CN110130108A - A kind of continuous carbofrax fibre epoxy resin sizing agent and preparation method and application - Google Patents
A kind of continuous carbofrax fibre epoxy resin sizing agent and preparation method and application Download PDFInfo
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- CN110130108A CN110130108A CN201910283605.9A CN201910283605A CN110130108A CN 110130108 A CN110130108 A CN 110130108A CN 201910283605 A CN201910283605 A CN 201910283605A CN 110130108 A CN110130108 A CN 110130108A
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- epoxy resin
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- fibre
- sizing agent
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 129
- 239000000835 fiber Substances 0.000 title claims abstract description 128
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 87
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 87
- 238000004513 sizing Methods 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000002270 dispersing agent Substances 0.000 claims abstract description 22
- 239000000080 wetting agent Substances 0.000 claims abstract description 21
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003755 preservative agent Substances 0.000 claims abstract description 13
- 230000002335 preservative effect Effects 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000004814 polyurethane Substances 0.000 claims description 41
- 229920002635 polyurethane Polymers 0.000 claims description 41
- 238000001035 drying Methods 0.000 claims description 35
- 229920000570 polyether Polymers 0.000 claims description 34
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 32
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 28
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 28
- 238000010792 warming Methods 0.000 claims description 28
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 26
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 229930185605 Bisphenol Natural products 0.000 claims description 14
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 14
- 238000009835 boiling Methods 0.000 claims description 14
- 239000006210 lotion Substances 0.000 claims description 14
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000004804 winding Methods 0.000 claims description 13
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 9
- -1 sorbitan fatty ester Chemical class 0.000 claims description 8
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims description 7
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 7
- 239000004970 Chain extender Substances 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 7
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 7
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 7
- 239000004359 castor oil Substances 0.000 claims description 7
- 235000019438 castor oil Nutrition 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000003999 initiator Substances 0.000 claims description 7
- 239000003002 pH adjusting agent Substances 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 claims description 7
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 claims description 7
- 150000004672 propanoic acids Chemical class 0.000 claims description 7
- 235000019260 propionic acid Nutrition 0.000 claims description 7
- 238000000197 pyrolysis Methods 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 6
- 239000006071 cream Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 claims 1
- 239000010426 asphalt Substances 0.000 claims 1
- UDEWPOVQBGFNGE-UHFFFAOYSA-N benzoic acid n-propyl ester Natural products CCCOC(=O)C1=CC=CC=C1 UDEWPOVQBGFNGE-UHFFFAOYSA-N 0.000 claims 1
- 239000003906 humectant Substances 0.000 claims 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 6
- 239000000428 dust Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000012298 atmosphere Substances 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract description 2
- 229920003257 polycarbosilane Polymers 0.000 abstract description 2
- 150000002334 glycols Chemical class 0.000 description 12
- 239000005058 Isophorone diisocyanate Substances 0.000 description 11
- 238000009955 starching Methods 0.000 description 7
- 150000002148 esters Chemical class 0.000 description 6
- 239000002585 base Substances 0.000 description 5
- 238000003837 high-temperature calcination Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 150000004040 pyrrolidinones Chemical class 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910003978 SiClx Inorganic materials 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009954 braiding Methods 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 238000009940 knitting Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 208000013403 hyperactivity Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
- D06M15/09—Cellulose ethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M15/53—Polyethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M15/55—Epoxy resins
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of continuous carbofrax fibre epoxy resin sizing agents, the continuous carbofrax fibre is prepared from the following raw materials in parts by weight with epoxy resin sizing agent: 65-71.5 parts of deionized water, 20-33.5 parts of epoxy resin, dispersing agent and 0.4-0.8 parts of levelling agent, 0.85-1.75 parts of wetting agent, 1.0-2.0 parts of emulsifier, preservative 0.1-0.3, film forming agent 0.5-0.75 parts of self-control, continuous carbofrax fibre epoxy resin sizing agent provided by the invention, ceramic fibre applied to polycarbosilane precusor conversion, such as the second generation, third generation continuous carbofrax fibre, the ceramic fibres such as broadband absorbing continuous carbofrax fibre, it can reinforce loose fiber filament bonding bunchy；Being conducive to fiber softening reduces the frictional force of fibre bundle and fibre bundle is made to be easier to weave；Be conducive to the cover of fiber surface defect hole and remedy, improves the intensity of fiber；The antistatic property for being conducive to improve fiber surface reduces hydrone and dust granules in absorption atmosphere.
Description
Technical field
The present invention relates to a kind of its composition of sizing agent and preparation method and application more particularly to a kind of continuous carbofrax fibres
With epoxy resin sizing agent and preparation method and application.
Background technique
PCS polymer-derived method produces continuous ceramic fiber, as the second generation, third generation silicon carbide fibre, wave transparent type silicon carbide are fine
It of dimension, broadband absorbing silicon carbide fibre (hereinafter referred to as " various fibers ") etc. has high-strength and high-modulus, fire-resistant oxidation resistant, low
The characteristics such as creep, low-density, anti-ablation, Flouride-resistani acid phesphatase are the key that long-life hot end structure and stealthy high-performance composite materials
Constituent element is the critical material of country's " two machines are special ", belongs to the strategic material of national defence section work, is that high temperature hot end material technology system is high
Point has important and is widely applied in the strategic field such as Aeronautics and Astronautics, nuclear power, such material is the military affairs embargoed in the world
Sensitive goods and materials, it is all the time external that technology blockage and product embargo are carried out to China.
