CN107365507A - A kind of lignin-base carbon fiber masterbatch and preparation method thereof - Google Patents
A kind of lignin-base carbon fiber masterbatch and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/18—Homopolymers or copolymers of nitriles
- C08L33/20—Homopolymers or copolymers of acrylonitrile
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/005—Lignin
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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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- 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
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- C08L2203/12—Applications used for fibers
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2312/00—Crosslinking
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Abstract
The invention discloses a kind of lignin-base carbon fiber masterbatch and preparation method thereof, the masterbatch is prepared including following parts by weight raw material：60 80 parts of lignin, 5 10 parts of paraffin, 25 parts of crosslinking agent, 0.01 0.05 parts of biology enzyme, 5 15 parts of polyacrylonitrile, 36 parts of oxidant, 25 parts of vinyl silicone oil；The masterbatch is by the way that the cross-linked polymeric of the monomer after lignin degradation or segment and organic material is formed；It is good with processability, the advantages of Stability Analysis of Structures, it can be directly used for preparing lignin-base carbon fiber, and obtained carbon fiber excellent performance.
Description
Technical field
The present invention relates to carbon fibre material field, and in particular to a kind of lignin-base carbon fiber masterbatch and preparation method thereof.
Background technology
Carbon fiber (carbon fiber, abbreviation CF), be a kind of high intensity of phosphorus content more than 95%, high-modulus it is new
Fiber type material.It is to be piled up to form along fiber axial direction by organic fibers such as flake graphites, through carbonization and graphitization
Microcrystalline graphite material obtained from processing.Carbon fiber has many premium properties, and the axial strength and modulus of carbon fiber are high, density
Low, higher than performance, no creep, superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, and specific heat and electric conductivity are between nonmetallic and golden
Between category, thermal coefficient of expansion is small and has anisotropy, and good corrosion resistance, X-ray transparent is good, and electrical and thermal conductivity performance is good, electric
Electromagnetic shielding performance is good etc., is all important materials in defence and military and civilian aspect.It not only has the intrinsic intrinsic property of carbon material,
Have both the soft machinability of textile fabric again, be the extraordinary reinforcing fiber of a new generation.
Industrial production carbon fiber is all that raw material first are made into precursor by certain processing method processing, then precursor is entered
Row carbonization treatment obtains, and therefore, the quality of precursor also directly affects the quality of carbon fiber.And the quality of precursor is by raw material
Quality directly affects.Although the part raw material of carbon fiber can directly be processed into precursor, often there is processing in raw material
The poor, quality of property differs or the defects of shredding process complexity, cause obtained precursor poor quality, and then thus precursor is prepared
The quality of carbon fiber is not also high.In order to obtain the carbon fiber of high-quality, it is necessary to the precursor to high-quality first prepared, and high-quality
Precursor then need the raw material of high-quality；Therefore, people have carried out modification to raw material, raw material are made to be easier to process
It is more preferable, more stable into silk or quality.
Lignin be in a kind of unbodied, molecular structure being widely present in plant containing oxo phenylpropanol or its
The armaticity high polymer of derivant structure unit.Due to containing a large amount of benzene ring structures in lignin, thus can be used for preparing carbon
Fiber, and lignin comes from plant, can be continuously generated by photosynthesis of plant, belongs to renewable resource, wide material sources,
Cost is cheap, and then reduces the production cost of carbon fiber, carbon fiber is applied to more areas, so as to improve people's
Production and living conditions.But lignin belongs to macromolecule organic material, and dissolubility is poor, poor in processability, it is unfavorable for the preparation of precursor, needs
Compound precursor can just be made after being mixed with other high polymer materials, the preparation for carbon fiber；Although it can be made using this method
It is standby to obtain lignin-base carbon fiber, but the accounting of lignin is small, and the poor performance of obtained carbon fiber, it is unfavorable for lignin-base carbon
The large-scale promotion application of fiber.
