CN107540850B - Plant fiber microwave liquefaction method - Google Patents

Plant fiber microwave liquefaction method Download PDF

Info

Publication number
CN107540850B
CN107540850B CN201610614719.3A CN201610614719A CN107540850B CN 107540850 B CN107540850 B CN 107540850B CN 201610614719 A CN201610614719 A CN 201610614719A CN 107540850 B CN107540850 B CN 107540850B
Authority
CN
China
Prior art keywords
parts
plant fiber
liquefaction
reaction kettle
microwave
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201610614719.3A
Other languages
Chinese (zh)
Other versions
CN107540850A (en
Inventor
文胜
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi Science and Technology Normal University
Original Assignee
Guangxi Science and Technology Normal University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangxi Science and Technology Normal University filed Critical Guangxi Science and Technology Normal University
Priority to CN201610614719.3A priority Critical patent/CN107540850B/en
Publication of CN107540850A publication Critical patent/CN107540850A/en
Application granted granted Critical
Publication of CN107540850B publication Critical patent/CN107540850B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention discloses a plant fiber microwave liquefaction method, which comprises the steps of firstly, uniformly mixing 100 parts of mechanically crushed plant fiber, 0.5-1 part of microbial agent and 20-25 parts of water, then sealing and fermenting for 5-6 days, opening a pool and airing until the water content is lower than 8%; then 100 parts of the mixture obtained in the step one, 2-8 parts of catalyst, 8-12 parts of hydrogen donor and 280 parts of liquefying agent of 200-; naturally cooling to 90 ℃, introducing cooling water into the reaction kettle, cooling the reaction kettle to room temperature, and discharging hydrogen; and (3) filtering the liquid in the reaction kettle to remove residues, distilling the obtained liquid at 45-50 ℃ by using a rotary evaporator, and obtaining the plant fiber liquefied product after distillation. According to the invention, a fermentation step is added before the plant fiber liquefaction reaction, so that the plant fiber is decomposed in advance, the subsequent liquefaction reaction is facilitated, the reaction condition is mild, and the liquefaction rate is high and can reach more than 95%.