When prior art technology produces above-mentioned various fibers, fiber is easy to produce lousiness and is even broken, and makes its strength reduction；
Next, due to receiving anti-corruption the effects of stretching, friction, being bent, distort, causes fluffing, pine during future usage braiding
It dissipates, split silk, cause fiber to be difficult to weave, and strength reduction；In addition, the microstructure of fiber there is also many defects, such as
Granular absorption, scratch are uneven, will increase fiber roll around, packed and transported, using the friction of braiding process, cause bigger damage
Evil；Meanwhile the fluffiness of fiber, it is invisible, but can cause damages to space environment and human body；Fiber is carried out
Slurry surface treatment, makes silicon carbide fibre surface physics coat one layer of thin and smooth organic film, is similar to adhesive, enables fiber
Form a film boundling, improves knitting property.Also sizing agent can be allowed to wrap up, fiberfill fibers surface defect, suitably mitigation fiber surface activity,
In order to avoid hyperactivity, adsorbs moisture in air and dust, generates and reduce between fiber in this way, sizing agent just can be reduced lousiness
Frictional force.In addition, sizing agent is also similar to wetting agent, wetting fibre surface, allow fiber surface preferably with ceramic matrix
Precursor combines.
The problems such as technique that domestic and international polymer-derived method produces above-mentioned various fibers is similar, encounters fibre pick, defect
Also similar, but external sizing agent, the preparation of sizing agent is considered as one of key technology, is holded in close confidence, and domestic PC S is converted
Ceramic fibre belongs to emerging field, and to the research of the sizing agent of this kind of ceramic fibre unlike carbon fiber is so mature, domestic literature is fresh
It appears in the newspapers and leads.The especially less rarely seen report of the sizing agent of epoxy resin.
Summary of the invention
Go out in process of production in view of the above-mentioned problems, can solve the existing above-mentioned various fibers of processing the present invention provides one kind
The sizing agent for the problems such as existing easy fluffing, broken end, defect or dust adsorbs, improves fiber continuity, improves its flexibility and volume
Knitting property.
The present invention is achieved by the following technical solutions:
A kind of continuous carbofrax fibre epoxy resin sizing agent, the continuous carbofrax fibre epoxy resin sizing agent by
The raw material of following parts by weight is made: 65-71.5 parts of deionized water, 20-33.5 parts of epoxy resin, and dispersing agent and levelling agent 0.4-
0.8 part, 0.85-1.75 parts of wetting agent, 1.0-2.0 parts of emulsifier, preservative 0.1-0.3, make film forming agent 0.5-0.75 parts by oneself.
Preferably, the epoxy resin is by bisphenol A-type tetraglycidel ether epoxy resin (E20) and bisphenol A-type glycidol
Ether epoxy resin (E51) is mixed according to the ratio that weight ratio is 1:1.
Preferably, the dispersing agent and levelling agent are carboxymethyl cellulose.
Preferably, the wetting agent is pressed by polyoxyethylene sorbitan monostearate and sorbitan fatty ester
It is mixed according to the ratio that weight ratio is 1:1.
Preferably, the emulsifier by castor oil polyoxyethylene ether (EL-80) and octyl phenol polyoxyethylene ether (TX-10) with
And polyether block polymerization amino-modified silicone oil (TF-463) is that 2:2:1 ratio is mixed according to weight ratio.
Preferably, the self-control film forming agent is Acrylate Modified Aqueous Polyurethane, wherein Acrylate Modified Aqueous Polyurethane
The preparation method is as follows: by polyether Glycols (GE220) vacuum (1.066kPa), temperature be 120 DEG C in the case where be dehydrated for 24 hours
It is spare, load weighted polyether Glycols (GE220) are placed in four-hole boiling flask, after being slowly warming up to 80 DEG C, while different Buddhist are added
That ketone diisocyanate (IPDI) and catalyst, are warming up to 100 DEG C of reaction 2h, then cool to 60 DEG C of addition dihydromethyl propionic acids
(DMPA) and N-Methyl pyrrolidone (NMP), 85 DEG C of reaction 6h are slowly warming up to, are continuously added acetone in reaction process to reduce
Performed polymer is transferred in high velocity dispersators by the viscosity of reactant when nco value reaches theoretical value in system, in high-speed stirring
Mix the polyether type aqueous poly- ammonia of self-emulsifying being scattered in dissolved in the distilled water of chain extender and neutralizer, obtained solid content is 20%
Then self-emulsifying polyether type aqueous polyurethane is removed solvent under 60 DEG C, the vacuum of 0.08kPa (gauge pressure) again by ester, finally, will
Load weighted aqueous polyurethane is placed in four-hole boiling flask, and pH adjusting agent is added, and the mixing list emulsified is added dropwise when being warming up to 80 DEG C
Body and initiator drip in 2~3h, and keep the temperature 3h at the same temperature, obtain Acrylate Modified Aqueous Polyurethane.