The content of the invention
It is an object of the invention to overcome to be currently used for the lignin material poor in processability for preparing carbon fiber, quality shakiness
A kind of inferior defect of carbon fiber that is fixed, obtaining, there is provided lignin-base carbon fiber masterbatch and preparation method thereof；The present invention is by wood
Cross-linked polymeric is carried out with Organic Ingredients after quality pretreatment, forms lignin composite material, i.e. lignin-base carbon fiber masterbatch, should
Masterbatch has the advantages of processability is good, Stability Analysis of Structures, can be directly used for preparing lignin-base carbon fiber, and obtained carbon fiber
Can be excellent.
In order to realize foregoing invention purpose, the invention provides a kind of lignin-base carbon fiber masterbatch, including following weight
Part raw material are prepared：Lignin 60-80 parts, paraffin 5-10 parts, crosslinking agent 2-5 parts, biology enzyme 0.01-0.05 parts, poly- third
Alkene nitrile 5-15 parts, oxidant 3-6 parts, vinyl silicone oil 2-5 parts.
Lignin-base carbon fiber masterbatch of the present invention, by by the monomer after lignin degradation or segment and organic material
Cross-linked polymeric, form the lignin composite material of macromolecular；The material has the advantages of processability is good, Stability Analysis of Structures, can be direct
For preparing lignin-base carbon fiber, and obtained carbon fiber excellent performance.
A kind of above-mentioned lignin-base carbon fiber masterbatch, wherein, described crosslinking agent is polyacid and/or polyalcohol；It is preferred that
, described crosslinking agent is benzenediol, the one or more in ethanedioic acid, ethylene glycol, glycerine.
Wherein, described biology enzyme is the one or more in lignin peroxidase, manganese peroxidase, laccase；
Lignin degradation can be quickly to monomer or lignin such as tonquinol, coniferyl alcohol, 5- hydroxyls coniferyl alcohol, sinapinic alcohols by biology enzyme
Fragment, be advantageous to cross-linked polymeric；Preferably, described biology enzyme is that lignin peroxidase, manganese peroxidase, laccase are pressed
The ratio between amount of material is the mixed enzyme of the ︰ 1 of 2 ︰ 1 compositions；By being reasonably used cooperatively a variety of biology enzymes, can accelerate wooden
The degraded of element, shorten process cycle, and reach optimal degradation effect.
Wherein, the molecular weight of described polyacrylonitrile is 500-2000；In the molecular weight ranges, obtained masterbatch performance
More preferably.
Wherein, described oxidant is hypochlorite；Preferably, described hypochlorite be calcium hypochlorite, sodium hypochlorite,
One or more in postassium hypochlorite；Oxidant can aoxidize the moieties in lignin monomer to form new alkyl or carboxylic
Base, it is easy to the cross-linked polymeric in later stage.
In order to realize foregoing invention purpose, further, present invention also offers a kind of lignin-base carbon fiber masterbatch
Preparation method, comprise the following steps：
（1）Lignin is subjected to degradation treatment with biology enzyme；
（2）Oxidant is added in lignin after degradation and carries out oxidation processes, separated after the completion of oxidation, be dried to obtain oxygen
Change lignin；
（3）After oxidative lignin is well mixed with paraffin, crosslinking agent, polyacrylonitrile, vinyl silicone oil, it is anti-to carry out cross-linked polymeric
Should, obtain lignin-base carbon fiber masterbatch through being granulated after completion.
The preparation method of lignin-base carbon fiber masterbatch of the present invention, first pass through biology enzyme and fast degradation carried out to lignin,
Obtain activity preferably lignin monomer or segment；The moieties in lignin are aoxidized by oxidant again, increase activity
Radical amount and activity；Finally utilize crosslinking agent and organic material, carry out cross-linking polymerization, obtain that processability is more preferable, knot
The more stable lignin-base carbon fiber masterbatch of structure, and the preparation method is simple, quick, reliable, is adapted to lignin-base carbon fiber female
Extensive, the industrialized production of material.
A kind of preparation method of above-mentioned lignin-base carbon fiber masterbatch, wherein, the end bar of degradation treatment described in step 1
Part is average degree of polymerization≤10 of lignin molecule；The lignin molecule degree of polymerization after degraded is excessive, is unfavorable for the oxidation in later stage
Handled with polymerization.
