CN1763208A - Separation and extraction method for lignin hydrolyzed by enzyme - Google Patents
Separation and extraction method for lignin hydrolyzed by enzyme Download PDFInfo
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- CN1763208A CN1763208A CN 200510099747 CN200510099747A CN1763208A CN 1763208 A CN1763208 A CN 1763208A CN 200510099747 CN200510099747 CN 200510099747 CN 200510099747 A CN200510099747 A CN 200510099747A CN 1763208 A CN1763208 A CN 1763208A
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Abstract
The present invention discloses two enzymolyzed lignin separating and extracting methods. Enzymolyzing saccharides in corn stalk with microbe to prepare alcohol is one effective way of solving energy crisis problem, and the present invention separates and extracts enzymolyzed lignin from microbe enzymolyzed corn stalk residue by means of organic solvent extraction and inorganic chemical treatment. During microbe fermentation and residue separation for preparing alcohol, enzymolyzed lignin is always in relatively mild state, so that the enzymolyzed lignin has the active groups of lignin well maintained. The present invention is suitable for modified lignin product in high economic value.
Description
Technical field:
The present invention relates to the technology and the prescription of separation and Extraction enzymolysis xylogen from the residue of microorganism enzymolysis corn stalk.
Background technology:
Tellurian petroleum resources are exhausted day by day, and the exploitation of substitute energy is extremely urgent.Energy ethanol is that each state adopts the starch conversion method to prepare energy ethanol all at the substitute products of a kind of gasoline of developing at present, and 1 ton of alcohol of every production needs 3.3-3.5 ton starch.From cost keeping, this method prepares alcohol and loses money.Corn is a kind of staple food crop, and countries in the world maize planting area is rather wide, all can produce hundred million tons of maize straws of 6-7 every year.There is hundred million tons of maize straws of 2-3 every year in China, except small part as feed or the preparation biogas, the most of burning is plant ash, not only wasted resource but also contaminate environment.Maize straw contains a large amount of polysaccharide fractions, and in order to save food and to reduce the manufacturing cost of energy ethanol, Chinese scholars is being explored biotechnologys such as utilizing microorganism, enzyme catalysis allows the polysaccharide in the maize straw change into energy ethanol.USDOE and Swedish government all drop into the huge fund support and develop this valuable source, the biotech company of Sweden, the U.S. is doing a lot of work aspect the bacterial screening of microorganism culturing, saccharification alcohol in the world, designed the test battery production technique, but they prepare the not further exploitation of residue of energy ethanol to microorganism enzymolysis corn stalk, only residue is acted as a fuel and burn, therefore economic benefit is not high, can't apply.Surplus professor generation Yuan of domestic Nanjing Forestry University has also carried out successful test, utilize microorganism enzymolysis corn stalk to prepare energy ethanol, can obtain 1 ton of energy ethanol and 1 ton of residue with 6.5 tons of corn stalks, same because of the xylogen that does not fully utilize in the residue, the pilot scale of this project does not stop because of economic benefit is good.Microorganism enzymolysis corn stalk prepares the enzymolysis xylogen that contains 40-50% in the residue of energy ethanol, the process of enzymolysis corn stalk is relatively gentleer, enzymolysis xylogen has kept the chemically reactive of natural lignin preferably, adopt appropriate means to separate, extract enzymolysis xylogen and can effectively utilize waste material, improve the economic benefit that microorganism enzymolysis corn stalk prepares energy ethanol, help applying of this environmental protection project, help Sustainable development.
Summary of the invention:
The invention solves existing microorganism enzymolysis corn stalk and prepare the existing problem of energy ethanol technology, provide two kinds production cost is low, processing method is easy, can keep preferably again the method for its chemically active enzymolysis xylogen separation and Extraction.
Technical scheme of the present invention has two kinds.The one, organic solvent extractionprocess, the 2nd, inorganics extraction method.
Concrete its step comprises:
1 organic solvent extractionprocess: the residue that utilizes organic solvent extraction enzymolysis corn stalk, enzymolysis xylogen is dissolved in the organic solvent and extracts, by filtering enzymolysis xylogen solution is separated with the impurity of other insoluble organic solvents, solution obtains enzymolysis xylogen after solvent is sloughed in underpressure distillation.