The present invention provides a kind of preparation methods of continuous carbofrax fibre epoxy resin sizing agent, it is according to the following steps
It carries out:
(1), 20-33.5 parts of epoxy resin, 0.85-1.75 parts of wetting agents, 1.0-2.0 parts of creams are added in heating stirring bucket
Agent and 0.5-0.75 parts of self-control film forming agents, and it is uniform in 75 DEG C of at a temperature of high-speed stirred, solution A is made；
(2), 65-71.5 parts of deionized waters are slowly added dropwise made of step (1) in solution A, continue high-speed stirred mixing,
Until forming stable lotion B；
(3), 0.4-0.8 parts of dispersing agents and levelling agent and 0.1-0.3 is added in the last lotion B formed into step (2)
Part preservative, continues to stir evenly, vacuumizes defoaming, as epoxy resin sizing agent.
The present invention also provides a kind of applications of continuous carbofrax fibre epoxy resin sizing agent, are used to prepare silicon carbide
Fiber comprising following steps:
(1), by the silicon carbide fibre after high temperature pyrolysis, with certain wire travelling speed by filling on prepared by the present invention
The sizing groove for starching agent, using drying oven flash baking, wherein the length of drying oven is 5 meters, and drying temperature is 150-180 DEG C,
Drying rate identical as wire travelling speed is 2.0-5.0m/min；
(2), the silicon carbide fibre after drying step (1) is by receiving silk, winding apparatus and paper tube winding to get the company of arriving
Continuous silicon carbide fibre.
By the above-mentioned description to structure of the invention it is found that compared to the prior art, the present invention has the advantage that
1, the continuous carbofrax fibre epoxy resin sizing agent of the present invention, the pottery applied to polycarbosilane precusor conversion
Porcelain fiber, such as the second generation, third generation continuous carbofrax fibre, broadband absorbing continuous carbofrax fibre ceramic fibre, can reinforce
Loose fiber filament bonds bunchy；Being conducive to fiber softening reduces the frictional force of fibre bundle and fibre bundle is made to be easier to weave；Have
Conducive to fiber surface defect hole cover and remedy, improve the intensity of fiber；Be conducive to improve the antistatic property of fiber surface
Can, reduce the hydrone and dust granules in absorption atmosphere.
2, the continuous carbofrax fibre epoxy resin sizing agent of the present invention, it is living using the non-ionic surface of latest generation
Property the components such as agent, dispersing agent, improve dispersion effect and efficiency；These components are mostly to apply in food row, harmless, right
Atmosphere is friendly；Each component is free of alkali metal ion (Li+, Na+, K+), and chemical attack will not be caused to fiber and keeps very good
Good fire-resistant oxidation resistant performance；And various raw material are easy to get, cheap, technique and its equipment are simple, prepared starching
Agent performance is stablized, and is easy, conveniently implements in the continuous production line.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
A kind of continuous carbofrax fibre epoxy resin sizing agent, the continuous carbofrax fibre epoxy resin sizing agent by
The raw material of following parts by weight is made: 65 parts of deionized water, 31 parts of epoxy resin, and dispersing agent and 0.6 part of levelling agent, wetting agent
1.1 parts, 1.5 parts of emulsifier, 0.3 part of preservative, make 0.5 part of film forming agent by oneself.
Epoxy resin is by bisphenol A-type tetraglycidel ether epoxy resin (E20) and bisphenol A-type tetraglycidel ether epoxy resin
(E51) it is mixed according to the ratio that weight ratio is 1:1.
Dispersing agent and levelling agent are carboxymethyl cellulose.
Wetting agent is according to weight ratio by polyoxyethylene sorbitan monostearate and sorbitan fatty ester
The ratio of 1:1 is mixed.
Emulsifier is by castor oil polyoxyethylene ether (EL-80) and octyl phenol polyoxyethylene ether (TX-10) and polyether block
Polymerization amino-modified silicone oil (TF-463) is that 2:2:1 ratio is mixed according to weight ratio.
Self-control film forming agent is Acrylate Modified Aqueous Polyurethane, and wherein the preparation method of Acrylate Modified Aqueous Polyurethane is such as
Under: polyether Glycols (GE220) are dehydrated spare for 24 hours in the case where vacuum (1.066kPa), temperature are 120 DEG C, will be weighed
Good polyether Glycols (GE220) are placed in four-hole boiling flask, after being slowly warming up to 80 DEG C, while isophorone diisocyanate are added
Ester (IPDI) and catalyst are warming up to 100 DEG C of reaction 2h, then cool to 60 DEG C of addition dihydromethyl propionic acids (DMPA) and N- first
Base pyrrolidones (NMP), is slowly warming up to 85 DEG C of reaction 6h, is continuously added acetone in reaction process to reduce the glutinous of reactant
Degree, when nco value reaches theoretical value in system, performed polymer is transferred in high velocity dispersators, is scattered in high-speed stirred molten
In the distilled water for having chain extender and neutralizer, the self-emulsifying polyether type aqueous polyurethane that solid content is 20% is made, then again will
Self-emulsifying polyether type aqueous polyurethane removes solvent under 60 DEG C, the vacuum of 0.08kPa (gauge pressure), finally, by load weighted water
Property polyurethane be placed in four-hole boiling flask, pH adjusting agent is added, the mix monomer and initiator that have emulsified are added dropwise when being warming up to 80 DEG C,
It is dripped in 2~3h, and keeps the temperature 3h at the same temperature, obtain Acrylate Modified Aqueous Polyurethane.
