CN114855310A - Production method of organic silicon carbon fiber precursor oiling agent - Google Patents
Production method of organic silicon carbon fiber precursor oiling agent Download PDFInfo
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- CN114855310A CN114855310A CN202111606151.8A CN202111606151A CN114855310A CN 114855310 A CN114855310 A CN 114855310A CN 202111606151 A CN202111606151 A CN 202111606151A CN 114855310 A CN114855310 A CN 114855310A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 30
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 239000002243 precursor Substances 0.000 title claims abstract description 27
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000008041 oiling agent Substances 0.000 title claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 239000003921 oil Substances 0.000 claims abstract description 20
- 230000000694 effects Effects 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 37
- 239000002994 raw material Substances 0.000 claims description 35
- 239000003054 catalyst Substances 0.000 claims description 20
- 239000010779 crude oil Substances 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000003381 stabilizer Substances 0.000 claims description 13
- 239000006260 foam Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 10
- 239000002518 antifoaming agent Substances 0.000 claims description 10
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 10
- -1 polydimethylsiloxane Polymers 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- 229920002545 silicone oil Polymers 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 6
- NLSFWPFWEPGCJJ-UHFFFAOYSA-N 2-methylprop-2-enoyloxysilicon Chemical compound CC(=C)C(=O)O[Si] NLSFWPFWEPGCJJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004593 Epoxy Substances 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 5
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 239000003945 anionic surfactant Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 5
- 239000000194 fatty acid Substances 0.000 claims description 5
- 229930195729 fatty acid Natural products 0.000 claims description 5
- 150000004665 fatty acids Chemical class 0.000 claims description 5
- 150000002191 fatty alcohols Chemical class 0.000 claims description 5
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002736 nonionic surfactant Substances 0.000 claims description 5
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical group C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000077 silane Inorganic materials 0.000 claims description 5
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 claims description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 5
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 5
- UJUWNSRXIGHHKM-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;didodecyl hydrogen phosphate Chemical compound OCC[NH+](CCO)CCO.CCCCCCCCCCCCOP([O-])(=O)OCCCCCCCCCCCC UJUWNSRXIGHHKM-UHFFFAOYSA-N 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002485 combustion reaction Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 27
- 239000000047 product Substances 0.000 abstract description 14
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 12
- 239000003063 flame retardant Substances 0.000 abstract description 12
- 239000003995 emulsifying agent Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 239000012466 permeate Substances 0.000 abstract description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 abstract description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 abstract description 3
- 229920013822 aminosilicone Polymers 0.000 abstract description 2
- 238000004945 emulsification Methods 0.000 abstract description 2
- 239000000839 emulsion Substances 0.000 abstract description 2
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 abstract 1
- 238000004513 sizing Methods 0.000 description 12
- 239000004744 fabric Substances 0.000 description 9
- 239000004094 surface-active agent Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000009972 noncorrosive effect Effects 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 238000006864 oxidative decomposition reaction Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- 239000012209 synthetic fiber Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229940087291 tridecyl alcohol Drugs 0.000 description 2
- BIHQJMSIEXRWPS-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;dodecyl dihydrogen phosphate Chemical compound OCCN(CCO)CCO.CCCCCCCCCCCCOP(O)(O)=O BIHQJMSIEXRWPS-UHFFFAOYSA-N 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/14—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with organic compounds, e.g. macromolecular compounds
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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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
- D01F11/123—Oxides
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a production method of an organic silicon carbon fiber precursor oiling agent, which relates to the technical field of organic silicon carbon fiber precursor oiling agents, and is characterized in that in the production of the traditional organic silicon carbon fiber precursor oiling agent, an environment-friendly type emulsifier with an isomeric tridecyl alcohol-polyoxyethylene ether chemical structure is used as a main emulsifier, 2 to 3 different EO number emulsifiers are selected and are matched with the HLB (hydrophile-lipophile balance) value of amino silicone oil to achieve the optimal emulsification and emulsion stabilization effects, meanwhile, a bundling agent is added into an oil product to enable the fiber to have proper viscosity and improve the saturation performance of the fiber, and meanwhile, an anti-flaming agent is arranged to enhance the flame retardant performance of the fiber, so that when the oil product deeply permeates into the fiber, the fiber can be well protected.
