CN105968380A - Extraction and refinement method of lignin for carbon fiber preparation - Google Patents
Extraction and refinement method of lignin for carbon fiber preparation Download PDFInfo
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- CN105968380A CN105968380A CN201610351643.XA CN201610351643A CN105968380A CN 105968380 A CN105968380 A CN 105968380A CN 201610351643 A CN201610351643 A CN 201610351643A CN 105968380 A CN105968380 A CN 105968380A
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- lignin
- organic solvent
- extraction
- carbon fiber
- purification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
- D01F9/17—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate from lignin
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Textile Engineering (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Compounds Of Unknown Constitution (AREA)
Abstract
The invention discloses an extraction and refinement method of lignin for carbon fiber preparation. The method comprises the following steps: a. pulverizing wood, dissolving the pulverized wood in an organic solvent I, adding an acidic catalyst, and stirring to react to obtain a raw solution; b. adding distilled water into the raw solution to perform cellulose regeneration; c. separating to obtain a filtrate system; d. dissolving the filtrate system in an organic solvent II to precipitate lignin; e. filtering and separating to obtain coarse lignin, dissolving in an organic solvent III, washing with hydrochloric acid, carrying out vacuum drying and concentrating; and f. dissolving the concentrated lignin in an aether petroleum-ether mixed solution, stirring to generate a precipitate, washing, and carrying out vacuum drying to obtain the refined lignin. The extracted lignin is subjected to coarse preparation and refinement, thereby greatly enhancing the lignin extraction purity. The method has the advantages of high lignin extraction rate and simple technique, and is convenient to operate. The organic solvents can be recovered and reutilized, thereby saving the cost and being beneficial to enhancing the economic benefit and social benefit.
Description
Technical field
The present invention relates to chemical industry and field of material technology, particularly relate to a kind of prepare for carbon fiber the extraction of lignin, process for purification.
Background technology
Carbon fiber is the phosphorus content fibrous material at 90 more than %, there is polytype, its high intensity, high-modulus make various composites, can be used for structural material to use, there is extensive use, but the raw material of carbon fibre material depends on fossil resource, therefore along with the enhancing of people's environmental consciousness and petering out of fossil resource, study hotspot is increasingly turned to utilize Renewable resource to substitute fossil resource and prepares the field of carbon fiber.One of big composition of during wherein lignin is plant three, in most plants, content accounts for 15～30%, and remaining carbon is high, thus can make various carbon materials, has particularly important strategic importance to the national economic development.But in the prior art, the extraction ratio of lignin is relatively low, and the lignin obtained also is rough lignin, and its purity is the highest, needs pretreatment before preparing carbon fiber so that technological process complicates, and cost puts into and strengthens.
Summary of the invention
It is an object of the invention to provide a kind of prepare for carbon fiber the extraction of lignin, process for purification, it is possible to solve in prior art that lignin extraction rate is relatively low, purity is the highest and lignin process the complicated problem such as loaded down with trivial details.
The present invention is directed to above-mentioned technological deficiency be the technical scheme is that
A kind of prepare for carbon fiber the extraction of lignin, process for purification, comprise the steps:
A, timber being placed in pulverizer the powder being ground into 50-100 mesh, be dissolved in by powder in organic solvent I, add acidic catalyst regulation pH to 3-4.5, at 180-200 DEG C, stirring reaction 35-60min i.e. obtains stock solution；
B, in the stock solution that step a obtains add 60-100 times of volume distilled water, carry out cellulose regenerated from room temperature to 150 DEG C in 15-25min, the recovery time is 2-6h；
C, the liquid processed through step b is carried out isolated filtrate systems so that filtrate systems isolated by organic solvent I, acidic catalyst and distilled water；
D, filtrate systems step c obtained are dissolved in organic solvent II and standing, until lignin all separates out；
E, by step d separate out lignin filtrate systems carry out filter the rough lignin of isolated, rough lignin is dissolved in the organic solvent III of 80-120 times of volume, adding concentration is the chlorohydric acid pickling of 36-38%, time is 1-2h, then it is filtrated to get filtrate, and is vacuum dried and concentrates at being placed on 120-150 DEG C；
F, the lignin that step e concentrates is dissolved in the mixed liquor of ether-petroleum ether and stir until precipitating whole generation, thereafter precipitation and centrifugal separation is filtered, centrifugal rotational speed is 6000-8000r/min, and carry out washing at least one times with the mixed liquor of ether-petroleum ether, at being finally placed in 60-80 DEG C, vacuum drying obtains refined lignin.