A kind of preparation method of continuous carbofrax fibre epoxy resin sizing agent provided by the invention, it is according to the following steps
It carries out:
(1), 31 parts of epoxy resin, 1.1 parts of wetting agents, 1.5 parts of emulsifiers and 0.5 part of self-control are added in heating stirring bucket
Film forming agent, and it is uniform in 75 DEG C of at a temperature of high-speed stirred, solution A is made；
(2), 65 parts of deionized waters are slowly added dropwise made of step (1) in solution A, continue high-speed stirred mixing, until
Form stable lotion B；
(3), 0.6 part of dispersing agent and levelling agent and 0.3 portion of preservative is added in the last lotion B formed into step (2),
Continue to stir evenly, vacuumizes defoaming, as epoxy resin sizing agent, be denoted as sizing agent -01.
The present invention also provides a kind of applications of continuous carbofrax fibre epoxy resin sizing agent, are used to prepare silicon carbide
Fiber comprising following steps:
(1), by the silicon carbide fibre after high temperature pyrolysis, with certain wire travelling speed by filling on prepared by the present invention
The sizing groove for starching agent, using drying oven flash baking, wherein the length of drying oven is 5 meters, and drying temperature is 150-180 DEG C,
Drying rate identical as wire travelling speed is 2.0-5.0m/min；
(2), the silicon carbide fibre after drying step (1) is by receiving silk, winding apparatus and paper tube winding to get the company of arriving
Continuous silicon carbide fibre, is denoted as fiber sample 01.Its rate of sizing is tested using high-temperature calcination.
Embodiment 2
A kind of continuous carbofrax fibre epoxy resin sizing agent, the continuous carbofrax fibre epoxy resin sizing agent by
The raw material of following parts by weight is made: 71.5 parts of deionized water, 24 parts of epoxy resin, and dispersing agent and 0.5 part of levelling agent, wetting agent
0.85 part, 1.3 parts of emulsifier, 0.2 part of preservative, make 0.7 part of film forming agent by oneself.
Epoxy resin is by bisphenol A-type tetraglycidel ether epoxy resin (E20) and bisphenol A-type tetraglycidel ether epoxy resin
(E51) it is mixed according to the ratio that weight ratio is 1:1.
Dispersing agent and levelling agent are carboxymethyl cellulose.
Wetting agent is according to weight ratio by polyoxyethylene sorbitan monostearate and sorbitan fatty ester
The ratio of 1:1 is mixed.
Emulsifier is by castor oil polyoxyethylene ether (EL-80) and octyl phenol polyoxyethylene ether (TX-10) and polyether block
Polymerization amino-modified silicone oil (TF-463) is that 2:2:1 ratio is mixed according to weight ratio.
Self-control film forming agent is Acrylate Modified Aqueous Polyurethane, and wherein the preparation method of Acrylate Modified Aqueous Polyurethane is such as
Under: polyether Glycols (GE220) are dehydrated spare for 24 hours in the case where vacuum (1.066kPa), temperature are 120 DEG C, will be weighed
Good polyether Glycols (GE220) are placed in four-hole boiling flask, after being slowly warming up to 80 DEG C, while isophorone diisocyanate are added
Ester (IPDI) and catalyst are warming up to 100 DEG C of reaction 2h, then cool to 60 DEG C of addition dihydromethyl propionic acids (DMPA) and N- first
Base pyrrolidones (NMP), is slowly warming up to 85 DEG C of reaction 6h, is continuously added acetone in reaction process to reduce the glutinous of reactant
Degree, when nco value reaches theoretical value in system, performed polymer is transferred in high velocity dispersators, is scattered in high-speed stirred molten
In the distilled water for having chain extender and neutralizer, the self-emulsifying polyether type aqueous polyurethane that solid content is 20% is made, then again will
Self-emulsifying polyether type aqueous polyurethane removes solvent under 60 DEG C, the vacuum of 0.08kPa (gauge pressure), finally, by load weighted water
Property polyurethane be placed in four-hole boiling flask, pH adjusting agent is added, the mix monomer and initiator that have emulsified are added dropwise when being warming up to 80 DEG C,
It is dripped in 2~3h, and keeps the temperature 3h at the same temperature, obtain Acrylate Modified Aqueous Polyurethane.