Description

Plant fiber microwave liquefaction method
Technical Field
The invention relates to the technical field of biomass liquefaction, in particular to a plant fiber microwave liquefaction method.
Background
In recent decades, the polyurethane industry has been rapidly developed, and because the properties and structure of the polyurethane polymer are closely related, the weight of the polyurethane polymer can be easily controlled by the structure of the raw material, and the polyurethane polymer can be respectively made into various product forms such as plastics, rubber or elastomers, fibers, coatings, sizing agents, synthetic leather and the like according to needs, and can be widely applied to various fields such as transportation, buildings, machinery, sports, medical treatment and the like. The conventional polyurethane industry relies mainly on the development of the petrochemical industry, and the rapid development of the petrochemical industry has for a long time provided the polyoxy ester industry with a large amount of inexpensive raw materials such as ethylene oxide and propylene oxide. With the general improvement of living standard, the energy demand of people on petroleum is greatly increased, the price of the petroleum is increased rapidly, and the polyurethane industry which depends on the petrochemical industry seriously is impacted seriously. In addition, people have come to recognize the environmental pollution of polymer industrial products in recent years, and have made green environmental protection requirements on polymer materials, and new environment-friendly polymer materials need to be developed to meet new social requirements.
The method has the advantages that firstly, the agricultural wastes such as the rice straws, the husks and the like belong to annual herbaceous plants, the annual output is huge, the price is low, the production cost of the green environment-friendly high polymer can be reduced to a certain extent, and the sustainability of producing biodegradable materials is facilitated; secondly, agricultural waste plant fiber treatment products are used for replacing petrochemical products, so that the dependence of biodegradable materials on petrochemical industry can be reduced in the future that petroleum supply is increasingly tense; the produced environment-friendly polymer has biodegradability, the polyurethane has biodegradability to a certain degree, and the polymer produced by using the plant fiber degradation product contains partial biomass, so that the biodegradation rate can be increased quickly, and the problem of current environmental pollution can be effectively solved. Therefore, the biodegradable polyurethane produced by utilizing agricultural wastes has good prospect.
Researches show that the main components of the plant fiber, namely cellulose, hemicellulose and lignin, all contain a large amount of warp bases, and the main components can be degraded into organic chemical raw materials by a proper technical means and used for producing biodegradable high polymer materials. A large number of researches show that although the herbaceous cellulose plants have different component contents due to different varieties, the content and the structural characteristics of the same plants are similar but not too large, one representative plant is selected as a research object to effectively obtain the treatment process of the herbaceous cellulose plants, wheat is one of main food crops in China, and the degradation characteristics and the process characteristics of the herbaceous plants can be better reflected by selecting wheat and rice straws as the research object.
The preparation of chemical raw materials by using plant fiber degradation has been researched in many ways at home and abroad, but the related industrial production is still in the exploration stage, and only a few varieties of biodegradable materials are produced in small scale in Europe and America and a few developed countries in Japan. Firstly, the liquefaction time is longer, the liquefaction efficiency is lower, and a new pretreatment method is needed to improve the liquefaction efficiency; secondly, the required amount of the liquefaction reagent is higher, the liquefaction reagent mainly comes from petrochemical industry, the dependence on the petrochemical industry is still too high, the cost of the produced product has larger relevance to the petrochemical industry, and the problem of high price of the biodegradable material cannot be really solved. Therefore, the bottleneck of preparing chemical raw materials by liquefying plant fibers lies in the urgent need of developing a novel pretreatment method and improving a liquefaction treatment process.
