CN110699401A - Method for pretreating caragana microphylla by using ethylenediamine - Google Patents
Method for pretreating caragana microphylla by using ethylenediamine Download PDFInfo
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- CN110699401A CN110699401A CN201910933495.6A CN201910933495A CN110699401A CN 110699401 A CN110699401 A CN 110699401A CN 201910933495 A CN201910933495 A CN 201910933495A CN 110699401 A CN110699401 A CN 110699401A
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- ethylenediamine
- caragana microphylla
- pretreated
- pretreating
- pretreatment
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- 241000223025 Caragana microphylla Species 0.000 title claims abstract description 51
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000002203 pretreatment Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 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 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 abstract description 15
- 239000001913 cellulose Substances 0.000 abstract description 15
- 229920002488 Hemicellulose Polymers 0.000 abstract description 10
- 229920005610 lignin Polymers 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 11
- 239000002994 raw material Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 108010059892 Cellulase Proteins 0.000 description 3
- 240000008042 Zea mays Species 0.000 description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 3
- 229940106157 cellulase Drugs 0.000 description 3
- 235000005822 corn Nutrition 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229940059442 hemicellulase Drugs 0.000 description 3
- 108010002430 hemicellulase Proteins 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 238000010299 mechanically pulverizing process Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 150000002772 monosaccharides Chemical class 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000233866 Fungi Species 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 239000002029 lignocellulosic biomass Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
Abstract
The invention provides a method for pretreating caragana microphylla by using ethylenediamine. And uniformly mixing the pulverized caragana microphylla and ethylenediamine, placing the mixture into a closed reaction container, and reacting at the temperature of 120-230 ℃ to obtain the pretreated caragana microphylla. The method can effectively remove lignin, retain cellulose, reduce cellulose crystallinity, and improve enzymolysis efficiency of cellulose and hemicellulose in Caragana microphylla. The method has the advantages of simple operation and small corrosion to equipment, and the ethylenediamine can be subsequently recovered, so the method is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of biomass refining, and particularly relates to a method for pretreating caragana microphylla by using ethylenediamine.
Background
With the gradual depletion of petroleum resources and the increasing deterioration of the environment, environmental-friendly renewable resources are receiving more and more attention. Renewable biomass with abundant reserves and wide sources is an important component of a novel resource system. Lignocellulosic biomass feedstock is composed mainly of cellulose, hemicellulose and lignin. In plant cell walls, lignin is filled between cellulose and hemicellulose, and is linked to carbohydrate polymers through hydrogen bonds and covalent bonds. This dense structure can help plants resist the invasion of microorganisms, but it seriously increases the difficulty of their development and utilization. The main functions of the pretreatment process are to separate hemicellulose and/or lignin, reduce the crystallinity of cellulose, increase gaps and the like, and improve the enzymolysis accessibility of the cellulose and the hemicellulose by destroying the stable structure of plant cell walls.
In the field of biomass refining, it is important to develop a raw material source and search for a cheap alternative raw material. The caragana microphylla is an important vegetation which is widely planted in arid and semiarid regions in northwest of China, has wind-proof and sand-fixing capabilities and improves the ecological environment. The planting area of the caragana microphylla in China is 300 ten thousand mu, and as the caragana microphylla needs to be cut down for about 3 years, about 3 tons of caragana microphylla stems can be obtained per mu, and 300 ten thousand tons of caragana microphylla resources are urgently needed to be developed and utilized every year. Cellulose, hemicellulose and the like in caragana microphylla can be converted into fuel ethanol through biological fermentation, so that the caragana microphylla becomes a substitute of the first generation of fuel ethanol taking grains as raw materials, and considerable economic and environmental benefits can be generated if the caragana microphylla is efficiently utilized. However, caragana microphylla belongs to perennial woody plants, the lignification degree of caragana microphylla is high, the cellulose release is difficult, the utilization rate is low, and the lignification degree is higher and higher along with the increase of the tree age, and the processing difficulty is increased. Therefore, the efficient separation of lignin and the efficient utilization of cellulose are key technologies for the resource utilization of caragana microphylla.
The existing pretreatment methods mainly comprise physical methods, such as mechanical crushing, microwave pretreatment, freezing pretreatment, ultrasonic treatment and the like; chemical methods such as acid, base, organic solvent and ionic liquid pretreatment; physical and chemical methods, such as steam explosion pretreatment, ammonia fiber explosion pretreatment, high-temperature liquid water pretreatment and the like; biological methods, such as biological enzyme pretreatment, brown rot fungus pretreatment, white rot fungus pretreatment, and the like. However, due to the large difference of chemical compositions and structures of different substrates (herbs and woody), different action mechanisms and limited application ranges of different pretreatment methods, an effective pretreatment mode needs to be explored for the woody plant, caragana microphylla, and the resource utilization level of the woody plant is improved.
