CN107130433A - A kind of preparation method of high-temperature resistance carbon fiber sizing agent - Google Patents
A kind of preparation method of high-temperature resistance carbon fiber sizing agent Download PDFInfo
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- CN107130433A CN107130433A CN201710265940.7A CN201710265940A CN107130433A CN 107130433 A CN107130433 A CN 107130433A CN 201710265940 A CN201710265940 A CN 201710265940A CN 107130433 A CN107130433 A CN 107130433A
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- carbon fiber
- sizing agent
- hole boiling
- boiling flask
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 32
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 32
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 31
- 238000004513 sizing Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000019260 propionic acid Nutrition 0.000 claims abstract description 14
- 230000018044 dehydration Effects 0.000 claims abstract description 13
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- 238000009413 insulation Methods 0.000 claims abstract description 13
- 239000000944 linseed oil Substances 0.000 claims abstract description 13
- 235000021388 linseed oil Nutrition 0.000 claims abstract description 13
- 150000004672 propanoic acids Chemical class 0.000 claims abstract description 13
- 238000007873 sieving Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 9
- BJZYYSAMLOBSDY-QMMMGPOBSA-N (2s)-2-butoxybutan-1-ol Chemical compound CCCCO[C@@H](CC)CO BJZYYSAMLOBSDY-QMMMGPOBSA-N 0.000 claims abstract description 8
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 6
- -1 butyl glycol ester diols Chemical class 0.000 claims abstract description 6
- 238000010008 shearing Methods 0.000 claims abstract description 6
- 238000009835 boiling Methods 0.000 claims description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 26
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 23
- 238000004108 freeze drying Methods 0.000 claims description 14
- 239000004408 titanium dioxide Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 208000005156 Dehydration Diseases 0.000 claims description 12
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical class O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical class CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 7
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 5
- 230000009267 minimal disease activity Effects 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 235000010215 titanium dioxide Nutrition 0.000 claims description 4
- 239000002131 composite material Substances 0.000 abstract description 16
- 239000000835 fiber Substances 0.000 abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- KIQKWYUGPPFMBV-UHFFFAOYSA-N diisocyanatomethane Chemical compound O=C=NCN=C=O KIQKWYUGPPFMBV-UHFFFAOYSA-N 0.000 abstract description 2
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 10
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 238000013461 design Methods 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 3
- 239000011354 acetal resin Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229920006324 polyoxymethylene Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229960003237 betaine Drugs 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 238000009955 starching Methods 0.000 description 2
- OZWRZVFUZNYXMF-NHDPSOOVSA-N (5z)-10-methoxy-2,2,4-trimethyl-5-[[3-[(2,2,2-trifluoroethylamino)methyl]thiophen-2-yl]methylidene]-1h-chromeno[3,4-f]quinolin-9-ol Chemical group C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1CNCC(F)(F)F OZWRZVFUZNYXMF-NHDPSOOVSA-N 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229930184093 Furanether Natural products 0.000 description 1
- ILACEZQKVDMRMW-UHFFFAOYSA-N Furanether A Natural products C1C2=COC=C2C2C3CC(C)(C)CC3C1(C)O2 ILACEZQKVDMRMW-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- PYBNTRWJKQJDRE-UHFFFAOYSA-L dodecanoate;tin(2+) Chemical class [Sn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O PYBNTRWJKQJDRE-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- AYVZZPVZDDNTBP-UHFFFAOYSA-N ethoxyethane;furan Chemical compound CCOCC.C=1C=COC=1 AYVZZPVZDDNTBP-UHFFFAOYSA-N 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexamethylene diamine Natural products NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000035935 pregnancy Effects 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
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Abstract
The invention belongs to the technical field of carbon fiber manufacture, and in particular to a kind of preparation method of high-temperature resistance carbon fiber sizing agent.The present invention is first by polyadipate 1, 4 butyl glycol ester diols and PTMG Hybrid Heating, methylene diisocyanate is added after dehydration, the stirring reactions such as dibutyl tin laurate, it is subsequently added 2, 2 dihydromethyl propionic acids, linseed oil etc., distilled water is added after standing, pyromellitic acid anhydride is added after shearing is scattered, MDA etc., after insulation reaction, it is dried to going out material and crushes and collect sieving particle, to finally sieve particle and water, the stirring mixing such as acetone can obtain high-temperature resistance carbon fiber sizing agent, the strong adaptability of carbon fiber sizing agent obtained by the present invention to environment, higher interlaminar shear strength is still maintained under the high temperature conditions, it ensure that carbon fibre composite has higher overall performance under the high temperature conditions.
