CN106543497A - A kind of oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping and preparation method thereof - Google Patents

A kind of oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping and preparation method thereof Download PDF

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Publication number
CN106543497A
CN106543497A CN201610913640.0A CN201610913640A CN106543497A CN 106543497 A CN106543497 A CN 106543497A CN 201610913640 A CN201610913640 A CN 201610913640A CN 106543497 A CN106543497 A CN 106543497A
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carbon fiber
oil
resistant
oil pipe
pressure oil
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CN201610913640.0A
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吴传兴
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Maanshan Jiechuang Plastic Science & Technology Co Ltd
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Maanshan Jiechuang Plastic Science & Technology Co Ltd
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Priority to CN201610913640.0A priority Critical patent/CN106543497A/en
Publication of CN106543497A publication Critical patent/CN106543497A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F132/00—Homopolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system
    • C08F132/02—Homopolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system having no condensed rings
    • C08F132/06—Homopolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system having no condensed rings having two or more carbon-to-carbon double bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • 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
    • C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
    • C08G18/4269—Lactones
    • C08G18/4277—Caprolactone and/or substituted caprolactone
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/18—Applications used for pipes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Rigid Pipes And Flexible Pipes (AREA)

Abstract

The invention discloses a kind of the oil resistant resistant material and its preparation technology for high-pressure oil pipe of modified carbon fiber doping, it is characterised in that with butadiene（Polymer grade）, naphthenic oil, nickel naphthenate, triisobutyl aluminium, boron trifluoride etherate, octanal, polycaprolactone diols, graphite, antioxidant TNP, UV absorbent UV 9, toluene di-isocyanate(TDI), dimethythiotoluene diamine, multi-walled carbon nano-tubes, dimethylformamide, dodecylbenzene sodium sulfonate, Silicon chloride., dcpd resin, nylon, carbon fiber etc. be raw material.The present invention is prepared for hydrolysis resistant polyurethane elastomer by prepolymer method, and graphite there occurs intercalation polymeric and favorable dispersibility in the base with polyurethane matrix；The multi-walled carbon nano-tubes being uniformly dispersed, amidine functional group is contained on surface is prepared for, the compatibility between nylon is improved, the dispersibility in nylon matrix is improve；Obtain a kind of oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping.

