CN108330569A - A kind of lignin-base activated carbon fiber presoma and the preparation method and application thereof - Google Patents
A kind of lignin-base activated carbon fiber presoma and the preparation method and application thereof Download PDFInfo
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- CN108330569A CN108330569A CN201810128715.3A CN201810128715A CN108330569A CN 108330569 A CN108330569 A CN 108330569A CN 201810128715 A CN201810128715 A CN 201810128715A CN 108330569 A CN108330569 A CN 108330569A
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- lignin
- phenolate
- enzymolysis
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- activated carbon
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- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
- Compounds Of Unknown Constitution (AREA)
Abstract
The present invention relates to a kind of lignin-base activated carbon fiber presomas and the preparation method and application thereof.This method includes：Appropriate distilled water is added in plant fiber material, in 160 180 DEG C of boiling 40min, is cleaned；Grinding；Cellulase is added and hemicellulase is digested；It cleans；Filter freezing is dried；Powder is made；Phenol, the concentrated sulfuric acid is added, is fully dissolved out, is dispersed in petroleum ether with ethyl acetate after reaction, filtered, it is dry, obtain the enzymolysis xylogen of phenolate modification；The phenolate lignin and lignin-base activated carbon fiber precursor of melt-spinnable can further be made.The present invention by enzymolysis xylogen carry out phenolate modification, to change its melting behaviour, can continuous spinning, meet the needs of industrialized production.The present invention successfully solves that lignin meltbility is poor, the problem of spinning hardly possible.
Description
Technical field
The present invention relates to plant celluloses to utilize technical field, and in particular to a kind of lignin-base activated carbon fiber presoma
And the preparation method and application thereof.
Background technology
Activated carbon fiber is due to abundant and flourishing pore structure, being often used as sorbing material, catalyst carrier, electricity
Pole material is widely used in fields such as environment, food, health, chemical industry, electrochemistry.Currently, manufacture activated carbon fiber
Primary raw material has viscose fiber, polyacrylonitrile fibre, pitch fibers and phenolic fibre.Since viscose fiber cost of material is high, third
Alkene nitrile, pitch and phenol are all oil based materials, lead to the higher price of final activated carbon fiber, constrain it and answer on a large scale
With.
Energy ethanol is that current each state all pays special attention to a kind of gasoline substitute products simultaneously competitively developed.This year, country's hair
15 departments such as exhibition reform committee, National Energy Board, which combine, to print and distribute《Vehicle is produced and promotes the use of about bio-fuel ethyl alcohol is expanded
With the embodiment of ethanol petrol》.According to《Scheme》, the year two thousand twenty is arrived, China will realize vehicle ethanol substantially in China
Gasoline all standing；By 2025, strive realizing cellulosic ethanol large-scale production.Domestic annual available stalk and forestry are useless
Gurry is more than 400,000,000 tons, allows the polysaccharide conversion in stalk or forestry waste at energy using biotechnologys such as microorganism, enzymatics
Source alcohol.Lignocellulosic enzymatic hydrolysis and fermentation produce bio-ethanol during residue in containing 30%~35% or so it is wooden
Element is usually directly burned and serves as fuel, and not only the economic benefit is not high, but also certain pollution is caused to environment.Lignin
It is complicated, be the three-dimensional high-molecular compound being formed by connecting by ehter bond and carbon-carbon bond by phenyl-propane class formation unit,
Since lignin contains more aromatic ring structure, carbon content is higher.It forms plant skeleton together with cellulose, hemicellulose
Main component, be quantitatively only second to cellulose.In needlebush, content of lignin 25-35%, leaf wood content of lignin
Up to 20-25%, tall graminaceous plant generally contains 15-25%.Wooden fibre will be improved by preparing activated carbon fiber with these enzymolysis xylogens
The economic benefit of inverting biological ethanol industry is tieed up, while alleviating the dependence to oil product, is reduced environmental pollution.
However the enzymolysis xylogen meltbility of prior art preparation is poor, it is difficult to directly carry out melt spinning.