Description
Technical field
The invention belongs to the technical field of carbon fiber manufacture, and in particular to a kind of preparation side of high-temperature resistance carbon fiber sizing agent
Method.
Background technology
In carbon fibre reinforced composite, for using sizing agent as mistake between enhanced carbon fiber and matrix resin
Cross layer, sizing agent can connect carbon fiber well, can connect matrix resin well again, make carbon fibre reinforced composite into
For an entirety, with very strong overall performance.Carbon fibre reinforced composite is due to big, anticorrosive with intensity height, modulus
Property strong, endurance degree is high, proportion is small etc. is better than the speciality of other fibre reinforced composites, and be widely used in production life
Various fields in work.With the development of Aero-Space, wind energy and automobile industry, to high temperature resistant type carbon fibre reinforced composite
Demand it is growing day by day, the application of carbon fibre composite at high temperature turns into another to pursue a goal after light-weight requirements are pursued.
Carbon fiber/epoxy resin（CF/EP）Composite is widely used in spacecraft with its various excellent performance
In material, the heat resisting temperature of the epoxy type sizing agent matched with it is usually no more than 180 DEG C, and the material that aviation field is equipped with
Majority needs to be resistant to more than 250 DEG C of hot environment.At present, the heat-proof water of resin matrix and carbon fiber reinforcement is average reachable
To requiring, composite entirety heat resistance is significantly limited by the thermal level of carbon fiber surface sizing agent.Therefore, to resistance to
The research of high temperature modification composite is pointing directly at as the development to high temperature resistant type sizing agent.
But, the carbon fiber sizing agent environmental suitability nowadays used is not strong, and with the raising of temperature, interlayer shear is strong
Rapid decrease is spent, so as to greatly affected the overall mechanical properties of carbon fibre composite under the high temperature conditions.Therefore, study
Develop a kind of environmental suitability strong, the carbon fiber sizing agent of higher interlaminar shear strength is still maintained under the high temperature conditions to be had
Important realistic meaning.
The content of the invention
The technical problems to be solved by the invention：It is strong for the carbon fiber sizing agent environmental suitability that nowadays uses,
With the raising of temperature, interlaminar shear strength declines, and have impact on the overall mechanical property of carbon fibre composite under the high temperature conditions
There is provided a kind of method of high-temperature resistance carbon fiber sizing agent for the defect of energy.
In order to solve the above technical problems, the present invention uses technical scheme as described below：
A kind of method of high-temperature resistance carbon fiber sizing agent, specific preparation process is：
（1）Count by weight, take 80~90 parts of polyadipates-BDO esterdiol, 32~35 parts of distilled water, 25~35
Part PTMG, 24~26 portions of linseed oil, 21~23 parts of hexamethylene diisocyanates, 17~22 parts of triethylamines,
13~16 parts of BDOs, 7~9 parts of catalyst, 5~7 parts of titanium dioxide and 4~6 parts of 2,2- dihydromethyl propionic acids；
（2）Polyadipate-BDO esterdiol and PTMG are put into thermometer, agitator and returned
In the four-hole boiling flask for flowing device, four-hole boiling flask is heated, temperature is 105~110 DEG C, and four-hole boiling flask is evacuated to very
Reciprocal of duty cycle is 16~20Pa, with 1~2h of 120r/min stirring dehydrations；
（3）After dehydration terminates, 65~70 DEG C are cooled to, hexamethylene diisocyanate is separately added into four-hole boiling flask, is urged
Agent and BDO, 3~5h of stirring reaction；
（4）After reaction to be mixed terminates, then add into four-hole boiling flask 2,2- dihydromethyl propionic acids, linseed oil and titanium dioxide,
75~80 DEG C are warming up to, continues 2~4h of stirring reaction, 45~50 DEG C are then cooled to, 3~5min is stood, by four-hole boiling flask
Mixture be put into high-shear emulsion machine, add triethylamine and distilled water, the scattered 8~12min of shearing obtains dispersion liquid；
（5）Count by weight, take 60~70 parts of dispersion liquids, 40~45 parts of pyromellitic acid anhydrides, 33~36 parts of trimethyls six
Methylene diamines, 10~15 parts of MDAs and 6~9 parts of trimethylmethoxysilanes are put into reactor, are protected using nitrogen, setting
Temperature is 105~115 DEG C, 10~12h of stirring insulation reaction；
（6）After insulation terminates, room temperature is naturally cooled to, is discharged, and is freeze-dried to going out material, must be freeze-dried
Thing, and use the absolute ethyl alcohol of 3~4 times of lyophilized substance amount to rinse freeze-drying thing, the freeze-drying thing after flushing is put
Enter and 6~8h is dried in 85 DEG C of drying boxes, collect dried object；
（7）Dried object is crushed, 200 mesh sieves are crossed, sieving particle is collected, counts by weight, 30~40 parts of sievings are taken
Grain, 50~60 parts of water, 32~36 parts of acetone and 12~14 parts of octodecyl betaines, be put into mixer stirring 30~
40min, collects stirring mixture, you can obtain high-temperature resistance carbon fiber sizing agent.