Description
Technical Field
The invention relates to the technical field of organic silicon carbon fiber precursor oiling agents, in particular to a production method of an organic silicon carbon fiber precursor oiling agent.
Background
The polyacrylonitrile-based carbon fiber is subjected to high-temperature processing for a long time in the production process, so that a fragile fiber precursor needs an oil agent with stable performance, high temperature resistance and good smoothness to protect the fiber from various damages as little as possible in the whole processing process, it is required that an oil agent is left on the fiber as much as possible from the early stage of the normal-temperature processing process of the carbon fiber precursor to the pre-oxidation of 300 ℃ and the high-temperature carbonization of more than 1000 ℃ to play a role in protection, and simultaneously, during the use process of the fiber, because the fiber has no obvious flame retardant property, the fiber can be rapidly combusted when encountering fire, and the production process technology of the carbon fiber is rapidly developed and innovated along with the continuous expansion of the application of the carbon fiber, the application prospect is very wide, the product development potential is huge, and therefore the organic silicon carbon fiber precursor oiling agent with excellent product performance has very important significance for the stable and high-speed development of the whole carbon fiber industry.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a production method of an organic silicon carbon fiber precursor oiling agent.
In order to achieve the purpose, the invention adopts the following technical scheme: the production method of the organic silicon carbon fiber precursor oiling agent comprises the following steps:
s1: mixing raw materials, namely firstly adding 80-95% of hydroxyl-terminated polydimethylsiloxane, 0.05-5.0% of organic silicon coupling agent and 0.1-5.0% of silane coupling agent as basic raw materials into a stirring kettle, then controlling the temperature of the stirring kettle at 50-60 ℃, and starting stirring equipment in the reaction kettle to enable the raw materials to carry out polymerization reaction at the stirring speed of 12500-17500 r/min;
s2: adding a catalyst, and then continuously adding 0.005-0.08% of an alkali catalyst into the stirring kettle, so as to accelerate the chemical reaction rate of the raw materials and improve the production capacity, wherein in the mixing process of the catalyst, the temperature in the stirring kettle is kept at 60-120 ℃, and the stirring time is 20-36 min;
s3: mixing additives, namely after the raw materials are preliminarily mixed, adding 0.5-1.5% of defoaming agent, 0.4-0.8% of stabilizing agent, 0.5-4% of bundling agent and 0.8-1.5% of anti-combustion agent into the reaction kettle, so as to destroy the stability factor of foam, realize the defoaming effect, improve the stability of raw material mixing, simultaneously control the temperature of the reaction kettle to be 120-135 ℃, and then carry out reaction mixing for 10-24 min;
s4: extracting crude oil, closing the reaction kettle to stop the stirring equipment in the reaction kettle, standing the crude oil in the reaction kettle for a period of time, and storing the crude oil in a container to obtain a finished product.
In order to produce different effects, the invention improves that in step S1, the polydimethylsiloxane with terminal hydroxyl can be replaced by octamethylcyclotetrasiloxane.
In order to improve the stability of oil products, the invention improves that in step S1, the organosilicon coupling agent is one or more of N-aminoethyl-3-aminopropylmethyldimethoxysilane, Y-aminopropyltrimethoxysilane or Y-aminopropyltriethoxysilane.
In order to prepare crude oil, the invention improves that in step S1, the silane coupling agent is one or more of vinyl silane, amino silane, epoxy silane, mercapto silane or methacryloxy silane.
In order to accelerate the reaction rate of the raw materials, the invention improves that in step S2, the alkali catalyst is one or more of potassium hydroxide, sodium hydroxide or potassium carbonate.
In order to eliminate the foam generated during the mixing, the invention improves that in the step S3, the defoaming agent is one or more of tributyl phosphate or water-based silicone oil.