Ethylenediamine is an organic base having a boiling point of 119 ℃ and can be recovered by heating or the like. The organic alkali can open ether bonds connected between the lignin and the hemicellulose, so that the lignin is removed, the cellulose and the hemicellulose are retained to a greater extent, and the crystal form of the cellulose can be changed. The ethylenediamine pretreatment can effectively improve the enzymolysis yield of herbaceous lignocellulose such as corn straws and the like. Publication No. CN104561183A provides a pretreatment method of corn stalks, which can effectively improve the enzymolysis efficiency of the corn stalks by using ethylenediamine, but due to the difference in chemical composition and structure between woody plants and herbaceous plants, the biological resistance of the woody plants is stronger than that of herbaceous plants.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for pretreating caragana microphylla with ethylenediamine, wherein the pretreatment method of the present invention can significantly improve the conversion rate of cellulose and hemicellulose of caragana microphylla of woody plants.
The invention provides a method for pretreating caragana microphylla by using ethylenediamine, which comprises the following steps:
and uniformly mixing the pulverized caragana microphylla and ethylenediamine, placing the mixture in a closed reactor, heating for reaction, taking out the reactor after a certain time, quickly cooling, and taking out the material to obtain the caragana microphylla pretreated by the ethylenediamine.
Preferably, the caragana microphylla selected by the invention has a size capable of passing through a 20-mesh sieve.
Preferably, the temperature for heating the reaction is 120-230 ℃.
Preferably, the heating reaction time is 10 to 60 min.
Preferably, the mass volume ratio of the caragana microphylla to the ethylenediamine is 1 g: (1-5) mL.
Preferably, the caragana microphylla is pretreated by ethylenediamine, washed by water, filtered or heated to recover ethylenediamine, so as to obtain pretreated solid, and then dried. The ethylenediamine can be recovered in a subsequent process using a suitable recovery unit. The invention provides a method for pretreating caragana microphylla by using ethylenediamine, which comprises the following steps: and (3) placing the pulverized caragana microphylla and ethylenediamine in a closed reactor, and carrying out heating reaction at the temperature of 120-230 ℃ to obtain the caragana microphylla pretreated by the ethylenediamine. The ethylenediamine pretreatment method provided by the invention can remove lignin, retain cellulose and hemicellulose to a greater extent, change the crystal form of cellulose, and improve the enzymolysis efficiency of pretreated caragana microphylla to a great extent. And the ethylenediamine can be recycled after being heated and recovered, so that the cost is saved. The results of the implementation case of the invention show that the yield of glucose obtained after the pretreatment and enzymolysis of the caragana microphylla ethylenediamine is 88.03%, and is obviously improved compared with the yield of glucose obtained after the enzymolysis of the untreated caragana microphylla, which is 9.63%.
Detailed Description
Example 1: the invention relates to a method for pretreating caragana microphylla by using ethylenediamine and carrying out enzymolysis
(1) Pretreatment method
Mechanically pulverizing the dried caragana microphylla raw material, sieving with a 40-mesh sieve, weighing 20g of the obtained caragana microphylla material, placing into a 250mL stainless steel reaction kettle with a sealing cover, adding 30mL ethylenediamine, stirring uniformly, and screwing the sealing cover. And (3) putting the reaction kettle containing the solid-liquid mixture into an oil bath kettle at the temperature of 120 ℃ for reaction for 10 min. And (3) taking out the reaction kettle, then putting cold water into the reaction kettle, rapidly cooling the reaction kettle, opening the reaction kettle, taking out the materials, washing the materials by using deionized water (or heating and recovering ethylenediamine), and filtering and airing the materials to obtain the pretreated caragana microphylla.
(2) Enzymolysis method
Adding a certain amount of material pretreated by ethylenediamine into a 100mL conical flask with a small opening, adding cellulase, hemicellulase and water, carrying out enzymolysis reaction for 72h in a shaking table at 50 ℃ and 200rpm, sampling after the reaction is finished, centrifuging at 12000rpm for 5min, and taking the supernatant and passing through a 0.22 mu m water system membrane. The monosaccharide content was determined using high performance liquid chromatography. The glucose conversion was calculated to be 62.98%.
Example 2: the invention relates to a method for pretreating caragana microphylla by using ethylenediamine and carrying out enzymolysis
(1) Pretreatment method
Mechanically pulverizing the dried caragana microphylla raw material, sieving with a 60-mesh sieve, weighing 20g of the obtained caragana microphylla material, placing into a 250mL stainless steel reaction kettle with a sealing cover, adding 70mL ethylenediamine, stirring uniformly, and screwing the sealing cover. And (3) putting the reaction kettle containing the solid-liquid mixture into an oil bath kettle at 180 ℃ for reaction for 30 min. And (3) taking out the reaction kettle, then putting cold water into the reaction kettle, rapidly cooling the reaction kettle, opening the reaction kettle, taking out the materials, washing the materials by using deionized water (or heating and recovering ethylenediamine), and filtering and airing the materials to obtain the pretreated caragana microphylla.
(2) Enzymolysis method
Adding a certain amount of material pretreated by ethylenediamine into a 100ml thin-mouth conical flask, adding cellulase, hemicellulase and water, carrying out enzymolysis reaction for 72h in a shaking table at 50 ℃ and 200rpm, sampling after the reaction is finished, centrifuging at 12000rpm for 5min, and taking the supernatant and passing through a 0.22 mu m water system membrane. The monosaccharide content was determined using high performance liquid chromatography. The glucose conversion was calculated to be 73.62%.