The step（1）Middle catalyst is dibutyl tin laurate, N, any in N dimethyl monoethanolamine or triphenylphosphine
It is a kind of.
The present invention is compared with other method, and advantageous effects are：
（1）The present invention is made with polyadipate-BDO esterdiol, PTMG and methylene diisocyanate
For base-material, using dibutyl tin laurate as catalyst, BDO is used as chain extender, 2,2- dihydromethyl propionic acid conducts
Hydrophilizing agent, synthesis of polyurethane is modified by linseed oil and titanium dioxide, improves the temperature tolerance of resin, by high speed shear,
Increase pliability, then by with the hybrid reaction such as pyromellitic acid anhydride and trimethyl hexamethylene diamine, obtain thermoplasticity polyamides
Imines and modified polyurethane hybrid resin, further improve temperature tolerance, and increasing hybrid resin by trimethylmethoxysilane exists
Adhesion property on carbon fiber, finally reduces the contact angle of hybrid resin, increase infiltration using octodecyl betaine
Property, is mixed with water, acetone etc., so as to obtain high-temperature resistance carbon fiber sizing agent；
（2）High-temperature resistance carbon fiber sizing agent prepared by the present invention to the strong adaptability of environment, still maintain under the high temperature conditions compared with
High interlaminar shear strength, it is ensured that carbon fibre composite has higher overall performance under the high temperature conditions；
（3）High-temperature resistance carbon fiber sizing agent preparation technology prepared by the present invention is simple, and required cost is low, applied widely, is worth
Promote the use of.
Embodiment
Count by weight, take 80~90 parts of polyadipates-BDO esterdiol, 32~35 parts of distilled water, 25~
35 parts of PTMGs, 24~26 parts of linseed oil, 21~23 parts of hexamethylene diisocyanates, 17~22 part of three second
Amine, 13~16 parts of BDOs, 7~9 parts of catalyst, 5~7 parts of titanium dioxide and 4~6 parts of 2,2- dihydromethyl propionic acids；Will
Polyadipate-BDO esterdiol and PTMG are put into thermometer, agitator and reflux
In four-hole boiling flask, and four-hole boiling flask is placed in oil bath pan, design temperature is 105~110 DEG C, and four-hole boiling flask is evacuated to very
Reciprocal of duty cycle is 16~20Pa, with 1~2h of 120r/min stirring dehydrations；After dehydration terminates, 65~70 DEG C are cooled to, to four-hole boiling flask
Middle hexamethylene diisocyanate, catalyst and BDO, with 3~5h of 200r/min stirring reactions；Reaction knot to be mixed
Shu Hou, 2,2- dihydromethyl propionic acids, linseed oil and titanium dioxide are added into four-hole boiling flask, are warming up to 75~80 DEG C, continue to stir
2~4h of reaction is mixed, 45~50 DEG C are then cooled to, 3~5min is stood；After standing terminates, by the mixture in four-hole boiling flask
It is put into high-shear emulsion machine, then is separately added into triethylamine and distilled water, with the scattered 8~12min of 8000r/min shearings, score
Dispersion liquid；Count by weight, take 60~70 parts of dispersion liquids, 40~45 parts of pyromellitic acid anhydrides, 33~36 parts of trimethyl pregnancy
Support diamines, 10~15 parts of MDAs and 6~9 parts of trimethylmethoxysilanes are put into reactor, are protected using nitrogen, setting temperature
Spend for 105~115 DEG C, with 10~12h of 150r/min stirring insulation reactions；After insulation terminates, room temperature is naturally cooled to, is carried out
Discharging, and be freeze-dried to going out material, freeze-drying thing is collected, and use the anhydrous second of 3~4 times of lyophilized substance amount
Alcohol rinses freeze-drying thing, and the freeze-drying thing after flushing is put into 85 DEG C of drying boxes and dries 6~8h, collects dried object；Will
Dried object is put into pulverizer and crushed, and crosses 200 mesh sieves, collects sieving particle, counts by weight, take 30~40 parts of sievings
Particle, 50~60 parts of water, 32~36 parts of acetone and 12~14 parts of octodecyl betaines, are put into mixer, with
300r/min stirs 30~40min, collects stirring mixture, you can obtain high-temperature resistance carbon fiber sizing agent.The catalyst is two
Any one in dibutyl tin laurate, N, N dimethyl monoethanolamine or triphenylphosphine.
