamboo pulp |
| CN102561082A (en) * | 2012-03-01 | 2012-07-11 | 北京林业大学 | Method of extracting hemicellulose, cellulose and lignin from wood fiber raw materials |
| CN108178837A (en) * | 2017-12-28 | 2018-06-19 | 盐城工业职业技术学院 | A kind of Ramulus Mori biomass cellulose full constituent aeroge and preparation method thereof |
Non-Patent Citations (2)
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| 《小麦秸秆冻融-酸碱相结合的预处理工艺研究;王新明;《中国优秀硕士学位论文全文数据库工程科技I期》;20131215(第12期);第16-31页 * |
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