A kind of preparation method of continuous carbofrax fibre epoxy resin sizing agent provided by the invention, it is according to the following steps
It carries out:
(1), certainly toward 24 parts of epoxy resin of the interior addition of heating stirring bucket, 0.85 part of wetting agent, 1.3 parts of emulsifiers and 0.7 part
Film is made, and uniform in 75 DEG C of at a temperature of high-speed stirred, solution A is made；
(2), 71.5 parts of deionized waters are slowly added dropwise made of step (1) in solution A, continue high-speed stirred mixing, directly
The lotion B stable to formation；
(3), 0.5 part of dispersing agent and levelling agent and 0.2 portion of preservative is added in the last lotion B formed into step (2),
Continue to stir evenly, vacuumizes defoaming, as epoxy resin sizing agent, be denoted as sizing agent -02.
The present invention also provides a kind of applications of continuous carbofrax fibre epoxy resin sizing agent, are used to prepare silicon carbide
Fiber comprising following steps:
(1), by the silicon carbide fibre after high temperature pyrolysis, with certain wire travelling speed by filling on prepared by the present invention
The sizing groove for starching agent, using drying oven flash baking, wherein the length of drying oven is 5 meters, and drying temperature is 150-180 DEG C,
Drying rate identical as wire travelling speed is 2.0-5.0m/min；
(2), the silicon carbide fibre after drying step (1) is by receiving silk, winding apparatus and paper tube winding to get the company of arriving
Continuous silicon carbide fibre, it is denoted as fiber sample 02.Its rate of sizing is tested using high-temperature calcination.
Embodiment 3
A kind of continuous carbofrax fibre epoxy resin sizing agent, the continuous carbofrax fibre epoxy resin sizing agent by
The raw material of following parts by weight is made: 70 parts of deionized water, 26 parts of epoxy resin, and dispersing agent and 0.7 part of levelling agent, wetting agent
0.9 part, 1.5 parts of emulsifier, 0.3 part of preservative, make 0.7 part of film forming agent by oneself.
Epoxy resin is by bisphenol A-type tetraglycidel ether epoxy resin (E20) and bisphenol A-type tetraglycidel ether epoxy resin
(E51) it is mixed according to the ratio that weight ratio is 1:1.
Dispersing agent and levelling agent are carboxymethyl cellulose.
Wetting agent is according to weight ratio by polyoxyethylene sorbitan monostearate and sorbitan fatty ester
The ratio of 1:1 is mixed.
Emulsifier is by castor oil polyoxyethylene ether (EL-80) and octyl phenol polyoxyethylene ether (TX-10) and polyether block
Polymerization amino-modified silicone oil (TF-463) is that 2:2:1 ratio is mixed according to weight ratio.
Self-control film forming agent is Acrylate Modified Aqueous Polyurethane, and wherein the preparation method of Acrylate Modified Aqueous Polyurethane is such as
Under: polyether Glycols (GE220) are dehydrated spare for 24 hours in the case where vacuum (1.066kPa), temperature are 120 DEG C, will be weighed
Good polyether Glycols (GE220) are placed in four-hole boiling flask, after being slowly warming up to 80 DEG C, while isophorone diisocyanate are added
Ester (IPDI) and catalyst are warming up to 100 DEG C of reaction 2h, then cool to 60 DEG C of addition dihydromethyl propionic acids (DMPA) and N- first
Base pyrrolidones (NMP), is slowly warming up to 85 DEG C of reaction 6h, is continuously added acetone in reaction process to reduce the glutinous of reactant
Degree, when nco value reaches theoretical value in system, performed polymer is transferred in high velocity dispersators, is scattered in high-speed stirred molten
In the distilled water for having chain extender and neutralizer, the self-emulsifying polyether type aqueous polyurethane that solid content is 20% is made, then again will
Self-emulsifying polyether type aqueous polyurethane removes solvent under 60 DEG C, the vacuum of 0.08kPa (gauge pressure), finally, by load weighted water
Property polyurethane be placed in four-hole boiling flask, pH adjusting agent is added, the mix monomer and initiator that have emulsified are added dropwise when being warming up to 80 DEG C,
It is dripped in 2~3h, and keeps the temperature 3h at the same temperature, obtain Acrylate Modified Aqueous Polyurethane.
A kind of preparation method of continuous carbofrax fibre epoxy resin sizing agent provided by the invention, it is according to the following steps
It carries out:
(1), 26 parts of epoxy resin, 0.9 part of wetting agent, 1.5 parts of emulsifiers and 0.7 part of self-control are added in heating stirring bucket
Film forming agent, and it is uniform in 75 DEG C of at a temperature of high-speed stirred, solution A is made；
(2), 70 parts of deionized waters are slowly added dropwise made of step (1) in solution A, continue high-speed stirred mixing, until
Form stable lotion B；
(3), 0.7 part of dispersing agent and levelling agent and 0.3 portion of preservative is added in the last lotion B formed into step (2),
Continue to stir evenly, vacuumizes defoaming, as epoxy resin sizing agent, be denoted as sizing agent -03.