In order to stably mix the raw materials, the present invention improves that in step S3, the stabilizer is formed by mixing fluorocarbon group-modified silicone oil, fatty acid and fatty alcohol, and the mixing ratio is 2:1: 1.
In order to improve the saturation of the fiber, the invention improves that in step S3, the bundling agent is formed by mixing monododecyl phosphate triethanolamine, an anionic surfactant, a nonionic surfactant and sodium bicarbonate, and the mixing ratio is 1:0.5:4: 0.05.
In order to improve the flame retardant property of the fiber, the invention improves that in step S3, the flame retardant is one or more of antimony trioxide, magnesium hydroxide or aluminum hydroxide.
In order to prepare the finished product, the invention improves the method that in the step S4, the standing and cooling time is 15-20min, and the temperature in the stirring kettle is 15-20 ℃.
Compared with the prior art, the invention has the advantages and positive effects that,
in the invention, in the production of the traditional organic silicon carbon fiber precursor oil agent, an environment-friendly emulsifier with an isomeric tridecyl alcohol polyoxyethylene ether chemical structure is used as a main emulsifier, the emulsifier with the isomeric tridecyl alcohol polyoxyethylene ether chemical structure is selected, 2 to 3 emulsifiers with different EO numbers are compounded to match the HLB value of amino silicone oil to achieve the optimal emulsification and emulsion stabilization effects, meanwhile, a bundling agent is added into an oil product to ensure that the fiber has proper viscosity and improve the saturation performance of the fiber, and meanwhile, the flame retardant property of the fiber is enhanced by arranging the flame retardant, so that when the oil product deeply permeates into the fiber, the fiber can be well protected.
Drawings
Fig. 1 is a preparation flow chart of the production method of the organic silicon carbon fiber precursor oiling agent provided by the invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be further described with reference to the accompanying drawings and examples. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and thus the present invention is not limited to the specific embodiments of the present disclosure.
In a first embodiment, referring to fig. 1, the present invention provides a technical solution: the production method of the organic silicon carbon fiber precursor oiling agent comprises the following steps:
s1: mixing raw materials, namely adding 85% of hydroxyl-terminated polydimethylsiloxane, 5% of organosilicon coupling agent and 5% of silane coupling agent as basic raw materials into a stirring kettle, controlling the temperature of the stirring kettle at 55 ℃, and starting stirring equipment in the reaction kettle to enable the raw materials to carry out polymerization reaction at the stirring speed of 13000 r/min;
s2: adding a catalyst, and then continuously adding 0.08% of an alkali catalyst into the stirring kettle, so as to accelerate the chemical reaction rate of the raw materials and improve the production capacity, wherein in the mixing process of the catalyst, the temperature in the stirring kettle is kept at 75 ℃, and the stirring time is 25 min;
s3: mixing additives, namely adding 1% of defoaming agent, 0.42% of stabilizing agent, 3% of bundling agent and 1.5% of flame retardant into the reaction kettle after the raw materials are preliminarily mixed, so that the stability factor of foam is damaged to realize the defoaming effect, the stability of raw material mixing is improved, the temperature of the reaction kettle is controlled at 130 ℃, and the raw materials are reacted and mixed for 15 min;
s4: extracting crude oil, closing the reaction kettle to stop the stirring equipment in the reaction kettle, standing the crude oil in the reaction kettle for a period of time, and storing the crude oil in a container to obtain a finished product.
In step S1, the hydroxyl terminated polydimethylsiloxane may also be replaced with octamethylcyclotetrasiloxane.
In step S1, the organosilicon coupling agent is one or more of N-aminoethyl-3-aminopropylmethyldimethoxysilane, Y-aminopropyltrimethoxysilane or Y-aminopropyltriethoxysilane.
In step S1, the silane coupling agent is one or more of vinyl silane, amino silane, epoxy silane, mercapto silane, or methacryloxy silane.
In step S2, the base catalyst is one or more of potassium hydroxide, sodium hydroxide, or potassium carbonate.