Along with the improvement of living standard of people, the demand of plastic products is increasing day by day, especially since the 70 s in the 20 th century, the alertness of dependence of people on petrochemical energy is caused by energy crisis, the dependence of the plastic industry on petrochemical industry is high, developed countries begin to research the research of transferring material sources, and the research is useful for researching naturally degradable high molecular materials, and the utilization of plant fibers becomes an important research field in the world. The thermochemical degradation method is generally called liquefaction, and is a utilization method of plant fibers by degrading plant fibers into liquid products at a certain temperature and under a certain pressure in the presence of a chemical solvent, a catalyst and the like.
In the 19 th century, researchers have made relevant studies on plant fibers, and research on hydrolysis of the plant fibers under the action of acid, alkali and the like shows that cellulose in the plant fibers forms macromolecular mixtures with various degrees of polymerization related to the degree of hydrolysis after hydrolysis. In the 20 th century, students simulated coal liquefaction to prepare liquid fuel by liquefying wood, and the research on plant fibers is calm for a while due to higher cost and lack of application markets. The research on the liquefaction of the plant fiber at this stage is mainly based on theoretical research.
After the oil crisis outbreak in the 70's of the 20 th century, developed countries in the united states, japan and europe, focused on the research related to the development of petrochemical energy, and a large number of scholars explored the production of biomass fuels by plant fiber liquefaction technology. Humphrey et al studied the hydrolysis mechanism of plant cellulose under the action of acid and enzyme catalysis; a plant fiber liquefaction method named PERC method is developed in the Pittsburgh energy research center by Appelll and 1971, and the method is carried out under the environment of hydrogen or carbon monoxide with the temperature of 300-350 ℃ and the pressure of 14-24 MPa and in the environment of Na2CO 3; converting wood fibers into liquefied oil under the catalytic action of (1), wherein the liquefaction efficiency is 40-45%; yokoyama et al liquefy wood to fuel oil in water at 300 ℃ under lOMPa under catalysis of Na2C03 without reducing gas. Minowa and the like research influence factors of plant fiber liquefaction in water under high temperature and high pressure, obtain 21-36% of fuel oil which can be obtained by liquefaction under the conditions of 300-350 ℃ and about 18MPa, and find that a catalyst can influence the liquefaction process to a great extent. In 2004, the Netherlands established an exemplary plant for producing biofuel oil at a high pressure liquefaction rate of 8 kg/h. After the 20 th century and the 90 th era, a great deal of resources are invested in the research of environmental protection materials in various countries, the liquefied product of the liquefied plant fiber becomes one of the key research directions as a chemical raw material for producing the environmental protection high polymer material, the technology of liquefying the plant fiber under normal pressure can be realized by selecting proper catalysts and organic solvents, and the technology of preparing fuel by biological degradation also becomes a novel utilization technology of the plant fiber, and the plant fiber liquefaction technology has diversity. Common liquefaction solvents of the normal-pressure liquefaction technology are mainly phenol, carbonate and dihydroxy alcohol (polymers of ethylene glycol, glycerol and ethylene glycol), catalyst-free complete liquefaction of wood fibers is realized by Bessel and the like in a benzene solvent at 250 ℃, the influence of factors such as temperature, liquefaction time and water content on liquefaction factors is examined, about 10% of wood fibers are gasified in the liquefaction process, and lignin is easier to liquefy than cellulose.
The contradiction of energy demand in China in the twentieth century for a long time is not prominent, the waste amount of chemical products is not large, and the research on utilizing plants to replace fossil energy is not much. With the rapid development of the economy of China, the research on the utilization of plant fibers is emphasized in the 90 s, and the related research is developed vigorously. China is a big agricultural country, wood is limited, and the yield of crop byproducts is huge, so that the main research direction is to research by taking the crop byproducts as fiber raw materials. Gorgongjie and the like of the university of Compound Dan respectively adopt cane sugar and corncobs to liquefy in a polyhydric alcohol solvent, and the discovery shows that the addition of glycerol or mono-ethylene glycol micromolecules as an auxiliary solvent can inhibit the re-polycondensation of liquefied products, remarkably improve the liquefying effect of plant fibers, and can remarkably improve the biodegradation performance of the plant fibers after the liquefied products are reacted with isocyanate to prepare the polyurethane material.