Further, organic solvent I described in step a is polyhydric alcohol, and described acidic catalyst is any one in hydrochloric acid, sulphuric acid or phosphoric acid.
Further, stock solution described in step b is cooled to 20-55 DEG C before regeneration.
Further, any one or its mixture during organic solvent II described in step d is hexamethylene or dichloromethane.
Further, any one or more than one the combination during organic solvent III described in step d is benzyl alcohol, sorbitol, cinnamyl alcohol, saligenin.
Further, washing times described in step f is 2-3 time.
Further, the organic solvent I described in step a-f, organic solvent II and organic solvent III are all distilled recycling.
The invention has the beneficial effects as follows: the lignin that the present invention extracts arrives refined two steps through rough, substantially increase the purity of lignin extraction, and lignin extraction rate is high, can be directly used for preparing carbon fiber, it is not necessary to carry out pretreatment, enormously simplify the preparation technology of carbon fiber, and technique is simple, easy to operate, organic solvent is all recycled, cost-effective, be conducive to improving the economic and social benefits.
Detailed description of the invention
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment is only used for explaining the present invention, is not intended that the restriction to protection scope of the present invention.
Embodiment 1
A kind of prepare for carbon fiber the extraction of lignin, process for purification, comprise the steps:
A, timber being placed in pulverizer the powder being ground into 50 mesh, be dissolved in polyhydric alcohol by powder, add salt acid for adjusting pH to 3, at 180 DEG C, stirring reaction 35min i.e. obtains stock solution, and polyhydric alcohol is distilled recycling；
B, in the stock solution that step a obtains add 60 times of volumes distilled water, carry out cellulose regenerated from room temperature to 150 DEG C in 15min, the recovery time is 2h, and stock solution is cooled to 20 DEG C before regeneration；
C, the liquid processed through step b is carried out isolated filtrate systems so that filtrate systems isolated by polyhydric alcohol, hydrochloric acid and distilled water；
D, filtrate systems step c obtained are dissolved in hexamethylene and standing, until lignin all separates out, hexamethylene is distilled recycling；
E, by step d separate out lignin filtrate systems carry out filter the rough lignin of isolated, rough lignin is dissolved in the mixture of the benzyl alcohol of 80 times of volumes, sorbitol, adding concentration is the chlorohydric acid pickling of 36%, time is 1h, then filtrate it is filtrated to get, and be placed at 120 DEG C and be vacuum dried and concentrate, benzyl alcohol, the mixture of sorbitol are distilled recycling；
F, the lignin that step e concentrates is dissolved in the mixed liquor of ether-petroleum ether and stir until precipitating whole generation, thereafter precipitation and centrifugal separation is filtered, centrifugal rotational speed is 6000r/min, and the washing of 2 times is carried out with the mixed liquor of ether-petroleum ether, finally it is placed at 60 DEG C vacuum drying and obtains refined lignin.