2 inorganics extraction methods: utilize xylogen can be dissolved in the characteristics of the aqueous phase system of inorganic base substance, enzymolysis xylogen in the residue of enzymolysis corn stalk is dissolved in the inorganic alkaline solution, separate with other components by filtering, enzymolysis xylogen solution through in the acid solution and after, enzymolysis xylogen is separated out with precipitation, obtains enzymolysis xylogen through centrifugation, washing after drying again.
The present invention has following advantage:
1, the organic solvent extractionprocess of the present invention's employing is under certain temperature, pressure condition, the residue for preparing energy ethanol with one or more mixed organic solvents extraction microorganism enzymolysis corn stalks, enzymolysis xylogen is dissolved among the organic solvent, makes it separate with other components in the residue.Outside desolventizing, the organic solvent extraction process do not add other chemical agents, the enzymolysis xylogen purity height that obtains, and ash oontent reduces by tens times than raw material.The enzymolysis xylogen that organic solvent extractionprocess obtains is dissolved in organic solvent easily, helps carrying out chemical modification in the organic phase system.Different according to the type of using solvent and extraction conditions can obtain the enzymolysis xylogen of material quantity 20-43%.
2. the inorganics extraction method of the present invention's employing is under certain temperature, pressure condition, the residue for preparing energy ethanol with inorganic alkaline aqueous solution extraction microorganism enzymolysis corn stalk, enzymolysis xylogen is dissolved among the inorganic alkaline aqueous solution, after making it and other components in the residue are separated by filtration, add acid neutralization alkalescence, enzymolysis xylogen is separated out with precipitation, according to the difference of extraction conditions, can obtain the enzymolysis xylogen of material quantity 30-48%.
3, the enzymolysis xylogen ash oontent is low, and the chemically reactive height is fit to it is carried out chemical modification, preparation enzymolysis xylogen derivative, and enzymolysis xylogen and derivative thereof keep more multi-active base group than traditional sulfonated lignin, thereby better modified effect is arranged.
4, the infrared spectra of the enzymolysis xylogen that makes of organic solvent extractionprocess of the present invention and inorganics extraction method and the test result of UV spectrum show that their molecular structure is basic identical, the active group that has kept natural lignin preferably, its chemical property is not subjected to preparation method's influence, can be used to prepare corresponding lignin derivative.
5, the present invention makes to such an extent that enzymolysis xylogen and derivative thereof can be used for engineering materialss such as rubber, plastics, tackiness agent, and the properties-correcting agent of coating or matrix material is of wide application, and has higher economic value.Of the present invention applying improved the economic benefit that microorganism enzymolysis corn stalk prepares energy ethanol greatly, helps applying of this environmental protection project, helps Sustainable development.
6, utilize the residue separation and Extraction enzymolysis xylogen of enzymolysis corn stalk, both can adopt organic solvent extractionprocess, also can adopt the inorganics extraction method, any method both can be carried out separately, also can be carried out repeatedly or two kinds of methods hocket, and can improve 1-6% to the yield of once extracting the enzymolysis xylogen that obtains with the multiple extraction ratio of a collection of residue separately.
Description of drawings:
The UV spectrum of the enzymolysis xylogen that Fig. 1 makes for different methods: 4h, Na and nh represent to use tetrahydrofuran (THF) respectively, the resulting enzymolysis xylogen of residue of sodium hydroxide and ammonia treatment enzymolysis corn stalk.
The infrared spectra of the enzymolysis xylogen that Fig. 2 makes for different methods: 4h, Na and nh represent to use tetrahydrofuran (THF) respectively, the resulting enzymolysis xylogen of residue of sodium hydroxide and ammonia treatment enzymolysis corn stalk.
Embodiment:
1. organic solvent extractionprocess:
(1) processing step: the residue of enzymolysis corn stalk mixed extracting with organic solvent, the temperature of extraction process is 30-100 ℃, pressure is 0-1.0MPa, time is 0.5-6 hour, make the residue and the organic solvent of enzymolysis corn stalk fully react dissolving, filtering separation, and, can obtain enzymolysis xylogen with the filtrate evaporation.