The Xishuangping of the institute of Process of Chinese academy of sciences liquefies the wheat and rice straw fiber in benzene at the temperature of l00 ℃ for 30min under the catalysis of 3% concentrated sulfuric acid, and liquefies lignin and hemicellulose by utilizing different selectivities of the liquefaction reaction activities of each component of the plant fiber to obtain a product with the cellulose residual amount reaching 70%. Zhang Hui et al studied the liquefaction of wood with benzene solvent under the action of various acid catalysts. Research shows that sulfuric acid and phosphoric acid are catalysts with good catalytic effect on the benzene liquefaction of plant fibers, and can liquefy wood fibers at the temperature of 150 ℃ until the residue rate is less than 5%. The Lianglingyun of the university of Chinese agriculture and the like research the liquefaction of a plurality of plants such as corn rice, wheat rice straw, corncob and the like, and the liquefaction difficulty degree of different plant fibers in different solvents is different but the difference is smaller. By analyzing the liquefaction mechanism of the liquefied product, a dynamic model of cellulose liquefaction is established, and the cellulose liquefaction initial stage is obtained and belongs to a pseudo-first-order reaction. Zhang Jian et al studied to prepare ethylol propionic acid from wood chips and starch, and obtained the ethylol propionic acid with 20% yield after reacting for 44min under the conditions of 215 ℃ of reaction temperature, 4.7% of dilute sulphuric acid and 12.8% of liquid-solid ratio. The study of wheat straw and red deer slag as plant material at 400-500 deg.c shows that the liquefied product has main components including compounds, acids, aldehydes, etc.
The factors influencing the normal pressure degradation efficiency of the plant fiber comprise the treatment of the plant fiber before the liquefaction reaction, the liquefaction reaction conditions (temperature and time), the selection (type and dosage) of the liquefaction solvent and the selection (type and dosage) of the catalyst, which are integrated with the related research at home and abroad. The current research is mainly in a laboratory stage, and the number of people applying the research to the synthesis of products is less, and a certain gap exists from the practical application.
Disclosure of Invention
The invention aims to solve the technical problem of providing a plant fiber microwave liquefaction method which is mild in reaction condition, high in plant fiber liquefaction degree and high in utilization rate.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a plant fiber microwave liquefaction method comprises the following steps:
step one, uniformly mixing 100 parts of mechanically crushed plant fiber, 0.5-1 part of microbial agent and 20-25 parts of water, sealing, fermenting for 5-6 days, opening a pool and airing until the water content is lower than 8%; firstly, the plant fiber is fermented, so that the subsequent liquefaction reaction condition of the plant fiber is mild, the reaction temperature can be reduced, the reaction time is shortened, and the liquefaction rate is improved.
Step two, putting 100 parts of the mixture obtained in the step one, 2-8 parts of catalyst, 8-12 parts of hydrogen donor and 280 parts of liquefying agent 200 plus materials into a microwave reaction kettle with a stirrer, setting the frequency of the microwave reaction kettle to be 2500Hz, heating to 150 plus materials and 170 ℃, filling hydrogen into the reaction kettle and pressurizing to 3-4MPa, stirring and preserving heat for 15-25min, and completing plant fiber liquefaction;
step three, after naturally cooling to 90 ℃, introducing cooling water into the reaction kettle, cooling the reaction kettle to room temperature, and discharging hydrogen;
and step four, filtering the liquid in the reaction kettle to remove residues, and distilling the obtained liquid at 45-50 ℃ by using a rotary evaporator, wherein the distilled liquid is the plant fiber liquefied product.
Particularly preferably, the microbial agent comprises one or more of cellulomonas, bacillus, phosphate solubilizing flora, nitrobacteria, growth flora, thermoactinomyces, thermomonospora, yeast, penicillium and humicola.
Particularly preferably, the microbial agent comprises a mixture consisting of 3 parts of cellulomonas, 2 parts of phosphate-solubilizing flora, 1 part of nitrobacteria, 1 part of thermoactinomycetes, 1 part of thermomonospora, 2 parts of yeast and 2 parts of humicola.
Particularly preferably, the catalyst is methyl benzene sulfonic acid, nitric acid or phosphoric acid.
Particularly preferably, the hydrogen donor is one or more of phenol, hydroquinone, catechol, p-methyl phenol, trimethylphenol and methoxyphenol.
Particularly preferably, the hydrogen donor is a mixture consisting of 3 parts of phenol, 1 part of hydroquinone, 1 part of trimethylphenol and 1 part of methoxyphenol
Particularly preferably, the liquefying agent is a mixture of an alcohol solvent and a salt solution.
Particularly preferably, the liquefying agent is a mixture consisting of 5 parts of alcohol solvent and 1 part of salt solution