Example 1
Count by weight, take 80 parts of polyadipates-BDO esterdiol, 32 parts of distilled water, 25 parts of PTMGs
Glycol, 24 parts of linseed oil, 21 parts of hexamethylene diisocyanates, 17 parts of triethylamines, 13 parts of BDOs, 7 parts of tin dilaurates
Dibutyl tin, 5 parts of titanium dioxide and 4 parts of 2,2- dihydromethyl propionic acids；By polyadipate-BDO esterdiol and poly- tetrahydrochysene
Furans ether glycol is put into the four-hole boiling flask with thermometer, agitator and reflux, and four-hole boiling flask is placed in into oil bath pan
In, design temperature is 105 DEG C, and vacuum is evacuated to four-hole boiling flask for 16Pa, with 120r/min stirring dehydrations 1h；In dehydration
After end, 65 DEG C are cooled to, hexamethylene diisocyanate, dibutyl tin laurate and Isosorbide-5-Nitrae-fourth two into four-hole boiling flask
Alcohol, with 200r/min stirring reactions 3h；After reaction to be mixed terminates, 2,2- dihydromethyl propionic acids, Asia are added into four-hole boiling flask
Sesame oil and titanium dioxide, are warming up to 75 DEG C, continue stirring reaction 2h, are then cooled to 45 DEG C, stand 3min；Terminate in standing
Afterwards, the mixture in four-hole boiling flask is put into high-shear emulsion machine, then is separately added into triethylamine and distilled water, with 8000r/
The scattered 8min of min shearings, obtains dispersion liquid；Count by weight, take 60 parts of dispersion liquids, 40 parts of pyromellitic acid anhydrides, 33 part three
Methyl hexamethylene diamine, 10 parts of MDAs and 6 parts of trimethylmethoxysilanes are put into reactor, are protected using nitrogen, setting
Temperature is 105 DEG C, with 150r/min stirring insulation reactions 10h；After insulation terminates, room temperature is naturally cooled to, is discharged, and
It is freeze-dried to going out material, collects freeze-drying thing, and use the absolute ethyl alcohol of 3 times of lyophilized substance amount to rinse freezing
Dried object, the freeze-drying thing after flushing is put into 85 DEG C of drying boxes and dries 6h, collects dried object；Dried object is put into crushing
Crushed in machine, cross 200 mesh sieves, collected sieving particle, count by weight, take 30 parts of sieving particles, 50 parts of water, 32 part third
Ketone and 12 parts of octodecyl betaines, are put into mixer, and 30min is stirred with 300r/min, collect stirring mixture,
High-temperature resistance carbon fiber sizing agent can be obtained.