In step S3, the defoaming agent is one or more of tributyl phosphate and water-based silicone oil, and is used to reduce the surface tension of water, solution, suspension, etc., to prevent the formation of foam, or to reduce or eliminate the original foam.
In step S3, the stabilizer is prepared by mixing fluorocarbon-based modified silicone oil, fatty acid and fatty alcohol at a ratio of 2:1:1, and by providing the stabilizer, the reaction is slowed down, chemical equilibrium is maintained, surface tension is reduced, and light, thermal decomposition or oxidative decomposition is prevented.
In step S3, the sizing agent is a mixture of didodecyl phosphate triethanolamine, an anionic surfactant, a nonionic surfactant and sodium bicarbonate, and the mixing ratio is 1:0.5:4:0.05, and the sizing agent is provided to enhance the sizing property of the synthetic fiber and to increase the fineness and strength thereof, so that the surfactant two added to the spin finish obtains the sizing property by utilizing the cohesive force generated by the action of the surfactant two with water.
In step S3, the anti-flaming agent is one or more of antimony trioxide, magnesium hydroxide or aluminum hydroxide, and is mixed with colorless transparent, non-combustible, non-toxic, non-corrosive and non-polluting additives, and is easy to permeate into the fiber fabric, and can remain between the surface of the fiber fabric and the fiber, and can generate complex chemical reaction under high temperature, and the product has obvious flame retardant and fireproof effects on the fabric to be treated.
In step S4, the standing cooling time was 20min while the stirred tank internal temperature was 18 ℃.
In a second embodiment, referring to fig. 1, the present invention provides a technical solution: the production method of the organic silicon carbon fiber precursor oiling agent comprises the following steps:
s1: mixing raw materials, namely adding 90% of hydroxyl-terminated polydimethylsiloxane, 4.5% of organosilicon coupling agent and 3.5% of silane coupling agent as basic raw materials into a stirring kettle, controlling the temperature of the stirring kettle at 58 ℃, and starting stirring equipment in the reaction kettle to enable the raw materials to carry out polymerization reaction at the stirring speed of 14550 r/min;
s2: adding a catalyst, and then continuously adding 0.06% of an alkali catalyst into the stirring kettle, so as to accelerate the chemical reaction rate of the raw materials and improve the production capacity, wherein in the mixing process of the catalyst, the temperature in the stirring kettle is kept at 110 ℃, and the stirring time is 30 min;
s3: mixing additives, namely adding 1.5% of defoaming agent, 0.75% of stabilizing agent, 0.5% of bundling agent and 0.69% of flame retardant into the reaction kettle after the raw materials are preliminarily mixed, so that the stability factor of foam is damaged, the defoaming effect is realized, the stability of raw material mixing is improved, meanwhile, the temperature of the reaction kettle is controlled at 135 ℃, and the raw materials are reacted and mixed for 13 min;
s4: extracting crude oil, closing the reaction kettle to stop the stirring equipment in the reaction kettle, standing the crude oil in the reaction kettle for a period of time, and storing the crude oil in a container to obtain a finished product.
In step S1, the hydroxyl terminated polydimethylsiloxane may also be replaced with octamethylcyclotetrasiloxane.
In step S1, the organosilicon coupling agent is one or more of N-aminoethyl-3-aminopropylmethyldimethoxysilane, Y-aminopropyltrimethoxysilane or Y-aminopropyltriethoxysilane.
In step S1, the silane coupling agent is one or more of vinyl silane, amino silane, epoxy silane, mercapto silane, or methacryloxy silane.
In step S2, the base catalyst is one or more of potassium hydroxide, sodium hydroxide, or potassium carbonate.
In step S3, the defoaming agent is one or more of tributyl phosphate and water-based silicone oil, and is used to reduce the surface tension of water, solution, suspension, etc., to prevent the formation of foam, or to reduce or eliminate the original foam.