Embodiment 2
A kind of prepare for carbon fiber the extraction of lignin, process for purification, comprise the steps:
A, timber being placed in pulverizer the powder being ground into 100 mesh, be dissolved in polyhydric alcohol by powder, add sulfur acid for adjusting pH to 4, at 200 DEG C, stirring reaction 45min i.e. obtains stock solution, and polyhydric alcohol is distilled recycling；
B, in the stock solution that step a obtains add 80 times of volumes distilled water, carry out cellulose regenerated from room temperature to 150 DEG C in 20min, the recovery time is 4h, and stock solution is cooled to 40 DEG C before regeneration；
C, the liquid processed through step b is carried out isolated filtrate systems so that filtrate systems isolated by polyhydric alcohol, sulphuric acid and distilled water；
D, filtrate systems step c obtained are dissolved in dichloromethane and standing, until lignin all separates out, dichloromethane is distilled recycling；
E, by step d separate out lignin filtrate systems carry out filter the rough lignin of isolated, rough lignin is dissolved in the mixture of the sorbitol of 100 times of volumes, cinnamyl alcohol, adding concentration is the chlorohydric acid pickling of 37%, time is 2h, then filtrate it is filtrated to get, and be placed at 120 DEG C and be vacuum dried and concentrate, sorbitol, the mixture of cinnamyl alcohol are distilled recycling；
F, the lignin that step e concentrates is dissolved in the mixed liquor of ether-petroleum ether and stir until precipitating whole generation, thereafter precipitation and centrifugal separation is filtered, centrifugal rotational speed is 7000r/min, and the washing of 2 times is carried out with the mixed liquor of ether-petroleum ether, finally it is placed at 70 DEG C vacuum drying and obtains refined lignin.
Embodiment 3
A kind of prepare for carbon fiber the extraction of lignin, process for purification, comprise the steps:
A, timber being placed in pulverizer the powder being ground into 100 mesh, be dissolved in polyhydric alcohol by powder, add phosphorus acid for adjusting pH to 4.5, at 200 DEG C, stirring reaction 60min i.e. obtains stock solution, and polyhydric alcohol is distilled recycling；
B, in the stock solution that step a obtains add 100 times of volumes distilled water, carry out cellulose regenerated from room temperature to 150 DEG C in 25min, the recovery time is 6h, and stock solution is cooled to 55 DEG C before regeneration；
C, the liquid processed through step b is carried out isolated filtrate systems so that filtrate systems isolated by polyhydric alcohol, phosphoric acid and distilled water；
D, filtrate systems step c obtained are dissolved in the mixed liquor of hexamethylene, dichloromethane and standing, until lignin all separates out, hexamethylene, the mixed liquor of dichloromethane are distilled recycling；
E, by step d separate out lignin filtrate systems carry out filter the rough lignin of isolated, rough lignin is dissolved in the mixture of the sorbitol of 120 times of volumes, cinnamyl alcohol, saligenin, adding concentration is the chlorohydric acid pickling of 38%, time is 2h, then filtrate it is filtrated to get, and be placed at 150 DEG C and be vacuum dried and concentrate, sorbitol, cinnamyl alcohol, the mixture of saligenin are distilled recycling；
F, the lignin that step e concentrates is dissolved in the mixed liquor of ether-petroleum ether and stir until precipitating whole generation, thereafter precipitation and centrifugal separation is filtered, centrifugal rotational speed is 8000r/min, and the washing of 3 times is carried out with the mixed liquor of ether-petroleum ether, finally it is placed at 80 DEG C vacuum drying and obtains refined lignin.
The invention has the beneficial effects as follows: the lignin that the present invention extracts arrives refined two steps through rough, substantially increase the purity of lignin extraction, and lignin extraction rate is high, can be directly used for preparing carbon fiber, it is not necessary to carry out pretreatment, enormously simplify the preparation technology of carbon fiber, and technique is simple, easy to operate, organic solvent is all recycled, cost-effective, be conducive to improving the economic and social benefits.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (7)
1. the extraction for lignin prepared for carbon fiber, process for purification, it is characterised in that: comprise the steps:
A, timber being placed in pulverizer the powder being ground into 50-100 mesh, be dissolved in by powder in organic solvent I, add acidic catalyst regulation pH to 3-4.5, at 180-200 DEG C, stirring reaction 35-60min i.e. obtains stock solution；
B, in the stock solution that step a obtains add 60-100 times of volume distilled water, carry out cellulose regenerated from room temperature to 150 DEG C in 15-25min, the recovery time is 2-6h；
C, the liquid processed through step b is carried out isolated filtrate systems so that filtrate systems isolated by organic solvent I, acidic catalyst and distilled water；
D, filtrate systems step c obtained are dissolved in organic solvent II and standing, until lignin all separates out；
E, by step d separate out lignin filtrate systems carry out filter the rough lignin of isolated, rough lignin is dissolved in the organic solvent III of 80-120 times of volume, adding concentration is the chlorohydric acid pickling of 36-38%, time is 1-2h, then it is filtrated to get filtrate, and is vacuum dried and concentrates at being placed on 120-150 DEG C；
F, the lignin that step e concentrates is dissolved in the mixed liquor of ether-petroleum ether and stir until precipitating whole generation, thereafter precipitation and centrifugal separation is filtered, centrifugal rotational speed is 6000-8000r/min, and carry out washing at least one times with the mixed liquor of ether-petroleum ether, at being finally placed in 60-80 DEG C, vacuum drying obtains refined lignin.