Example 2
Count by weight, take 90 parts of polyadipates-BDO esterdiol, 35 parts of distilled water, 35 parts of PTMGs
Glycol, 26 portions of linseed oil, 23 parts of hexamethylene diisocyanates, 22 parts of triethylamines, 16 parts of BDOs, 9 parts of triphenylphosphines,
7 parts of titanium dioxide and 6 parts of 2,2- dihydromethyl propionic acids；By polyadipate-BDO esterdiol and PTMG two
Alcohol is put into the four-hole boiling flask with thermometer, agitator and reflux, and four-hole boiling flask is placed in oil bath pan, setting temperature
Spend for 110 DEG C, vacuum is evacuated to four-hole boiling flask for 20Pa, with 120r/min stirring dehydrations 2h；After dehydration terminates, drop
Temperature is to 70 DEG C, hexamethylene diisocyanate, triphenylphosphine and BDO into four-hole boiling flask, anti-with 200r/min stirrings
Answer 5h；After reaction to be mixed terminates, 2,2- dihydromethyl propionic acids, linseed oil and titanium dioxide are added into four-hole boiling flask, is heated up
To 80 DEG C, continue stirring reaction 4h, be then cooled to 50 DEG C, stand 5min；After standing terminates, by the mixing in four-hole boiling flask
Thing is put into high-shear emulsion machine, then is separately added into triethylamine and distilled water, with the scattered 12min of 8000r/min shearings, obtains scattered
Liquid；Count by weight, take 70 parts of dispersion liquids, 45 parts of pyromellitic acid anhydrides, 36 parts of trimethyl hexamethylene diamines, 15 parts the third two
Aldehyde and 9 parts of trimethylmethoxysilanes are put into reactor, are protected using nitrogen, and design temperature is 115 DEG C, is stirred with 150r/min
Mix insulation reaction 12h；After insulation terminates, room temperature is naturally cooled to, is discharged, and is freeze-dried to going out material, is received
Collection freeze-drying thing, and use the absolute ethyl alcohol of 4 times of lyophilized substance amount to rinse freeze-drying thing, the freezing after flushing is done
Dry thing, which is put into 85 DEG C of drying boxes, dries 8h, collects dried object；Dried object is put into pulverizer and crushed, 200 mesh sieves are crossed,
Sieving particle is collected, is counted by weight, 40 parts of sieving particles, 60 parts of water, 36 parts of acetone and 14 parts of octadecyldimethyls are taken
Glycine betaine, is put into mixer, and 40min is stirred with 300r/min, collects stirring mixture, you can obtain high-temperature resistance carbon fiber starching
Agent.
Example 3
Count by weight, take 85 parts of polyadipates-BDO esterdiol, 32 parts of distilled water, 30 parts of PTMGs
Glycol, 25 parts of linseed oil, 22 parts of hexamethylene diisocyanates, 20 parts of triethylamines, 15 parts of BDOs, 8 parts of N, N dimethyl
Monoethanolamine, 6 parts of titanium dioxide and 5 parts of 2,2- dihydromethyl propionic acids；By polyadipate-BDO esterdiol and poly- tetrahydrochysene furan
Ether glycol of muttering is put into the four-hole boiling flask with thermometer, agitator and reflux, and four-hole boiling flask is placed in oil bath pan,
Design temperature is 108 DEG C, and vacuum is evacuated to four-hole boiling flask for 18Pa, with 120r/min stirring dehydrations 1.5h；In dehydration
After end, 68 DEG C are cooled to, hexamethylene diisocyanate, N into four-hole boiling flask, N dimethyl monoethanolamine and BDO,
With 200r/min stirring reactions 4h；After reaction to be mixed terminates, 2,2- dihydromethyl propionic acids, linseed oil are added into four-hole boiling flask
And titanium dioxide, 78 DEG C are warming up to, continues stirring reaction 3h, 48 DEG C are then cooled to, 4min is stood；, will after standing terminates
Mixture in four-hole boiling flask is put into high-shear emulsion machine, then is separately added into triethylamine and distilled water, is sheared with 8000r/min
Scattered 10min, obtains dispersion liquid；Count by weight, take 65 parts of dispersion liquids, 42 parts of pyromellitic acid anhydrides, 35 parts of trimethyls six
Methylene diamines, 12 parts of MDAs and 8 parts of trimethylmethoxysilanes are put into reactor, are protected using nitrogen, design temperature is
110 DEG C, with 150r/min stirring insulation reactions 11h；After insulation terminates, room temperature is naturally cooled to, is discharged, and to discharging
Thing is freeze-dried, and collects freeze-drying thing, and use the absolute ethyl alcohol of 3 times of lyophilized substance amount to rinse freeze-drying
Thing, the freeze-drying thing after flushing is put into 85 DEG C of drying boxes and dries 7h, collects dried object；Dried object is put into pulverizer
Crushed, cross 200 mesh sieves, collect sieving particle, count by weight, take 35 parts sieving particles, 55 parts of water, 34 parts of acetone and
13 parts of octodecyl betaines, are put into mixer, and 35min is stirred with 300r/min, collect stirring mixture, you can
Obtain high-temperature resistance carbon fiber sizing agent.