The present invention also provides a kind of applications of continuous carbofrax fibre epoxy resin sizing agent, are used to prepare continuous carbon
SiClx fiber comprising following steps:
(1), by the silicon carbide fibre after high temperature pyrolysis, with certain wire travelling speed by filling on prepared by the present invention
The sizing groove for starching agent, using drying oven flash baking, wherein the length of drying oven is 5 meters, and drying temperature is 150-180 DEG C,
Drying rate identical as wire travelling speed is 2.0-5.0m/min；
(2), the silicon carbide fibre after drying step (1) arrives carbon by receiving silk, winding apparatus and paper tube winding
SiClx fiber is denoted as fiber sample 03.Its rate of sizing is tested using high-temperature calcination.
Embodiment 4
A kind of continuous carbofrax fibre epoxy resin sizing agent, the continuous carbofrax fibre epoxy resin sizing agent by
The raw material of following parts by weight is made: 67.5 parts of deionized water, 28.7 parts of epoxy resin, and dispersing agent and 0.8 part of levelling agent, wetting
1.75 parts of agent, 1.0 parts of emulsifier, 0.1 part of preservative, make 0.65 part of film forming agent by oneself.
Epoxy resin is by bisphenol A-type tetraglycidel ether epoxy resin (E20) and bisphenol A-type tetraglycidel ether epoxy resin
(E51) it is mixed according to the ratio that weight ratio is 1:1.
Dispersing agent and levelling agent are carboxymethyl cellulose.
Wetting agent is according to weight ratio by polyoxyethylene sorbitan monostearate and sorbitan fatty ester
The ratio of 1:1 is mixed.
Emulsifier is by castor oil polyoxyethylene ether (EL-80) and octyl phenol polyoxyethylene ether (TX-10) and polyether block
Polymerization amino-modified silicone oil (TF-463) is that 2:2:1 ratio is mixed according to weight ratio.
Self-control film forming agent is Acrylate Modified Aqueous Polyurethane, and wherein the preparation method of Acrylate Modified Aqueous Polyurethane is such as
Under: polyether Glycols (GE220) are dehydrated spare for 24 hours in the case where vacuum (1.066kPa), temperature are 120 DEG C, will be weighed
Good polyether Glycols (GE220) are placed in four-hole boiling flask, after being slowly warming up to 80 DEG C, while isophorone diisocyanate are added
Ester (IPDI) and catalyst are warming up to 100 DEG C of reaction 2h, then cool to 60 DEG C of addition dihydromethyl propionic acids (DMPA) and N- first
Base pyrrolidones (NMP), is slowly warming up to 85 DEG C of reaction 6h, is continuously added acetone in reaction process to reduce the glutinous of reactant
Degree, when nco value reaches theoretical value in system, performed polymer is transferred in high velocity dispersators, is scattered in high-speed stirred molten
In the distilled water for having chain extender and neutralizer, the self-emulsifying polyether type aqueous polyurethane that solid content is 20% is made, then again will
Self-emulsifying polyether type aqueous polyurethane removes solvent under 60 DEG C, the vacuum of 0.08kPa (gauge pressure), finally, by load weighted water
Property polyurethane be placed in four-hole boiling flask, pH adjusting agent is added, the mix monomer and initiator that have emulsified are added dropwise when being warming up to 80 DEG C,
It is dripped in 2~3h, and keeps the temperature 3h at the same temperature, obtain Acrylate Modified Aqueous Polyurethane.
A kind of preparation method of continuous carbofrax fibre epoxy resin sizing agent provided by the invention, it is according to the following steps
It carries out:
(1), 67.5 parts of epoxy resin of addition, 1.75 parts of wetting agents, 1.0 parts of emulsifiers and 0.65 part in heating stirring bucket
It makes film forming agent by oneself, and uniform in 75 DEG C of at a temperature of high-speed stirred, solution A is made；
(2), 67.5 parts of deionized waters are slowly added dropwise made of step (1) in solution A, continue high-speed stirred mixing, directly
The lotion B stable to formation；
(3), 0.8 part of dispersing agent and levelling agent and 0.1 portion of preservative is added in the last lotion B formed into step (2),
Continue to stir evenly, vacuumizes defoaming, as epoxy resin sizing agent, be denoted as sizing agent -04.
The present invention also provides a kind of applications of continuous carbofrax fibre epoxy resin sizing agent, are used to prepare continuous carbon
SiClx fiber comprising following steps:
(1), by the silicon carbide fibre after high temperature pyrolysis, with certain wire travelling speed by filling on prepared by the present invention
The sizing groove for starching agent, using drying oven flash baking, wherein the length of drying oven is 5 meters, and drying temperature is 150-180 DEG C,
Drying rate identical as wire travelling speed is 2.0-5.0m/min；
(2), the silicon carbide fibre after drying step (1) arrives carbon by receiving silk, winding apparatus and paper tube winding
SiClx fiber is denoted as fiber sample 04.Its rate of sizing is tested using high-temperature calcination.
Embodiment 5
A kind of continuous carbofrax fibre epoxy resin sizing agent, the continuous carbofrax fibre epoxy resin sizing agent by
The raw material of following parts by weight is made: 70 parts of deionized water, 33.5 parts of epoxy resin, and dispersing agent and 0.4 part of levelling agent, wetting agent
1.5 parts, 2.0 parts of emulsifier, 0.25 part of preservative, make 0.75 part of film forming agent by oneself.