In step S3, the stabilizer is prepared by mixing fluorocarbon-based modified silicone oil, fatty acid and fatty alcohol at a ratio of 2:1:1, and by providing the stabilizer, the reaction is slowed down, chemical equilibrium is maintained, surface tension is reduced, and light, thermal decomposition or oxidative decomposition is prevented.
In step S3, the sizing agent is a mixture of didodecyl phosphate triethanolamine, an anionic surfactant, a nonionic surfactant and sodium bicarbonate, and the mixing ratio is 1:0.5:4:0.05, and the sizing agent is provided to enhance the sizing property of the synthetic fiber and to increase the fineness and strength thereof, so that the surfactant two added to the spin finish obtains the sizing property by utilizing the cohesive force generated by the action of the surfactant two with water.
In step S3, the anti-flaming agent is one or more of antimony trioxide, magnesium hydroxide or aluminum hydroxide, and is mixed with colorless transparent, non-combustible, non-toxic, non-corrosive and non-polluting additives, and is easy to permeate into the fiber fabric, and can remain between the surface of the fiber fabric and the fiber, and can generate complex chemical reaction under high temperature, and the product has obvious flame retardant and fireproof effects on the fabric to be treated.
In step S4, the standing cooling time was 18min while the stirred tank internal temperature was 20 ℃.
In a third embodiment, referring to fig. 1, the present invention provides a technical solution: the production method of the organic silicon carbon fiber precursor oiling agent comprises the following steps:
s1: mixing raw materials, namely firstly adding 88 percent of hydroxyl-terminated polydimethylsiloxane, 3.5 percent of organosilicon coupling agent and 4 percent of silane coupling agent as basic raw materials into a stirring kettle, then controlling the temperature of the stirring kettle at 52 ℃, and starting stirring equipment in the reaction kettle to ensure that the raw materials can carry out polymerization reaction at the stirring speed of 16000 r/min;
s2: adding a catalyst, and then continuously adding 0.55% of an alkali catalyst into the stirring kettle, so as to accelerate the chemical reaction rate of the raw materials and improve the production capacity, wherein in the mixing process of the catalyst, the temperature in the stirring kettle is kept at 115 ℃, and the stirring time is 26 min;
s3: mixing additives, namely adding 0.95% of defoaming agent, 0.8% of stabilizing agent, 0.7% of bundling agent and 1.5% of flame retardant into the reaction kettle after the raw materials are preliminarily mixed, so that the stability factor of foam is damaged, the defoaming effect is realized, the stability of raw material mixing is improved, the temperature of the reaction kettle is controlled at 122 ℃, and the raw materials are reacted and mixed for 20 min;
s4: extracting crude oil, closing the reaction kettle to stop the stirring equipment in the reaction kettle, standing the crude oil in the reaction kettle for a period of time, and storing the crude oil in a container to obtain a finished product.
In step S1, the hydroxyl terminated polydimethylsiloxane may also be replaced with octamethylcyclotetrasiloxane.
In step S1, the organosilicon coupling agent is one or more of N-aminoethyl-3-aminopropylmethyldimethoxysilane, Y-aminopropyltrimethoxysilane or Y-aminopropyltriethoxysilane.
In step S1, the silane coupling agent is one or more of vinyl silane, amino silane, epoxy silane, mercapto silane, or methacryloxy silane.
In step S2, the base catalyst is one or more of potassium hydroxide, sodium hydroxide, or potassium carbonate.
In step S3, the defoaming agent is one or more of tributyl phosphate and water-based silicone oil, and is used to reduce the surface tension of water, solution, suspension, etc., to prevent the formation of foam, or to reduce or eliminate the original foam.
In step S3, the stabilizer is prepared by mixing fluorocarbon-based modified silicone oil, fatty acid and fatty alcohol at a ratio of 2:1:1, and by providing the stabilizer, the reaction is slowed down, chemical equilibrium is maintained, surface tension is reduced, and light, thermal decomposition or oxidative decomposition is prevented.