Wherein, the temperature of degradation treatment described in step 1 is 20-35 DEG C；In the temperature range, the activity of biology enzyme is most
It is good, it is best to the degradation effect of lignin.
Wherein, the oxidation treatment time described in step 2 is 30-60min；In the reaction time, lignin oxidation's degree
Preferably, the carbon fiber performance that pretreated lignin is prepared is optimal.
Wherein, cross-linking polymerization is carried out with double screw extruder in step 3；Workspace in described double screw extruder
Maximum temperature be arranged to 330-350 DEG C, minimum temperature is arranged to 280-290 DEG C；Material is in the residence time in an extruder
Control is in 60-120s；Temperature is too high, and side reaction is more, is unfavorable for the cross-linking polymerization of raw material, and temperature is too low, and raw material are not
Melting, cross-linking reaction be not thorough.
Compared with prior art, beneficial effects of the present invention：
1st, lignin-base carbon fiber masterbatch of the present invention be will after lignin degradation with organic material cross-linked polymeric formed it is wooden
Plain composite, there is the advantages of processability is good, Stability Analysis of Structures.
2nd, vinyl silicone oil is with the addition of in lignin-base carbon fiber masterbatch of the present invention, can during carbon fiber is prepared
Carbon silicon bonds are formed, adjacent flake graphite are connected, so as to add the performance of carbon fiber.
3rd, preparation method of the present invention is simple, quick, reliable, is adapted to extensive, the industrialization of lignin-base carbon fiber masterbatch
Production.
Embodiment
With reference to test example and embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
（1）After 70 parts of lignin is dispersed in water, add 0.03 part by lignin peroxidase, manganese peroxidating
The mixed enzyme of thing enzyme, laccase by the ratio between amount of material for the ︰ 1 of 2 ︰ 1 compositions, degradation treatment 2h is carried out at a temperature of 30 DEG C, is formed
Mixed solution；
（2）5 parts of sodium hypochlorite is added in the mixed solution that step 1 obtains and carries out oxidation processes 60min, oxidation is completed laggard
Row separation, it is dried to obtain oxidative lignin；
（3）The oxidative lignin that step 2 is obtained and 8 parts of paraffin, 3 parts of benzenediol, 10 parts of polyacrylonitrile, 5 parts of second
After alkenyl silicone oil is well mixed, cross-linking polymerization is carried out, lignin-base carbon fiber masterbatch is obtained through being granulated after completion.
Embodiment 2
（1）After 80 parts of lignin is dispersed in water, add 0.05 part by lignin peroxidase, manganese peroxidating
Mixed enzyme of the thing enzyme by the ratio between amount of material for 1 ︰ 1 compositions, degradation treatment 3h is carried out at a temperature of 25 DEG C, it is molten to form mixing
Liquid；
（2）6 parts of postassium hypochlorite is added in the mixed solution that step 1 obtains and carries out oxidation processes 30min, oxidation is completed laggard
Row separation, it is dried to obtain oxidative lignin；
（3）The oxidative lignin that step 2 is obtained and 5 parts of paraffin, 2 parts of ethanedioic acid, 3 parts of ethylene glycol, poly- the third of 15 parts
After alkene nitrile, 2 parts of vinyl silicone oil are well mixed, cross-linking polymerization is carried out, lignin-base carbon fibre is obtained through being granulated after completion
Tie up masterbatch.
Embodiment 3
（1）After 60 parts of lignin is dispersed in water, 0.01 part of lignin peroxidase is added, in 30 DEG C of temperature
Degree is lower to carry out degradation treatment 4h, forms mixed solution；
（2）The calcium hypochlorite and 2 parts of sodium hypochlorite that 1 part is added in the mixed solution that step 1 obtains carry out oxidation processes
60min, separated after the completion of oxidation, be dried to obtain oxidative lignin；
（3）Oxidative lignin that step 2 is obtained and 10 parts of paraffin, 2 parts of glycerine, 5 parts of polyacrylonitrile, 5 parts of second
After alkenyl silicone oil is well mixed, cross-linking polymerization is carried out, lignin-base carbon fiber masterbatch is obtained through being granulated after completion.