Be respectively 1.66% by the parts by weight containing slurry of the carbon fiber after the sizing agent starching prepared in example 1~3,1.72%,
1.69%, and gained carbon fiber is subjected to twin-screw reactive extrursion respectively prepares fibre reinforced acetal resin based composites,
The mechanical property for determining prepared fibre reinforced acetal resin based composites is as shown in table 1.
The mechanical property of the fibre reinforced acetal resin based composites of table 1
| Example | Tensile strength/MPa | Impact strength（KJ/m2） | Rockwell hardness/HRR | Bending strength/MPa |
| 1 | 113 | 16..32 | 94 | 185.35 |
| 2 | 115 | 18.72 | 98 | 188.41 |
| 3 | 114 | 17.50 | 96 | 187.08 |
Claims (2)
1. a kind of preparation method of high-temperature resistance carbon fiber sizing agent, it is characterised in that specifically preparation process is：
（1）Count by weight, take 80~90 parts of polyadipates-BDO esterdiol, 32~35 parts of distilled water, 25~35
Part PTMG, 24~26 portions of linseed oil, 21~23 parts of hexamethylene diisocyanates, 17~22 parts of triethylamines,
13~16 parts of BDOs, 7~9 parts of catalyst, 5~7 parts of titanium dioxide and 4~6 parts of 2,2- dihydromethyl propionic acids；
（2）Polyadipate-BDO esterdiol and PTMG are put into thermometer, agitator and returned
In the four-hole boiling flask for flowing device, four-hole boiling flask is heated, temperature is 105~110 DEG C, and four-hole boiling flask is evacuated to very
Reciprocal of duty cycle is 16~20Pa, with 1~2h of 120r/min stirring dehydrations；
（3）After dehydration terminates, 65~70 DEG C are cooled to, hexamethylene diisocyanate is separately added into four-hole boiling flask, is urged
Agent and BDO, 3~5h of stirring reaction；
（4）After reaction to be mixed terminates, then add into four-hole boiling flask 2,2- dihydromethyl propionic acids, linseed oil and titanium dioxide,
75~80 DEG C are warming up to, continues 2~4h of stirring reaction, 45~50 DEG C are then cooled to, 3~5min is stood, by four-hole boiling flask
Mixture be put into high-shear emulsion machine, add triethylamine and distilled water, the scattered 8~12min of shearing obtains dispersion liquid；
（5）Count by weight, take 60~70 parts of dispersion liquids, 40~45 parts of pyromellitic acid anhydrides, 33~36 parts of trimethyls six
Methylene diamines, 10~15 parts of MDAs and 6~9 parts of trimethylmethoxysilanes are put into reactor, are protected using nitrogen, setting
Temperature is 105~115 DEG C, 10~12h of stirring insulation reaction；
（6）After insulation terminates, room temperature is naturally cooled to, is discharged, and is freeze-dried to going out material, must be freeze-dried
Thing, and use the absolute ethyl alcohol of 3~4 times of lyophilized substance amount to rinse freeze-drying thing, the freeze-drying thing after flushing is put
Enter and 6~8h is dried in 85 DEG C of drying boxes, collect dried object；
（7）Dried object is crushed, 200 mesh sieves are crossed, sieving particle is collected, counts by weight, 30~40 parts of sievings are taken
Grain, 50~60 parts of water, 32~36 parts of acetone and 12~14 parts of octodecyl betaines, be put into mixer stirring 30~
40min, collects stirring mixture, you can obtain high-temperature resistance carbon fiber sizing agent.
2. a kind of preparation method of high-temperature resistance carbon fiber sizing agent according to claim 1, it is characterised in that：The step
（1）Middle catalyst is any one in dibutyl tin laurate, N, N dimethyl monoethanolamine or triphenylphosphine.
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