In step S3, the sizing agent is a mixture of didodecyl phosphate triethanolamine, an anionic surfactant, a nonionic surfactant and sodium bicarbonate, and the mixing ratio is 1:0.5:4:0.05, and the sizing agent is provided to enhance the sizing property of the synthetic fiber and to increase the fineness and strength thereof, so that the surfactant two added to the spin finish obtains the sizing property by utilizing the cohesive force generated by the action of the surfactant two with water.
In step S3, the anti-flaming agent is one or more of antimony trioxide, magnesium hydroxide or aluminum hydroxide, and is mixed with colorless transparent, non-combustible, non-toxic, non-corrosive and non-polluting additives, and is easy to permeate into the fiber fabric, and can remain between the surface of the fiber fabric and the fiber, and can generate complex chemical reaction under high temperature, and the product has obvious flame retardant and fireproof effects on the fabric to be treated.
In step S4, the standing cooling time was 15min while the stirred tank internal temperature was 20 ℃.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes, without departing from the technical spirit of the present invention, and any simple modification, equivalent change and change made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the technical spirit of the present invention.
Claims (10)
1. The production method of the organic silicon carbon fiber precursor oiling agent is characterized by comprising the following steps:
s1: mixing raw materials, namely firstly adding 80-95% of hydroxyl-terminated polydimethylsiloxane, 0.05-5.0% of organic silicon coupling agent and 0.1-5.0% of silane coupling agent as basic raw materials into a stirring kettle, then controlling the temperature of the stirring kettle at 50-60 ℃, and starting stirring equipment in the reaction kettle to enable the raw materials to carry out polymerization reaction at the stirring speed of 12500-17500 r/min;
s2: adding a catalyst, and then continuously adding 0.005-0.08% of an alkali catalyst into the stirring kettle, so as to accelerate the chemical reaction rate of the raw materials and improve the production capacity, wherein in the mixing process of the catalyst, the temperature in the stirring kettle is kept at 60-120 ℃, and the stirring time is 20-36 min;
s3: mixing additives, namely after the raw materials are preliminarily mixed, adding 0.5-1.5% of defoaming agent, 0.4-0.8% of stabilizing agent, 0.5-4% of bundling agent and 0.8-1.5% of anti-combustion agent into the reaction kettle, so as to destroy the stability factor of foam, realize the defoaming effect, improve the stability of raw material mixing, simultaneously control the temperature of the reaction kettle to be 120-135 ℃, and then carry out reaction mixing for 10-24 min;
s4: extracting crude oil, closing the reaction kettle to stop the stirring equipment in the reaction kettle, standing the crude oil in the reaction kettle for a period of time, and storing the crude oil in a container to obtain a finished product.
2. The method for producing the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S1, the hydroxyl terminated polydimethylsiloxane may also be replaced with octamethylcyclotetrasiloxane.
3. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S1, the organosilicon coupling agent is one or more of N-aminoethyl-3-aminopropylmethyldimethoxysilane, Y-aminopropyltrimethoxysilane or Y-aminopropyltriethoxysilane.
4. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S1, the silane coupling agent is one or more of vinyl silane, amino silane, epoxy silane, mercapto silane, or methacryloxy silane.
5. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S2, the base catalyst is one or more of potassium hydroxide, sodium hydroxide, or potassium carbonate.
6. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S3, the defoaming agent is one or more of tributyl phosphate or water-based silicone oil.
7. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S3, the stabilizer is formed by mixing fluorocarbon-based modified silicone oil, fatty acid and fatty alcohol, and the mixing ratio is 2:1: 1.
8. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S3, the bundling agent is formed by mixing didodecyl phosphate triethanolamine, an anionic surfactant, a nonionic surfactant and sodium bicarbonate, and the mixing ratio is 1:0.5:4: 0.05.
9. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S3, the anti-flaming agent is one or more of antimony trioxide, magnesium hydroxide or aluminum hydroxide.
10. The production method of the organic silicon carbon fiber precursor oil agent according to claim 1, characterized in that: in step S4, the standing and cooling time is 15-20min, and the temperature in the stirring kettle is 15-20 ℃.
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