Comparative example 1
（1）After 70 parts of lignin is dispersed in water, add 0.03 part by lignin peroxidase, manganese peroxidating
The mixed enzyme of thing enzyme, laccase by the ratio between amount of material for the ︰ 1 of 2 ︰ 1 compositions, carries out degradation treatment 2h, degraded at a temperature of 30 DEG C
After the completion of separated, be dried to obtain lignin degrading；
（2）The lignin degrading that step 1 is obtained and 8 parts of paraffin, 3 parts of benzenediol, 10 parts of polyacrylonitrile, 5 parts of second
After alkenyl silicone oil is well mixed, cross-linking polymerization is carried out, lignin-base carbon fiber masterbatch is obtained through being granulated after completion.
Comparative example 2
（1）After 70 parts of lignin is dispersed in water, add 0.03 part by lignin peroxidase, manganese peroxidating
The mixed enzyme of thing enzyme, laccase by the ratio between amount of material for the ︰ 1 of 2 ︰ 1 compositions, degradation treatment 2h is carried out at a temperature of 30 DEG C, is formed
Mixed solution；
（2）5 parts of sodium hypochlorite is added in the mixed solution that step 1 obtains and carries out oxidation processes 60min, oxidation is completed laggard
Row separation, it is dried to obtain oxidative lignin；
（3）The oxidative lignin that step 2 obtains is well mixed with 8 parts of paraffin, 3 parts of benzenediol, 10 parts of polyacrylonitrile
Afterwards, cross-linking polymerization is carried out, lignin-base carbon fiber masterbatch is obtained through being granulated after completion.
Comparative example 3
（1）70 parts of lignin is dispersed in water and forms mixed solution, 5 parts of oxidant is added and carries out oxidation processes
60min, separated after the completion of oxidation, be dried to obtain oxidative lignin；
（2）The oxidative lignin that step 2 is obtained and 8 parts of paraffin, 3 parts of benzenediol, 10 parts of polyacrylonitrile, 5 parts of second
After alkenyl silicone oil is well mixed, cross-linking polymerization is carried out, lignin-base carbon fiber masterbatch is obtained through being granulated after completion.
Comparative example 4
（1）After 70 parts of lignin is dispersed in water, add 0.03 part by lignin peroxidase, manganese peroxidating
The mixed enzyme of thing enzyme, laccase by the ratio between amount of material for the ︰ 1 of 2 ︰ 1 compositions, degradation treatment 2h is carried out at a temperature of 30 DEG C, is formed
Mixed solution；
（2）5 parts of sodium hypochlorite is added in the mixed solution that step 1 obtains and carries out oxidation processes 60min, oxidation is completed laggard
Row separation, it is dried to obtain oxidative lignin；
（3）The oxidative lignin that step 2 is obtained and 8 parts of paraffin, 3 parts of benzenediol, 20 parts of polyacrylonitrile, 5 parts of second
After alkenyl silicone oil is well mixed, cross-linking polymerization is carried out, lignin-base carbon fiber masterbatch is obtained through being granulated after completion.
Preparation-obtained lignin-base carbon fiber masterbatch in above-described embodiment 1-3 and comparative example 1-3 is added respectively
Work detects, and records testing result；Obtained lignin-base carbon fiber masterbatch is melted respectively, spinning, pre-oxidation, carbonization
Processing, is prepared lignin-base carbon fiber, carbon fiber performance is detected and recorded；Record data is as follows：
| Numbering | Processability | Diameter（μm） | Tensile strength（MPa） | Stretch modulus（Gpa） |
| Embodiment 1 | +++++ | 5.0 | 2430 | 173 |
| Embodiment 2 | +++++ | 5.0 | 2380 | 172 |
| Embodiment 3 | +++++ | 5.0 | 2310 | 180 |
| Comparative example 1 | ++ | 5.0 | 1130 | 106 |
| Comparative example 2 | ++++ | 5.0 | 2030 | 162 |
| Comparative example 3 | + | 5.0 | 1880 | 151 |
| Comparative example 4 | ++ | 5.0 | 2280 | 167 |
Note："+" is more, and statement processability is better.