Particularly preferably, the alcohol solvent is one or a mixture of methanol, ethanol, glycol, glycerol, isopropanol and polyethylene glycol; the salt solution is a 10% ammonium bifluoride solution.
Particularly preferably, the plant fiber comprises one or a mixture of several of bagasse, manioc waste, bamboo waste, corn straw, sorghum straw, wheat straw, beanstalk, fiber grass, wheat straw, reed and rice straw, and the water content of the plant fiber is lower than 5%, so that the subsequent calculation of adding various raw materials is facilitated, and the reaction is more accurate and controllable.
Compared with the prior art, the invention has the following beneficial effects:
(1) the fermentation step is added before the plant fiber liquefaction reaction, so that the plant fiber can be decomposed in advance, the subsequent liquefaction reaction is facilitated, and the reaction condition is mild.
(2) The strong dispersion, stirring and shearing action of the reaction in the microwave reaction kettle can make the mixture of the organic solvent and the plant fiber more uniform, and the gradual temperature rise is also accompanied.
(3) Under the condition of proper liquefaction reaction, the plant fiber is liquefied in one step, carbonization and gasification are basically avoided, and the liquefaction rate is high and can reach more than 95%.
(4) The obtained liquefied product has high taste, and can be used as raw material for chemical industry.
Detailed Description
The present invention will be described more fully hereinafter, with reference to the accompanying drawings, in which some, but not all embodiments of the invention are shown and described, and all other embodiments, which can be derived by those skilled in the art without any inventive step, are within the scope of the present invention. The reagents or apparatus used are not indicated by the manufacturer and are commercially available.
The present invention is described in further detail below with reference to specific examples.
Example 1
A plant fiber microwave liquefaction method comprises the following steps:
step one, uniformly mixing 100 parts of mechanically crushed plant fiber, 8 parts of microbial agent and 22 parts of water, sealing, fermenting for 5 days, opening a pool, and airing until the water content is 7.5%;
step two, putting 100 parts of the mixture obtained in the step one, 5 parts of catalyst, 10 parts of hydrogen donor and 250 parts of liquefier into a microwave reaction kettle with a stirrer, setting the frequency of the microwave reaction kettle to be 2500Hz, heating to 160 ℃, filling hydrogen into the reaction kettle, pressurizing to 3.5MPa, stirring, preserving heat for 18min, and completing plant fiber liquefaction;
step three, after naturally cooling to 90 ℃, introducing cooling water into the reaction kettle, cooling the reaction kettle to room temperature, and discharging hydrogen;
and step four, filtering the liquid in the reaction kettle to remove residues, and distilling the obtained liquid at 48 ℃ by using a rotary evaporator, wherein the distilled liquid is the plant fiber liquefied product.
Particularly preferably, the microbial agent comprises a mixture consisting of 3 parts of cellulomonas, 2 parts of phosphate-solubilizing flora, 1 part of nitrobacteria, 1 part of thermoactinomycetes, 1 part of thermomonospora, 2 parts of yeast and 2 parts of humicola.
Particularly preferably, the catalyst is methyl benzene sulfonic acid and is analytically pure.
Particularly preferably, the hydrogen donor is a mixture consisting of 3 parts of phenol, 1 part of hydroquinone, 1 part of trimethylphenol and 1 part of methoxyphenol
Particularly preferably, the liquefying agent is a mixture consisting of 5 parts of alcohol solvent and 1 part of salt solution
Particularly preferably, the alcohol solvent is one or a mixture of methanol, ethanol, glycol, glycerol, isopropanol and polyethylene glycol; the salt solution is a 10% ammonium bifluoride solution.
Particularly preferably, the plant fiber comprises one or a mixture of several of bagasse, manioc waste, bamboo waste, corn straw, sorghum straw, wheat straw, beanstalk, fiber grass, wheat straw, reed and rice straw, and the water content of the plant fiber is 4.5%.
The liquefaction rate of the plant fiber in the embodiment is 96.6%, and the calculation method comprises the following steps: (weight of plant fiber-weight of residue)/weight of plant fiber × 100%.
Example 2
A plant fiber microwave liquefaction method comprises the following steps:
step one, uniformly mixing 100 parts of mechanically crushed plant fiber, 0.5 part of microbial agent and 25 parts of water, sealing, fermenting for 5 days, opening a pool, and airing until the water content is 7%;
step two, putting 100 parts of the mixture obtained in the step one, 8 parts of catalyst, 8 parts of hydrogen donor and 280 parts of liquefier into a microwave reaction kettle with a stirrer, setting the frequency of the microwave reaction kettle to be 2500Hz, heating to 150 ℃, filling hydrogen into the reaction kettle, pressurizing to 4MPa, stirring, keeping the temperature for 15min, and completing plant fiber liquefaction;