Example 3: the invention relates to a method for pretreating caragana microphylla by using ethylenediamine and carrying out enzymolysis
(1) Pretreatment method
Mechanically pulverizing the dried caragana microphylla raw material, sieving with a 80-mesh sieve, weighing 20g of the obtained caragana microphylla material, placing into a 250mL stainless steel reaction kettle with a sealing cover, adding 100mL ethylenediamine, stirring uniformly, and screwing the sealing cover. And (3) putting the reaction kettle containing the solid-liquid mixture into an oil bath kettle at 230 ℃ for reaction for 60 min. And (3) taking out the reaction kettle, then putting cold water into the reaction kettle, rapidly cooling the reaction kettle, opening the reaction kettle, taking out the materials, washing the materials by using deionized water (or heating and recovering ethylenediamine), and filtering and airing the materials to obtain the pretreated caragana microphylla.
(2) Enzymolysis method
Adding a certain amount of material pretreated by ethylenediamine into a 100mL conical flask with a small opening, adding cellulase, hemicellulase and water, carrying out enzymolysis reaction for 72h in a shaking table at 50 ℃ and 200rpm, sampling after the reaction is finished, centrifuging at 12000rpm for 5min, and taking the supernatant and passing through a 0.22 mu m water system membrane. The monosaccharide content was determined using high performance liquid chromatography. The glucose conversion was calculated to be 88.03%.
Claims (6)
1. A method for pretreating caragana microphylla by ethylenediamine comprises the following steps:
and uniformly mixing the pulverized caragana microphylla and ethylenediamine, placing the mixture in a closed reactor, heating for reaction, taking out the reactor after a certain time, quickly cooling, and taking out the material to obtain the caragana microphylla pretreated by the ethylenediamine.
2. The pretreatment method of claim 1, wherein the caragana microphylla is selected to have a size capable of passing through a 20-mesh screen.
3. The pretreatment method as claimed in claim 1, wherein the temperature of the heating reaction is 120-230 ℃.
4. The pretreatment method according to claim 1, wherein the heating reaction time is 10 to 60 min.
5. The pretreatment method according to claim 1, wherein the mass-to-volume ratio of caragana microphylla to ethylenediamine is 1 g: (1-5) ml.
6. The pretreatment method of claim 1, wherein the caragana microphylla is pretreated with ethylenediamine, washed with water, filtered or heated to recover ethylenediamine, to obtain pretreated solid, and dried. The glucose yield is obviously improved after enzymolysis, and the ethylenediamine can be recovered by adopting a proper recovery device in the subsequent process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910933495.6A CN110699401A (en) | 2019-09-29 | 2019-09-29 | Method for pretreating caragana microphylla by using ethylenediamine |
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| CN201910933495.6A CN110699401A (en) | 2019-09-29 | 2019-09-29 | Method for pretreating caragana microphylla by using ethylenediamine |
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|---|---|
| CN110699401A true CN110699401A (en) | 2020-01-17 |
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| CN201910933495.6A Pending CN110699401A (en) | 2019-09-29 | 2019-09-29 | Method for pretreating caragana microphylla by using ethylenediamine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115786420A (en) * | 2022-12-02 | 2023-03-14 | 天津大学 | Pretreatment method of crop straw and preparation method of lignin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104611394A (en) * | 2015-03-04 | 2015-05-13 | 天津大学 | Method for pretreating lignocellulose raw material and application |
| WO2017049739A1 (en) * | 2015-09-25 | 2017-03-30 | 广东工业大学 | Method for improving enzymolysis efficiency of lignocellulosic biomass |
| CN109055440A (en) * | 2018-09-17 | 2018-12-21 | 天津科技大学 | A kind of preprocess method of lignocellulosic |
| CN109182396A (en) * | 2018-09-26 | 2019-01-11 | 天津科技大学 | A method of improving caragana microphylla steam blasting effect |
-
2019
- 2019-09-29 CN CN201910933495.6A patent/CN110699401A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104611394A (en) * | 2015-03-04 | 2015-05-13 | 天津大学 | Method for pretreating lignocellulose raw material and application |
| WO2017049739A1 (en) * | 2015-09-25 | 2017-03-30 | 广东工业大学 | Method for improving enzymolysis efficiency of lignocellulosic biomass |
| CN109055440A (en) * | 2018-09-17 | 2018-12-21 | 天津科技大学 | A kind of preprocess method of lignocellulosic |
| CN109182396A (en) * | 2018-09-26 | 2019-01-11 | 天津科技大学 | A method of improving caragana microphylla steam blasting effect |
Non-Patent Citations (1)
| Title |
|---|
| 何士成等: "碱处理中温度对不同底物特性木质纤维素结构及酶解的影响", 《江苏农业科学》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115786420A (en) * | 2022-12-02 | 2023-03-14 | 天津大学 | Pretreatment method of crop straw and preparation method of lignin |
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Application publication date: 20200117 |