Epoxy resin is by bisphenol A-type tetraglycidel ether epoxy resin (E20) and bisphenol A-type tetraglycidel ether epoxy resin
(E51) it is mixed according to the ratio that weight ratio is 1:1.
Dispersing agent and levelling agent are carboxymethyl cellulose.
Wetting agent is according to weight ratio by polyoxyethylene sorbitan monostearate and sorbitan fatty ester
The ratio of 1:1 is mixed.
Emulsifier is by castor oil polyoxyethylene ether (EL-80) and octyl phenol polyoxyethylene ether (TX-10) and polyether block
Polymerization amino-modified silicone oil (TF-463) is that 2:2:1 ratio is mixed according to weight ratio.
Self-control film forming agent is Acrylate Modified Aqueous Polyurethane, and wherein the preparation method of Acrylate Modified Aqueous Polyurethane is such as
Under: polyether Glycols (GE220) are dehydrated spare for 24 hours in the case where vacuum (1.066kPa), temperature are 120 DEG C, will be weighed
Good polyether Glycols (GE220) are placed in four-hole boiling flask, after being slowly warming up to 80 DEG C, while isophorone diisocyanate are added
Ester (IPDI) and catalyst are warming up to 100 DEG C of reaction 2h, then cool to 60 DEG C of addition dihydromethyl propionic acids (DMPA) and N- first
Base pyrrolidones (NMP), is slowly warming up to 85 DEG C of reaction 6h, is continuously added acetone in reaction process to reduce the glutinous of reactant
Degree, when nco value reaches theoretical value in system, performed polymer is transferred in high velocity dispersators, is scattered in high-speed stirred molten
In the distilled water for having chain extender and neutralizer, the self-emulsifying polyether type aqueous polyurethane that solid content is 20% is made, then again will
Self-emulsifying polyether type aqueous polyurethane removes solvent under 60 DEG C, the vacuum of 0.08kPa (gauge pressure), finally, by load weighted water
Property polyurethane be placed in four-hole boiling flask, pH adjusting agent is added, the mix monomer and initiator that have emulsified are added dropwise when being warming up to 80 DEG C,
It is dripped in 2~3h, and keeps the temperature 3h at the same temperature, obtain Acrylate Modified Aqueous Polyurethane.
A kind of preparation method of continuous carbofrax fibre epoxy resin sizing agent provided by the invention, it is according to the following steps
It carries out:
(1), 33.5 parts of epoxy resin of addition, 1.5 parts of wetting agents, 2.0 parts of emulsifiers and 0.75 part in heating stirring bucket
It makes film forming agent by oneself, and uniform in 75 DEG C of at a temperature of high-speed stirred, solution A is made；
(2), 70 parts of deionized waters are slowly added dropwise made of step (1) in solution A, continue high-speed stirred mixing, until
Form stable lotion B；
(3), 0.4 part of dispersing agent and levelling agent and 0.25 part of anti-corrosion is added in the last lotion B formed into step (2)
Agent continues to stir evenly, and vacuumizes defoaming, as epoxy resin sizing agent, is denoted as sizing agent -05.
The present invention also provides a kind of applications of continuous carbofrax fibre epoxy resin sizing agent, are used to prepare silicon carbide
Fiber comprising following steps:
(1), by the silicon carbide fibre after high temperature pyrolysis, with certain wire travelling speed by filling on prepared by the present invention
The sizing groove for starching agent, using drying oven flash baking, wherein the length of drying oven is 5 meters, and drying temperature is 150-180 DEG C,
Drying rate identical as wire travelling speed is 2.0-5.0m/min；
(2), the silicon carbide fibre after drying step (1) is by receiving silk, winding apparatus and paper tube winding to get the company of arriving
Continuous silicon carbide fibre, is denoted as fiber sample 05.Its rate of sizing is tested using high-temperature calcination.
The rate of sizing of 1 silicon carbide fibre of table under the conditions of different sizing agents and its sizing technique
| Sizing agent serial number | Fiber sample serial number | The rate of sizing |
| Sizing agent 01 | Fiber sample 01 | 0.21% |
| Sizing agent 02 | Fiber sample 02 | 2.87% |
| Sizing agent 03 | Fiber sample 03 | 0.55% |
| Sizing agent 04 | Fiber sample 04 | 1.87% |
| Sizing agent 05 | Fiber sample 05 | 2.08 |
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of continuous carbofrax fibre epoxy resin sizing agent, which is characterized in that the continuous carbofrax fibre asphalt mixtures modified by epoxy resin
Rouge sizing agent is prepared from the following raw materials in parts by weight: 65-71.5 parts of deionized water, 20-33.5 parts of epoxy resin, dispersing agent is simultaneous
0.4-0.8 parts of levelling agent, 0.85-1.75 parts of wetting agent, 1.0-2.0 parts of emulsifier, preservative 0.1-0.3, make film forming agent by oneself
0.5-0.75 parts.