(2) raw material is formed and the total amount portion rate:
100 parts of the residues of enzymolysis corn stalk
Organic solvent 200-1000 part
Described organic solvent is one or more in dioxane, tetrahydrofuran (THF), trichloromethane, methylene dichloride, dimethyl formamide, pimelinketone, ethanol, Virahol and the acetone
2. inorganics extraction method:
(1) processing step: the residue of enzymolysis corn stalk is mixed with inorganic alkaline solution, heating, pressurization through certain hour, make the residue and the inorganic alkaline solution of enzymolysis corn stalk fully react dissolving, filtering separation, in filtrate, add weak (or rare) acid and neutralize, and add water the enzymolysis xylogen precipitation is separated out; Enzymolysis xylogen washing, filtration, oven dry with separating out can obtain enzymolysis xylogen.
(2) raw material is formed and the total amount portion rate:
100 parts of the residues of enzymolysis corn stalk
Concentration is inorganic alkaline solution 200-1000 part of 1-35%
Described inorganic alkaline solution is: sodium hydroxide, potassium hydroxide, calcium hydroxide, ammoniacal liquor or the like.
The raw material of preparation enzymolysis xylogen is the residue that microorganism enzymolysis corn stalk prepares energy ethanol, and wherein the content of enzymolysis xylogen is 40-50%.Organic solvent and alkaline inorganics all can be bought in Chemicals market.
Concrete processing step and condition:
1. organic solvent extractionprocess: the residue of 100 parts of enzymolysis corn stalks, be dissolved in 200-1000 part organic solvent, stir and promote that enzymolysis xylogen is dissolved in the organic solvent, with mixture heating up to 30-100 ℃ and be pressurized to 0-1.0MPa, through 0.5-6.0 hour, by filtering enzymolysis xylogen solution is separated with the impurity of other insoluble organic solvents, solution obtains enzymolysis xylogen after solvent is sloughed in distillation.
2. inorganics extraction method: the residue of 100 parts of enzymolysis corn stalks, being dissolved in 200-1000 part concentration is that 1-35% oxyhydroxide or concentration are in the 1-35% ammoniacal liquor, stir and promote that enzymolysis xylogen is dissolved in the alkaline aqueous solution, mixture heating up is arrived 30-100 ℃, and be pressurized to pressure 0-1.0MPa, through 0.5-6.0 hour, by filtering enzymolysis xylogen solution is separated with the impurity of other insoluble alkaline aqueous solutions, solution is after concentration is neutralized to neutrality (PH=7) for 1-35% hydrochloric acid, stir on one side, the water that adds 3-8 times of volume of this solution on one side, left standstill 10-60 minute, the enzymolysis xylogen precipitation is separated out, washing, filtering separation also obtains enzymolysis xylogen to precipitation oven dry.
Embodiment 1.
Take by weighing the residue of 100 gram enzymolysis corn stalks, put into 1500 milliliters there-necked flask, the mixing solutions (volume ratio of tetrahydrofuran (THF) and dioxane is 2: 1) that adds 600 milliliters of tetrahydrofuran (THF)s, dioxane, stir and promoted that enzymolysis xylogen was dissolved in the organic solvent in 15 minutes, be heated to 90 ℃, pressure 0.3MPa then, kept 1.5 hours, by filtering enzymolysis xylogen solution is separated with the impurity of other insoluble organic solvents, solution obtains enzymolysis xylogen 40.20 grams after solvent is sloughed in distillation.
Embodiment 2.
Take by weighing the residue of 100 parts of enzymolysis corn stalks, put into 1500 milliliters there-necked flask, adding 500 ml concns is in 10% sodium hydroxide solution, stir and promoted that enzymolysis xylogen was dissolved in the alkali aqueous solution in 15 minutes, be heated to 95 ℃ and be forced into 0.3MPa then, kept 1.0 hours, by filtering the insoluble impurity of enzymolysis xylogen solution and other is separated, after 152 milliliter of 30% hydrochloric acid of solution adding is neutralized to neutrality (PH=7), stir on one side,, left standstill 30 minutes Yi Bian add the water of 4 times of volumes of this solution, the enzymolysis xylogen precipitation is separated out filtering separation, water washing and precipitating also obtains enzymolysis xylogen 45.31 grams to precipitation oven dry.