step three, after naturally cooling to 90 ℃, introducing cooling water into the reaction kettle, cooling the reaction kettle to room temperature, and discharging hydrogen;
and step four, filtering the liquid in the reaction kettle to remove residues, and distilling the obtained liquid at 45-50 ℃ by using a rotary evaporator, wherein the distilled liquid is the plant fiber liquefied product.
Particularly preferably, the microbial agent comprises a mixture consisting of 3 parts of cellulomonas, 1 part of bacillus, 2 parts of growth flora, 1 part of thermoactinomycetes, 1 part of penicillium and 1 part of humicola.
Particularly preferably, the catalyst is nitric acid, and the catalyst is analytically pure and has a mass fraction of 65%.
Particularly preferably, the hydrogen donor is one or more of phenol, hydroquinone, catechol, p-methyl phenol, trimethylphenol and methoxyphenol.
Particularly preferably, the hydrogen donor is a mixture consisting of 1 part of hydroquinone, 1 part of catechol and 1 part of methoxyphenol
Particularly preferably, the liquefying agent is a mixture of an alcohol solvent and a salt solution.
Particularly preferably, the liquefying agent is a mixture consisting of 5 parts of alcohol solvent and 1 part of salt solution
Particularly preferably, the alcohol solvent is one or a mixture of methanol, ethanol, glycol, glycerol, isopropanol and polyethylene glycol; the salt solution is a 10% ammonium bifluoride solution.
Particularly preferably, the plant fiber comprises one or a mixture of several of bagasse, manioc waste, bamboo waste, corn straw, sorghum straw, wheat straw, beanstalk, fiber grass, wheat straw, reed and rice straw, and the water content of the plant fiber is 4%.
The liquefaction ratio of the plant fiber in this example was 95.5%.
Example 3
A plant fiber microwave liquefaction method comprises the following steps:
step one, uniformly mixing 100 parts of mechanically crushed plant fiber, 1 part of microbial agent and 20 parts of water, sealing, fermenting for 6 days, opening a pool, and airing until the water content is 6.5%; firstly, the plant fiber is fermented, so that the subsequent liquefaction reaction condition of the plant fiber is mild, the reaction temperature can be reduced, the reaction time is shortened, and the liquefaction rate is improved.
Step two, putting 100 parts of the mixture obtained in the step one, 2 parts of catalyst, 12 parts of hydrogen donor and 200 parts of liquefier into a microwave reaction kettle with a stirrer, setting the frequency of the microwave reaction kettle to be 2500Hz, heating to 170 ℃, filling hydrogen into the reaction kettle, pressurizing to 3MPa, stirring, preserving heat for 25min, and completing plant fiber liquefaction;
step three, after naturally cooling to 90 ℃, introducing cooling water into the reaction kettle, cooling the reaction kettle to room temperature, and discharging hydrogen;
and step four, filtering the liquid in the reaction kettle to remove residues, and distilling the obtained liquid at 45-50 ℃ by using a rotary evaporator, wherein the distilled liquid is the plant fiber liquefied product.
Particularly preferably, the microbial agent comprises a mixture consisting of 3 parts of cellulomonas, 1 part of bacillus, 1 part of nitrobacter, 2 parts of thermoactinomyces, 1 part of thermomonospora, 1 part of penicillium and 2 parts of humicola.
Particularly preferably, the catalyst is phosphoric acid, and the mass fraction of the catalyst is 85% of the analytically pure catalyst.
Particularly preferably, the hydrogen donor is one or more of phenol, hydroquinone, catechol, p-methyl phenol, trimethylphenol and methoxyphenol.
Particularly preferably, the hydrogen donor is a mixture consisting of 3 parts of phenol, 1 part of catechol, 1 part of trimethylphenol and 1 part of methoxyphenol
Particularly preferably, the liquefying agent is a mixture of an alcohol solvent and a salt solution.
Particularly preferably, the liquefying agent is a mixture consisting of 5 parts of alcohol solvent and 1 part of salt solution
Particularly preferably, the alcohol solvent is one or a mixture of methanol, ethanol, glycol, glycerol, isopropanol and polyethylene glycol; the salt solution is a 10% ammonium bifluoride solution.
Particularly preferably, the plant fiber comprises one or a mixture of several of bagasse, manioc waste, bamboo waste, corn straw, sorghum straw, wheat straw, beanstalk, fiber grass, wheat straw, reed and rice straw, and the water content of the plant fiber is 4.8%.
The liquefaction rate of the plant fiber in the example was 95.8%
The present invention has been described in detail with reference to the examples and comparative examples, but the present invention is not limited to the examples and comparative examples, and various changes can be made without departing from the concept of the present invention within the knowledge of those skilled in the art.