2. a kind of continuous carbofrax fibre epoxy resin sizing agent, it is characterised in that: the epoxy resin is shunk by bisphenol A-type
Glycerin ether epoxy resin (E20) and bisphenol A-type tetraglycidel ether epoxy resin (E51) are carried out according to the ratio that weight ratio is 1:1
Mixing.
3. a kind of continuous carbofrax fibre epoxy resin sizing agent according to claim 1, it is characterised in that: described point
Powder and levelling agent are carboxymethyl cellulose.
4. a kind of continuous carbofrax fibre epoxy resin sizing agent according to claim 1, it is characterised in that: the profit
Humectant by polyoxyethylene sorbitan monostearate and sorbitan fatty ester according to the ratio that weight ratio is 1:1 into
Row mixing.
5. a kind of continuous carbofrax fibre epoxy resin sizing agent according to claim 1, it is characterised in that: the cream
Agent is changed by castor oil polyoxyethylene ether (EL-80) and octyl phenol polyoxyethylene ether (TX-10) and polyether block polymerization amino
Property silicone oil (TF-463) according to weight ratio be 2:2:1 ratio mixed.
6. a kind of continuous carbofrax fibre epoxy resin sizing agent according to claim 1, it is characterised in that: described anti-
Rotten agent is to carboxyl propyl benzoate.
7. a kind of continuous carbofrax fibre epoxy resin sizing agent according to claim 1, it is characterised in that: it is described from
Be made film be Acrylate Modified Aqueous Polyurethane, wherein Acrylate Modified Aqueous Polyurethane the preparation method is as follows: by polyethers
Dihydric alcohol (GE220) vacuum (1.066kPa), temperature be 120 DEG C in the case where be dehydrated it is spare for 24 hours, by load weighted polyethers two
First alcohol (GE220) is placed in four-hole boiling flask, after being slowly warming up to 80 DEG C, while be added isophorone diisocyanate (IPDI) and
Catalyst is warming up to 100 DEG C of reaction 2h, then cools to 60 DEG C of addition dihydromethyl propionic acids (DMPA) and N-Methyl pyrrolidone
(NMP), 85 DEG C of reaction 6h are slowly warming up to, are continuously added acetone to reduce the viscosity of reactant, when in system in reaction process
When nco value reaches theoretical value, performed polymer is transferred in high velocity dispersators, is scattered in dissolved with chain extender in high-speed stirred
In the distilled water of agent, the self-emulsifying polyether type aqueous polyurethane that solid content is 20% is made, then again by self-emulsifying polyether-type
Aqueous polyurethane removes solvent under 60 DEG C, the vacuum of 0.08kPa (gauge pressure), finally, load weighted aqueous polyurethane is placed in
In four-hole boiling flask, pH adjusting agent is added, the mix monomer and initiator emulsified is added dropwise when being warming up to 80 DEG C, is added dropwise in 2~3h
It is complete, and 3h is kept the temperature at the same temperature, obtain Acrylate Modified Aqueous Polyurethane.
8. a kind of preparation side of continuous carbofrax fibre epoxy resin sizing agent according to any one of claims 1 to 7
Method, it is characterised in that it is sequentially included the following steps:
(1), 20-33.5 parts of epoxy resin, 0.85-1.75 parts of wetting agents, 1.0-2.0 parts of emulsifiers are added in heating stirring bucket
It is and uniform in 75 DEG C of at a temperature of high-speed stirred with 0.5-0.75 parts of self-control film forming agents, solution A is made；
(2), 65-71.5 parts of deionized waters are slowly added dropwise made of step (1) in solution A, continue high-speed stirred mixing, until
Form stable lotion B；
(3), 0.4-0.8 parts of dispersing agents and levelling agent is added in the last lotion B formed into step (2) and 0.1-0.3 parts anti-
Rotten agent continues to stir evenly, and vacuumizes defoaming, as epoxy resin sizing agent.
9. according to claim 1 to the application of any one of 7 continuous carbofrax fibre epoxy resin sizing agents, which is characterized in that
It is used to prepare silicon carbide fibre.
10. the application of continuous carbofrax fibre epoxy resin sizing agent according to claim 9, which is characterized in that packet
Include following steps:
(1), by the silicon carbide fibre after high temperature pyrolysis, with certain wire travelling speed by filling sizing agent prepared by the present invention
Sizing groove, using drying oven flash baking, wherein the length of drying oven be 5 meters, drying temperature be 150-180 DEG C, drying
Speed identical as wire travelling speed is 2.0-5.0m/min；(2), silicon carbide fibre after drying step (1) through receipts silk,
Winding apparatus and paper tube wind to arrive continuous carbofrax fibre.
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| CN116180451A (en) * | 2023-03-01 | 2023-05-30 | 湖南泽睿新材料有限公司 | A kind of continuous silicon carbide fiber sizing agent and its application |
| CN118529947A (en) * | 2024-05-21 | 2024-08-23 | 巨石集团有限公司 | A low-hair fiber glass film-forming agent and its preparation method, sizing agent, product and application |
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| CN118529947A (en) * | 2024-05-21 | 2024-08-23 | 巨石集团有限公司 | A low-hair fiber glass film-forming agent and its preparation method, sizing agent, product and application |
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Application publication date: 20190816 |