Embodiment 3
Take by weighing the residue of 100 parts of enzymolysis corn stalks, put into 1500 milliliters there-necked flask, adding 350 ml concns is in 15% ammoniacal liquor, stir and promoted that enzymolysis xylogen was dissolved in the ammonia soln in 15 minutes, be heated to 95 ℃ and be forced into 0.3MPa then, kept 1.0 hours, by filtering the insoluble impurity of enzymolysis xylogen solution and other is separated, after 370 milliliter of 30% hydrochloric acid of solution adding is neutralized to neutrality (PH=7), stir on one side, add the water of 4 times of volumes of this solution on one side, left standstill 30 minutes, enzymolysis xylogen precipitation is separated out, filtering separation, and water washing and precipitating also obtains enzymolysis xylogen 42.52 grams to the precipitation oven dry.
Table 1. enzymolysis xylogen ash measured result
| Sample | Enzymolysis corn stalk residue | Enzymolysis xylogen embodiment 1 | Enzymolysis xylogen embodiment 2 | Enzymolysis xylogen embodiment 3 | Calcium lignosulfonate |
| Ash oontent/% | 11.45 | 0.34 | 0.38 | 0.35 | 21.2 |
Claims (11)
1, a kind of separating and extracting method of enzymolysis xylogen, it is characterized in that: enzymolysis xylogen is dissolved in the organic solvent extracts, by filtration the impurity that enzymolysis xylogen solution and other are insoluble to organic solvent is separated, solution obtains enzymolysis xylogen after solvent is sloughed in underpressure distillation.
2, the separating and extracting method of enzymolysis xylogen according to claim 1, it is characterized in that: the residue of enzymolysis corn stalk is mixed with organic solvent, through heating, pressurization, make the residue of enzymolysis corn stalk and organic solvent fully react dissolving, after filtering separation, filtrate is evaporated.
3, the separating and extracting method of enzymolysis xylogen according to claim 2 is characterized in that: the Heating temperature of extraction process is 30-100 ℃, and pressure is 0-1.0MPa, and the time is 0.5-6 hour.
4, the separating and extracting method of enzymolysis xylogen according to claim 3 is characterized in that: its raw material is formed and ratio of weight and number is:
100 parts of the residues of enzymolysis corn stalk
Organic solvent 200-1000 part.
5, according to the separating and extracting method of claim 1 or 2 or 4 described enzymolysis xylogens, it is characterized in that: described organic solvent is: one or more in dioxane, tetrahydrofuran (THF), trichloromethane, methylene dichloride, dimethyl formamide, pimelinketone, ethanol, Virahol and the acetone.
6, a kind of separating and extracting method of enzymolysis xylogen, it is characterized in that: enzymolysis xylogen is dissolved in the inorganic alkaline solution, separate with other insoluble components by filtering, enzymolysis xylogen solution through in the acid solution and after, add water enzymolysis xylogen is separated out with precipitation, obtain enzymolysis xylogen through centrifugation, washing, drying again.
7, the separating and extracting method of enzymolysis xylogen according to claim 6, it is characterized in that: the residue of enzymolysis corn stalk is mixed with inorganic alkaline solution, through heating, pressurization, make the residue of enzymolysis corn stalk and inorganic alkaline solution fully react dissolving.
8, the separating and extracting method of enzymolysis xylogen according to claim 7 is characterized in that: with the temperature of heat be 30-100 ℃, the pressure of pressurization be 0-1.0MPa, and through 0.5-6.0 hour.
9, the separating and extracting method of enzymolysis xylogen according to claim 8 is characterized in that: its raw material is formed and ratio of weight and number is:
100 parts of the residues of enzymolysis corn stalk
Concentration is inorganic alkaline solution 200-1000 part of 1-35%.
10, according to the separating and extracting method of claim 6 or 7 or 9 described enzymolysis xylogens, it is characterized in that: described inorganic alkaline solution is one or more in sodium hydroxide, potassium hydroxide, calcium hydroxide, the ammoniacal liquor.
11, the separating and extracting method of enzymolysis xylogen according to claim 6 is characterized in that: described acid solution is weak acid or diluted acid.