Claims (7)

1. The microwave plant fiber liquefying method is characterized by comprising the following steps of:
step one, uniformly mixing 100 parts of mechanically crushed plant fiber, 0.5-1 part of microbial agent and 20-25 parts of water, sealing, fermenting for 5-6 days, opening a pool and airing until the water content is lower than 8%;
step two, putting 100 parts of the mixture obtained in the step one, 2-8 parts of catalyst, 8-12 parts of hydrogen donor and 280 parts of liquefying agent 200 plus materials into a microwave reaction kettle with a stirrer, setting the frequency of the microwave reaction kettle to be 2500Hz, heating to 150 plus materials and 170 ℃, filling hydrogen into the reaction kettle and pressurizing to 3-4MPa, stirring and preserving heat for 15-25min, and completing plant fiber liquefaction;
step three, after naturally cooling to 90 ℃, introducing cooling water into the reaction kettle, cooling the reaction kettle to room temperature, and discharging hydrogen;
step four, filtering the liquid in the reaction kettle to remove residues, and distilling the obtained liquid at 45-50 ℃ by using a rotary evaporator, wherein the distilled liquid is the plant fiber liquefied product;
the microbial agent comprises one or more of cellulomonas, bacillus, phosphorus-solubilizing flora, nitrate flora, growth flora, high-temperature actinomycetes, high-temperature monospore, yeast, penicillium and humicola;
the catalyst is methyl benzene sulfonic acid, nitric acid or phosphoric acid;
the hydrogen donor is one or a mixture of phenol, hydroquinone, catechol, p-methyl phenol, trimethylphenol and methoxyphenol.
2. The microwave liquefaction method of plant fiber according to claim 1, characterized in that: the microbial agent comprises a mixture consisting of 3 parts of cellulomonas, 2 parts of phosphate-solubilizing flora, 1 part of nitrobacteria, 1 part of high-temperature actinomycetes, 1 part of high-temperature monospore, 2 parts of yeast and 2 parts of humicola.
3. The microwave liquefaction method of plant fiber according to claim 1, characterized in that: the hydrogen donor is a mixture consisting of 3 parts of phenol, 1 part of hydroquinone, 1 part of trimethylphenol and 1 part of methoxyphenol.
4. The microwave liquefaction method of plant fiber according to claim 1, characterized in that: the liquefying agent is a mixture consisting of an alcohol solvent and a salt solution.
5. The microwave liquefaction method of plant fiber according to claim 4, characterized in that: the liquefying agent is a mixture consisting of 5 parts of alcohol solvent and 1 part of salt solution.
6. The microwave liquefaction method of plant fiber according to claim 5, characterized in that: the alcohol solvent is one or a mixture of methanol, ethanol, glycol, glycerol, isopropanol and polyethylene glycol; the salt solution is a 10% ammonium bifluoride solution.
7. The microwave liquefaction method of plant fiber according to claim 1, characterized in that: the plant fiber comprises one or a mixture of several of bagasse, manioc waste, bamboo waste, corn straw, sorghum straw, wheat straw, beanstalk, fiber grass, wheat straw, reed and rice straw, and the water content of the plant fiber is lower than 5%.
CN201610614719.3A 2016-07-28 2016-07-28 Plant fiber microwave liquefaction method Expired - Fee Related CN107540850B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610614719.3A CN107540850B (en) 2016-07-28 2016-07-28 Plant fiber microwave liquefaction method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610614719.3A CN107540850B (en) 2016-07-28 2016-07-28 Plant fiber microwave liquefaction method