Invention content
The present invention is intended to provide a kind of lignin-base activated carbon fiber presoma and the preparation method and application thereof, the present invention is logical
Cross to enzymolysis xylogen carry out phenolate modification, to change its melting behaviour, can continuous spinning, meet the need of industrialized production
It wants.
Technical solution of the present invention is as follows：
A kind of preparation method of lignin-base activated carbon fiber presoma, includes the following steps：
1) appropriate distilled water is added in plant fiber material, in 160-180 DEG C of boiling 40min；Deionized water is used after taking-up
It cleans up and (generally at least cleans three times) repeatedly；
Further, plant fiber material includes all kinds of straws, chips, bamboo wood etc..
Further, the amount that distilled water is added is 5-15 times, preferably 10 times of plant fiber material weight.
2) step 1) resulting material is ground；Cellulase is added and hemicellulase is digested；It is used after enzymolysis
Deionized water cleans enzymolysis residue repeatedly until pH value is neutral, and then filter freezing is dried；Grind or be ground into powder (preferably 60
Mesh)；
Usually, digested raw material can be first ground with fiberizer, break coupling for lignin and cellulose；Further use
The further grinding material of beater；Reduce material size by grinding, increases enzymolysis contact area, improve enzymolysis efficiency.Then
Centrifugation is put into 4 DEG C of refrigerators and preserves.
Further, enzymolysis carries out under the conditions of rotating speed 180r/min.
Further, hydrolysis temperature is 55 DEG C；Enzymolysis time is 72h.
Under above-mentioned optimum condition, preferably hydrolysis result can be obtained.
3) step 2) resulting material is heated with phenol at 90-130 DEG C and is uniformly mixed, the concentrated sulfuric acid is then added, it is fully anti-
It answers；
Further, the dosage of phenol is 3-5 times of step 2) resulting material weight.
Further, the dosage of the concentrated sulfuric acid is the 5-10% of step 2) resulting material weight.
Usually, reaction time 2-4h.
4) mixture after being reacted step 3) with suitable ethyl acetate dissolves out, and is dispersed in the petroleum ether of certain volume
The phenol for having neither part nor lot in reaction is washed away, stirring is filtered after a certain period of time, dry, obtains the enzymolysis xylogen of phenolate modification.
Further, the above method is further comprising the steps of：
5) the organic solvents extraction steps 4 such as acetone or ethyl acetate are used) enzymolysis xylogen that gained phenolate is modified, it has been evaporated
Solvent, obtaining can be with the phenolate lignin of melt spinning.
Further, the above method is further comprising the steps of：
6) step 5) gained can be carried out with the phenolate lignin of melt spinning with certain rotating speed within the scope of 160-175 DEG C
Melt spinning obtains lignin-base activated carbon fiber precursor.
The raw materials used in the present invention is commercially available to buy, or is prepared by this field conventional method.
On the basis of common knowledge of the art, above-mentioned each optimum condition can be combined with each other each preferably to get the present invention
Example.
The invention also includes lignin-base activated carbon fiber presoma (i.e. lignin-base activity carbon fibers prepared by the above method
Tie up precursor)；Further include the above method prepare the enzymolysis xylogen being modified by phenolate, can be wooden with the phenolate of melt spinning
Element.
The invention also includes above-mentioned lignin-base activated carbon fiber presomas to adsorb, newly in water resource purification, toxic gas
The application in the fields such as energy electric vehicle, food, chemical industry.
The present invention successfully solves that lignin meltbility is poor, the problem of spinning hardly possible.
It is feasible that the present invention has been subjected to experimental verification.In 160-180 DEG C of temperature range, phenolate is changed by melt spinning machine
Property lignin soluble fraction carry out spinning trial, can long period continuous spinning, and spun fibre diameter is very thin, about exists
10μm。
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..It is not specified in embodiment specific
Technology or condition person carry out according to technology or condition described in document in the art, or according to product description.It is used
Production firm person is not specified in reagent or instrument, is the conventional products that can be commercially available by regular distributor.