Above-mentioned analysis of experimental data is understood, technical solution of the present invention is used in embodiment 1-3, obtained lignin-base carbon
Fiber master batch processability is good, and the carbon fiber being prepared draws Shen intensity and stretch modulus good；And in comparative example 1, not to drop
The lignin of solution carries out oxidation processes, therefore, is unfavorable for the cross-linked polymeric in later stage, obtained lignin-base carbon fiber masterbatch processing
Property significantly reduce, and the carbon fiber that is prepared draws Shen intensity and stretch modulus to be significantly reduced；It is being crosslinked in comparative example 2
Vinyl silicone oil is not added during polymerization, although influenceing less, be prepared on the processability of lignin-base carbon fiber masterbatch
To carbon fiber in, without the formation of carbon silicon bonds, cause carbon fiber to draw Shen intensity and stretch modulus to significantly reduce；In comparative example 3
Degradation treatment is not carried out to lignin, the oxidation effectiveness of direct oxidation is poor, is also unfavorable for the cross-linked polymeric in later stage, obtained wood
Quality base carbon fibre masterbatch processability significantly reduces, and the carbon fiber being prepared draws Shen intensity and stretch modulus also significantly to drop
It is low；The addition of polyacrylonitrile is excessive in comparative example 4, and the lignin-base carbon fiber masterbatch processability after cross-linked polymeric significantly drops
Low, the influence for drawing Shen intensity and stretch modulus to final carbon fiber is smaller.
Claims (10)
1. a kind of lignin-base carbon fiber masterbatch, it is characterised in that be prepared including following parts by weight raw material：Lignin
60-80 parts, paraffin 5-10 parts, crosslinking agent 2-5 parts, biology enzyme 0.01-0.05 parts, polyacrylonitrile 5-15 parts, oxidant 3-6 parts,
Vinyl silicone oil 2-5 parts.
2. masterbatch according to claim 1, it is characterised in that described crosslinking agent is polyacid and/or polyalcohol.
3. masterbatch according to claim 2, it is characterised in that described crosslinking agent be benzenediol, ethanedioic acid, ethylene glycol,
One or more in glycerine.
4. masterbatch according to claim 1, it is characterised in that described biology enzyme is lignin peroxidase, manganese mistake
One or more in oxide enzyme, laccase.
5. masterbatch according to claim 4, it is characterised in that described biology enzyme is lignin peroxidase, manganese mistake
The mixed enzyme of oxide enzyme, laccase by the ratio between amount of material for the ︰ 1 of 2 ︰ 1 compositions.
6. masterbatch according to claim 1, it is characterised in that the molecular weight of described polyacrylonitrile is 500-2000.
7. masterbatch according to claim 1, it is characterised in that described oxidant is hypochlorite.
8. masterbatch according to claim 7, it is characterised in that described hypochlorite is calcium hypochlorite, sodium hypochlorite, secondary
One or more in potassium chlorate.
9. a kind of preparation method of the masterbatch as described in claim any one of 1-8, it is characterised in that comprise the following steps：
（1）Lignin is subjected to degradation treatment with biology enzyme；
（2）Oxidant is added in lignin after degradation and carries out oxidation processes, separated after the completion of oxidation, be dried to obtain oxygen
Change lignin；
（3）After oxidative lignin is well mixed with paraffin, crosslinking agent, polyacrylonitrile, vinyl silicone oil, it is anti-to carry out cross-linked polymeric
Should, obtain lignin-base carbon fiber masterbatch through being granulated after completion.
10. preparation method according to claim 9, it is characterised in that carry out crosslinking with double screw extruder in step 3 and gather
Close reaction；The maximum temperature of workspace is arranged to 330-350 DEG C in described double screw extruder, and minimum temperature is arranged to 280-
290℃；Material is controlled in 60-120s in the residence time in an extruder.
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| CN201710750470.3A CN107365507A (en) | 2017-08-28 | 2017-08-28 | A kind of lignin-base carbon fiber masterbatch and preparation method thereof |
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| CN201710750470.3A CN107365507A (en) | 2017-08-28 | 2017-08-28 | A kind of lignin-base carbon fiber masterbatch and preparation method thereof |
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| CN107365507A true CN107365507A (en) | 2017-11-21 |
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