The most according to claim 1 a kind of prepare for carbon fiber the extraction of lignin, process for purification, it is characterised in that: organic solvent I described in step a is polyhydric alcohol, and described acidic catalyst is any one in hydrochloric acid, sulphuric acid or phosphoric acid.
The most according to claim 1 a kind of prepare for carbon fiber the extraction of lignin, process for purification, it is characterised in that: stock solution described in step b is cooled to 20-55 DEG C before regeneration.
The most according to claim 1 a kind of prepare for carbon fiber the extraction of lignin, process for purification, it is characterised in that: organic solvent II described in step d is any one or its mixture in hexamethylene or dichloromethane.
The most according to claim 1 a kind of prepare for carbon fiber the extraction of lignin, process for purification, it is characterised in that: organic solvent III described in step d is any one or more than one the combination in benzyl alcohol, sorbitol, cinnamyl alcohol, saligenin.
The most according to claim 1 a kind of prepare for carbon fiber the extraction of lignin, process for purification, it is characterised in that: washing times described in step f is 2-3 time.
The most according to claim 1 a kind of prepare for carbon fiber the extraction of lignin, process for purification, it is characterised in that: the organic solvent I described in step a-f, organic solvent II and organic solvent III are all distilled recycling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610351643.XA CN105968380A (en) | 2016-05-25 | 2016-05-25 | Extraction and refinement method of lignin for carbon fiber preparation |
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| CN201610351643.XA CN105968380A (en) | 2016-05-25 | 2016-05-25 | Extraction and refinement method of lignin for carbon fiber preparation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107474260A (en) * | 2017-08-02 | 2017-12-15 | 江苏道勤新材料科技有限公司 | A kind of extraction of the lignin prepared for carbon fiber, process for purification |
| CN109453747A (en) * | 2018-11-27 | 2019-03-12 | 华南理工大学 | A method of cellulase adsorbent is used for based on lignin preparation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298744A (en) * | 2008-06-04 | 2008-11-05 | 大连工业大学 | Method for stalk liquefaction preprocessing to prepare fuel ethyl hydrate raw material |
| CN103597085A (en) * | 2011-06-10 | 2014-02-19 | 先正达参股股份有限公司 | Methods for converting lignocellulosic material to useful products |
| CN104411712A (en) * | 2012-05-03 | 2015-03-11 | 威尔迪亚有限公司 | Methods for treating lignocellulosic materials |
-
2016
- 2016-05-25 CN CN201610351643.XA patent/CN105968380A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298744A (en) * | 2008-06-04 | 2008-11-05 | 大连工业大学 | Method for stalk liquefaction preprocessing to prepare fuel ethyl hydrate raw material |
| CN103597085A (en) * | 2011-06-10 | 2014-02-19 | 先正达参股股份有限公司 | Methods for converting lignocellulosic material to useful products |
| CN104411712A (en) * | 2012-05-03 | 2015-03-11 | 威尔迪亚有限公司 | Methods for treating lignocellulosic materials |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107474260A (en) * | 2017-08-02 | 2017-12-15 | 江苏道勤新材料科技有限公司 | A kind of extraction of the lignin prepared for carbon fiber, process for purification |
| CN109453747A (en) * | 2018-11-27 | 2019-03-12 | 华南理工大学 | A method of cellulase adsorbent is used for based on lignin preparation |
| CN109453747B (en) * | 2018-11-27 | 2021-09-21 | 华南理工大学 | Method for preparing cellulase adsorbent based on lignin |
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Application publication date: 20160928 |