Publications (2)

Publication Number Publication Date
CN107540850A CN107540850A (en) 2018-01-05
CN107540850B true CN107540850B (en) 2020-02-07

Family

ID=60966721

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610614719.3A Expired - Fee Related CN107540850B (en) 2016-07-28 2016-07-28 Plant fiber microwave liquefaction method

Country Status (1)

Country Link
CN (1) CN107540850B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1486364A (en) * 2001-01-10 2004-03-31 ������������ʽ���� Vegetable fiber-digesting agent and method of processing vegetable waste by using the same
CN102504275A (en) * 2011-11-21 2012-06-20 浙江省林业科学研究院 Production method of bamboo phenolic alcohol liquefied products
CN102731797A (en) * 2012-07-10 2012-10-17 中国林业科学研究院亚热带林业研究所 Method for liquefying bamboo wood
CN102939323A (en) * 2010-05-12 2013-02-20 国际壳牌研究有限公司 Process for liquefying a cellulosic material
CN105111462A (en) * 2015-08-04 2015-12-02 华南理工大学 Liquefied plant fiber feedstock and preparation method therefor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1486364A (en) * 2001-01-10 2004-03-31 ������������ʽ���� Vegetable fiber-digesting agent and method of processing vegetable waste by using the same
CN102939323A (en) * 2010-05-12 2013-02-20 国际壳牌研究有限公司 Process for liquefying a cellulosic material
CN102504275A (en) * 2011-11-21 2012-06-20 浙江省林业科学研究院 Production method of bamboo phenolic alcohol liquefied products
CN102731797A (en) * 2012-07-10 2012-10-17 中国林业科学研究院亚热带林业研究所 Method for liquefying bamboo wood
CN105111462A (en) * 2015-08-04 2015-12-02 华南理工大学 Liquefied plant fiber feedstock and preparation method therefor

Also Published As

Publication number Publication date
CN107540850A (en) 2018-01-05

Similar Documents

Publication Publication Date Title
Xing et al. Novel dihydrogen-bonding deep eutectic solvents: Pretreatment of rice straw for butanol fermentation featuring enzyme recycling and high solvent yield
Solarte-Toro et al. Acid pretreatment of lignocellulosic biomass for energy vectors production: a review focused on operational conditions and techno-economic assessment for bioethanol production
Peng et al. Compositional changes of rice straw fibers after pretreatment with diluted acetic acid: towards enhanced biomethane production
Badger Ethanol from cellulose: a general review
Guo et al. Heteropoly acids enhanced neutral deep eutectic solvent pretreatment for enzymatic hydrolysis and ethanol fermentation of Miscanthus x giganteus under mild conditions
Nanda et al. Pathways of lignocellulosic biomass conversion to renewable fuels
Raj et al. Improved co-production of ethanol and xylitol from low-temperature aqueous ammonia pretreated sugarcane bagasse using two-stage high solids enzymatic hydrolysis and Candida tropicalis
Bolivar-Telleria et al. Second-generation bioethanol from coconut husk
Liang et al. Liquefaction of crop residues for polyol production
US20130078698A1 (en) Process for fractionation of biomass
Niju et al. Pretreatment of lignocellulosic sugarcane leaves and tops for bioethanol production
Xu et al. Influence of surfactant-free ionic liquid microemulsions pretreatment on the composition, structure and enzymatic hydrolysis of water hyacinth
Cheng et al. Resource recovery from lignocellulosic wastes via biological technologies: Advancements and prospects
Singh et al. Valorization of jute (Corchorus sp.) biomass for bioethanol production
CN101148458A (en) Cogeneration method for sugar and acetylpropionic acid by utilizing lignocellulose-like biomass
Zheng et al. Achieving high ethanol yield by co-feeding corncob residues and tea-seed cake at high-solids simultaneous saccharification and fermentation
Zhang et al. Alkaline hydrogen peroxide pretreatment combined with bio-additives to boost high-solids enzymatic hydrolysis of sugarcane bagasse for succinic acid processing
Silveira et al. Second generation ethanol production: potential biomass feedstock, biomass deconstruction, and chemical platforms for process valorization
Guo et al. Integrated biorefinery of bamboo for fermentable sugars, native-like lignin, and furfural production by novel deep eutectic solvents treatment
CN109880865B (en) Efficient separation and conversion method of corn straws
Rathour et al. Non-food crops derived lignocellulose biorefinery for sustainable production of biomaterials, biochemicals and bioenergy: a review on trends and techniques
Camargo et al. Biogas from lignocellulosic feedstock: A review on the main pretreatments, inocula and operational variables involved in anaerobic reactor efficiency
US20140065683A1 (en) Method for producing ethanol and solvents from lignocellulosic biomass including the recirculation of a butyl wine obtained by fermenting pentoses
Sahu Appropriateness of rose (Rosa hybrida) for bioethanol conversion with enzymatic hydrolysis: Sustainable development on green fuel production
US20130017585A1 (en) Process for the production of alcohols and/or solvents from papermaking pulps with recycling of non-hydrolyzed vegetation

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20200207

Termination date: 20210728

CF01 Termination of patent right due to non-payment of annual fee