Embodiment 1
1. measuring the moisture content of straw or chips, a certain amount of gas dry raw material is put into boiling vessel, is added simultaneously
Enter the distilled water of 10 times of raw material oven dry weights, 160-180 DEG C of boiling 40 minutes.Boiling it is complete after outwells cooking liquor, spend from
Sub- water cleans the raw material after boiling three times repeatedly；
2. grind digested raw material using fiberizer, break coupling for lignin and cellulose.It is used in combination beater into one
Grinding material is walked, material size is reduced by grinding, increases enzymolysis contact area, improves enzymolysis efficiency.It is then centrifuged for, is put into 4
DEG C refrigerator preserves；
3. measuring the moisture content of slurry.Slurry is digested under the conditions of 55 DEG C with certain density cellulase and hemicellulase
Material, shaking speed 180r/min, enzymolysis time 72 hours.Enzymolysis residue is cleaned repeatedly in deionized water after enzymolysis
Property, then filter freezing is dried；
4. the enzymolysis xylogen after freeze-drying, which is ground into, can cross the powder of 60 mesh sieve, then gained enzymolysis xylogen is carried out
Constituent analysis detects the content of Degree of Enzymatic Hydrolysis and lignin；
5. taking dry enzymolysis xylogen 10g to heat at 90-130 DEG C with 30-50g phenol to be uniformly mixed, base is then added
In the concentrated sulfuric acid of lignin weight 5-10%, 2-4h is reacted；
6. being dissolved out the mixture after reaction with a certain amount of ethyl acetate, it is dispersed in the petroleum ether of certain volume and washes away
The phenol of reaction is had neither part nor lot in, stirring is filtered after a certain period of time, dry to get the enzymolysis xylogen being modified to phenolate；
7. the enzymolysis xylogen being modified with the extracting phenolate of the organic solvents such as acetone or ethyl acetate, then uses Rotary Evaporators
Solvent evaporated, just obtaining can be with the phenolate lignin of melt spinning；
8. carrying out melting spinning to solvable phenolate modified enzymolysis lignin in 160-175 DEG C of temperature range with certain rotating speed
Silk, you can obtain lignin-base activated carbon fiber precursor.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of preparation method of lignin-base activated carbon fiber presoma, which is characterized in that include the following steps：
1) appropriate distilled water is added in plant fiber material, in 160-180 DEG C of boiling 40min；After taking-up repeatedly with deionized water
It cleans up；
2) step 1) resulting material is ground；Cellulase is added and hemicellulase is digested；Spent after enzymolysis from
Sub- water cleans enzymolysis residue repeatedly until pH value is neutral, and then filter freezing is dried；Grind or be ground into powder；
3) step 2) resulting material is heated with phenol at 90-130 DEG C and is uniformly mixed, the concentrated sulfuric acid is then added, fully reacted；
4) mixture after being reacted step 3) with suitable ethyl acetate dissolves out, and is dispersed in the petroleum ether of certain volume and washes away
The phenol of reaction is had neither part nor lot in, stirring is filtered after a certain period of time, dry, obtains the enzymolysis xylogen of phenolate modification；
Alternatively, further, the above method is further comprising the steps of：
5) use organic solvent extraction steps 4) gained phenolate be modified enzymolysis xylogen, be evaporated organic solvent, obtain to melt
The phenolate lignin of spinning；
Alternatively, further, the above method is further comprising the steps of：
6) step 5) gained can be melted with the phenolate lignin of melt spinning with certain rotating speed within the scope of 160-175 DEG C
Spinning obtains lignin-base activated carbon fiber precursor.
2. according to the method described in claim 1, it is characterized in that, the dosage of phenol is step 2) resulting material weight in step 3)
3-5 times of amount；And/or
The dosage of the concentrated sulfuric acid is the 5-10% of step 2) resulting material weight in step 3).
3. according to the method described in claim 2, it is characterized in that, the step 3) reaction time is 2-4h.