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| CNB2005100997478A CN100487126C (en) | 2004-12-22 | 2005-09-05 | Separation and extraction method for lignin hydrolyzed by enzyme |
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| CN200410061438 | 2004-12-22 | ||
| CN200410061438.7 | 2004-12-22 | ||
| CNB2005100997478A CN100487126C (en) | 2004-12-22 | 2005-09-05 | Separation and extraction method for lignin hydrolyzed by enzyme |
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| CNA2006101438894A Division CN1982322A (en) | 2005-09-05 | 2005-09-05 | Method for organically separating and extracting enzymic lignin |
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Cited By (13)
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|---|---|---|---|---|
| CN101824155A (en) * | 2010-05-15 | 2010-09-08 | 福州大学 | Method for preparing enzymatic hydrolysis (EH) lignin-dimer fatty acid derivative |
| CN101337981B (en) * | 2008-08-18 | 2010-09-22 | 昆明理工大学 | Method for preparing lignin using bagasse as raw material |
| CN101628920B (en) * | 2009-08-17 | 2011-12-14 | 福州大学 | Comprehensive utilization method of corn cob |
| CN102286545A (en) * | 2010-06-17 | 2011-12-21 | 中国科学院过程工程研究所 | Method for removing butanol fermentation-inhibiting soluble lignin from straw enzymolysis solution |
| CN106008890A (en) * | 2016-06-25 | 2016-10-12 | 仇颖超 | Preparation method of flame-retardant hard polyurethane foam |
| CN106065080A (en) * | 2016-04-06 | 2016-11-02 | 南京林业大学 | A kind of dissolving recycled wood quality extracting method |
| CN108117652A (en) * | 2016-11-29 | 2018-06-05 | 中国石油化工股份有限公司 | A kind of extracting method of enzymolysis xylogen |
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| CN109485871A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of high activity enzymolysis xylogen and preparation method thereof |
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| CN111793220A (en) * | 2020-07-16 | 2020-10-20 | 北京林业大学 | Method for improving antioxidant activity of corn straw enzymatic hydrolysis lignin by separating acetone aqueous solution |
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- 2005-09-05 CN CNB2005100997478A patent/CN100487126C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337981B (en) * | 2008-08-18 | 2010-09-22 | 昆明理工大学 | Method for preparing lignin using bagasse as raw material |
| CN101628920B (en) * | 2009-08-17 | 2011-12-14 | 福州大学 | Comprehensive utilization method of corn cob |
| CN101824155B (en) * | 2010-05-15 | 2012-07-25 | 福州大学 | Method for preparing enzymatic hydrolysis (EH) lignin-dimer fatty acid derivative |
| CN101824155A (en) * | 2010-05-15 | 2010-09-08 | 福州大学 | Method for preparing enzymatic hydrolysis (EH) lignin-dimer fatty acid derivative |
| CN102286545A (en) * | 2010-06-17 | 2011-12-21 | 中国科学院过程工程研究所 | Method for removing butanol fermentation-inhibiting soluble lignin from straw enzymolysis solution |
| CN106065080A (en) * | 2016-04-06 | 2016-11-02 | 南京林业大学 | A kind of dissolving recycled wood quality extracting method |
| CN106008890A (en) * | 2016-06-25 | 2016-10-12 | 仇颖超 | Preparation method of flame-retardant hard polyurethane foam |
| CN108117652A (en) * | 2016-11-29 | 2018-06-05 | 中国石油化工股份有限公司 | A kind of extracting method of enzymolysis xylogen |
| CN108117652B (en) * | 2016-11-29 | 2022-11-11 | 中国石油化工股份有限公司 | Extraction method of enzymatic hydrolysis lignin |
| CN109485065B (en) * | 2017-09-09 | 2021-03-05 | 中国石油化工股份有限公司 | Hierarchical pore molecular sieve and preparation method thereof |
| CN109485871A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of high activity enzymolysis xylogen and preparation method thereof |
| CN109485065A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of multistage porous molecular sieve and preparation method thereof |
| CN108504178A (en) * | 2018-05-10 | 2018-09-07 | 芜湖市创源新材料有限公司 | A kind of preparation method of high stability Environmental-protection water-based ink |
| CN109456634A (en) * | 2018-09-30 | 2019-03-12 | 安徽开林新材料股份有限公司 | A kind of preparation method of wear-resistant paint |
| CN111793220A (en) * | 2020-07-16 | 2020-10-20 | 北京林业大学 | Method for improving antioxidant activity of corn straw enzymatic hydrolysis lignin by separating acetone aqueous solution |
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