4. according to claim 1-3 any one of them methods, which is characterized in that step 2) is digested in rotating speed 180r/min conditions
Lower progress.
5. according to claim 1-4 any one of them methods, which is characterized in that the step 2) hydrolysis temperature is 55 DEG C；Enzyme
The solution time is 72h.
6. according to claim 1-5 any one of them methods, which is characterized in that the amount that distilled water is added is plant fiber material
5-15 times of weight, preferably 10 times.
7. according to claim 1-6 any one of them methods, which is characterized in that the plant fiber material includes plant straw
Stalk, chips, bamboo wood.
8. according to the preparation method of any one of claim 1-7, which is characterized in that include the following steps：
1) plant fiber material is added to the distilled water of 5-15 times of weight, in 180 DEG C of boiling 40min；Deionized water is used after taking-up
It cleans up repeatedly；
2) step 1) resulting material is ground；Cellulase is added and hemicellulase is digested；Spent after enzymolysis from
Sub- water cleans enzymolysis residue repeatedly until pH value is neutral, and then filter freezing is dried；Grind or be ground into powder；
Enzymolysis carries out under the conditions of rotating speed 180r/min, and hydrolysis temperature is 55 DEG C；Enzymolysis time is 72h；
3) step 2) resulting material is heated with phenol at 90-130 DEG C and is uniformly mixed, the concentrated sulfuric acid is then added, fully reacts 2-
4h；
The dosage of phenol is 3-5 times of step 2) resulting material weight, and the dosage of the concentrated sulfuric acid is step 2) resulting material weight
5-10%；
4) mixture after being reacted step 3) with suitable ethyl acetate dissolves out, and is dispersed in the petroleum ether of certain volume and washes away
The phenol of reaction is had neither part nor lot in, stirring is filtered after a certain period of time, dry, obtains the enzymolysis xylogen of phenolate modification；
Alternatively, further, the above method is further comprising the steps of：
5) use organic solvent extraction steps 4) gained phenolate be modified enzymolysis xylogen, be evaporated organic solvent, obtain to melt
The phenolate lignin of spinning；
Alternatively, further, the above method is further comprising the steps of：
6) step 5) gained can be melted with the phenolate lignin of melt spinning with certain rotating speed within the scope of 160-175 DEG C
Spinning obtains lignin-base activated carbon fiber precursor.
9. lignin-base activated carbon fiber presoma prepared by any one of claim 1-8 the methods.
10. lignin-base activated carbon fiber presoma described in claim 9 is in water resource purification, toxic gas absorption, new energy
The application of electric vehicle, food, chemical field.
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Cited By (4)
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| 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 |
| CN109518308A (en) * | 2018-11-29 | 2019-03-26 | 青岛大学 | A kind of chain extension of lignin is modified and its preparation method of melt spun fibre |
| CN109680363A (en) * | 2018-11-30 | 2019-04-26 | 北京林业大学 | A kind of solidification processing method and products therefrom of lignin-base fiber |
| CN111472069A (en) * | 2020-05-28 | 2020-07-31 | 中国科学院化学研究所 | Porous activated carbon fiber and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| CN109518308A (en) * | 2018-11-29 | 2019-03-26 | 青岛大学 | A kind of chain extension of lignin is modified and its preparation method of melt spun fibre |
| CN109518308B (en) * | 2018-11-29 | 2021-02-19 | 青岛大学 | Chain extension modification of lignin and preparation method of melt-spun fiber thereof |
| CN109680363A (en) * | 2018-11-30 | 2019-04-26 | 北京林业大学 | A kind of solidification processing method and products therefrom of lignin-base fiber |
| CN109680363B (en) * | 2018-11-30 | 2021-06-01 | 北京林业大学 | Curing treatment method of lignin-based fiber and obtained product |
| CN111472069A (en) * | 2020-05-28 | 2020-07-31 | 中国科学院化学研究所 | Porous activated carbon fiber and preparation method thereof |
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