Description

A kind of doping of modified carbon fiber for high-pressure oil pipe oil resistant resistant material and its Preparation method
Technical field
The present invention relates to processing of high molecular material technology, and in particular to a kind of doping of modified carbon fiber for high-pressure oil pipe Oil resistant resistant material, and its preparation technology.
Background technology
Polybutadiene rubber has numerous excellent performance characteristics such as high tensile, high-tear strength, high-wearing feature.Buddhist nun Dragon has good combination property, including mechanical property, thermostability, wear resistance, chemical proofing and self lubricity, and rubs Wipe coefficient low, have certain anti-flammability, it is easy to process.
Zhao Yongbing is in its Master's thesis《The research and development of oil-extended butadiene rubber Technology》In, prepare butadiene with it is molten Agent oil（Hydrogasoline；Filling oil：Naphthenic oil）Mixture, be put into water bath with thermostatic control, be heated to 70 DEG C of polymerization temperature, with needle tubing will The catalyst for preparing（Nickel naphthenate and triisobutyl aluminium mixing, ageing；Boron trifluoride etherate and octanal are first by certain Ratio is prepared, and is diluted to 500-1000 times）Be added thereto, stirring makes which fully mix, 2h is stirred after temperature in the kettle is stable It is oil-filled to complete, then oil-extended butadiene rubber glue is dried with mill Jing after vapor cohesion.But exist for high-pressure oil pipe resistance to Corrosivity are not enough.
The present invention with polycaprolactone diols, toluene di-isocyanate(TDI) and dimethythiotoluene diamine as raw material, with stone Ink is filler, is prepared for hydrolysis resistant polyurethane elastomer by prepolymer method, and graphite there occurs intercalation polymeric with polyurethane matrix And favorable dispersibility in the base；The multi-walled carbon nano-tubes being uniformly dispersed, amidine functional group is contained on surface is prepared for, is improved The compatibility between nylon, improves the dispersibility in nylon matrix；
Synthesize high Mooney viscosity basis glue by adjusting catalyst proportion；Carbon fiber after high-temperature oxydation, filled composite material Material, its mechanical property are improved；Obtain a kind of oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping.
The content of the invention
The invention mainly solves the technical problem of providing a kind of oil resistant for high-pressure oil pipe of modified carbon fiber doping Resistant material and its preparation technology, the automobile plastic uptake material made according to the technique have wear-resisting, oil resistant, tear-resistant, resilience The premium properties such as power is good, resistance to chemical attack.
The technical problem to be solved is realized using following technical scheme：
Butadiene（Polymer grade）20-28, naphthenic oil 12-20, nickel naphthenate 3-7, triisobutyl aluminium 4-8, three
Fluorination diethyl etherate 3-7, octanal 2-4, polycaprolactone diols 2-4, graphite 1-2, antioxidant TNP 0.5-1.5, UV absorbent UV-9 0.1-0.3, toluene di-isocyanate(TDI) 1-3, dimethythiotoluene diamine 1-3, multi-walled carbon nano-tubes 1- 2, dimethylformamide 1-2, ethylenediamine 1-2, dodecylbenzene sodium sulfonate 2-4, Silicon chloride. 1-2, dcpd resin 3- 5, nylon 5-8, carbon fiber 5-10, Silane coupling agent KH550 0.05-0.1, Zinc Oxide 0.25-0.5, stearic acid 0.05-0.15, Antioxidant MB 0.05-0.1, SOCl2, tetrahydrofuran, ethanol, appropriate hexamethylene.
A kind of preparation method of the oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping, its feature exist In carrying out according to the following steps：
A. polycaprolactone diols and graphite are mixed into 1-2h, is warmed up to 100-140 DEG C of vacuum dehydration 1-2h, is cooled to After 40-50 DEG C, quick stirring is lower to add antioxidant TNP, UV absorbent UV-9, toluene di-isocyanate(TDI), at 70-90 DEG C Reaction 1-3h, vacuum defoamation 1-2h, are again heated to 80-90 DEG C, add dimethythiotoluene diamine, stir rapidly, will be mixed Compound is placed in 105-115 DEG C, preheating, gel；
B. in multi-walled carbon nano-tubes with 20:1-2 adds SOCl2And dimethylformamide, the constant temperature in 60-90 DEG C of water-bath Heated and stirred 2-4h, is mixed with ethylenediamine, under 130-170 DEG C of oil bath of constant temperature stirs 1-2h, with tetrahydrofuran and washing with alcohol 3-5 time, filter, it is after filter cake is vacuum dried 2-5h at 70-90 DEG C, stand-by；
C. by dodecylbenzene sodium sulfonate, nickel naphthenate, triisobutyl aluminium mixing, in 50-90 DEG C of heated at constant temperature magnetic agitation, After reaction 2-3h, boron trifluoride etherate, octanal, Silicon chloride. is added to carry out coupling 1-2h, with washing with alcohol 3-5 time, Filter, product is air-dried prior in fume hood, then be placed in 50-80 DEG C of vacuum drying oven, it is dried to constant weight；
D. butadiene is mixed with naphthenic oil, adds the cyclohexane solution of dcpd resin, be put into water bath with thermostatic control, heated To 70-90 DEG C of polymerization temperature, the catalyst prepared in c is added thereto with needle tubing, stirring makes which fully mix, temperature stabilization For 60-80 DEG C of stirring, 2-4h is oil-filled completes, then by oil-extended butadiene rubber glue Jing after vapor cohesion, in 110-140 DEG C of cylinder Upper rolling is dry；
E. first carbon fiber is placed in 250-350 DEG C of Muffle furnace is dried and take out after 1-2h, Silane coupling agent KH550 is dissolved in into ethanol In, stir, add the carbon fiber of high temperature modified mistake, after stirring, be put into 60-80 DEG C of stirred in water bath 1-2h, pour into After drying in container, in being put into 60-90 DEG C of baking oven, 3-5h is dried；
F. by resulting material in a, b, d, e and other residual componentss mix homogeneously, add double screw extruder
It is interior, in 230-260 DEG C, 50-120r/min melt blendings, extruding pelletization, that is, obtain a kind of use of modified carbon fiber doping In the oil resistant resistant material of high-pressure oil pipe.
The present invention reaction mechanism and have the beneficial effect that：
（1）With polycaprolactone diols, toluene di-isocyanate(TDI) and dimethythiotoluene diamine as raw material, with graphite to fill out Material, is prepared for hydrolysis resistant polyurethane elastomer by prepolymer method, and graphite there occurs intercalation polymeric and in base with polyurethane matrix Favorable dispersibility in body, composite have the spies such as excellent wear-resisting, oil resistant, the good, resistance to chemical attack of tear-resistant, resilience force Property, so as to extend the service life of oil pipe.
（2）Amination treatment is carried out to multi-walled carbon nano-tubes, the amidine functional group in its surface grafting is prepared for dispersion equal The multi-walled carbon nano-tubes of amidine functional group is contained on even, surface, improves the compatibility between nylon, improves in nylon matrix In dispersibility.
（3）With dodecylbenzene sodium sulfonate, nickel naphthenate, triisobutyl aluminium, boron trifluoride etherate, octanal, four Silicon chloride prepares new catalyst, adjusts catalyst proportion synthesis high Mooney viscosity basis glue；Make the glue production letter of high Mooney basis Easy row, control are flexible, and Mooney viscosity is high, and oil-filled property is good, stable performance.
（4）Nylon has a good combination property, including mechanical property, thermostability, wear resistance, chemical proofing and Self lubricity, and coefficient of friction is low, has certain anti-flammability, it is easy to process；There is polybutadiene rubber high tensile, height to tear Numerous excellent performance characteristics such as resistance to spalling, high-wearing feature.
（5）Carbon fiber has that density is low, higher than performance, fatigue durability is good, good corrosion resistance, electrical and thermal conductivity performance are good etc. is permitted Many premium properties, the carbon fiber after high-temperature oxydation, filled composite materials, its mechanical property are improved.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping, by the original of following weight parts (g) Material is obtained：
Butadiene（Polymer grade）28, naphthenic oil 12-, nickel naphthenate 7, triisobutyl aluminium 4, boron trifluoride second
Ether complexes 3, octanal 4, polycaprolactone diols 2, graphite 2, antioxidant TNP 0.5, UV absorbent UV-9 0.1, Toluene di-isocyanate(TDI) 1, dimethythiotoluene diamine 3, multi-walled carbon nano-tubes 2, dimethylformamide 1, ethylenediamine 2, dodecane Base benzene sulfonic acid sodium salt 4, Silicon chloride. 2, dcpd resin 3, nylon 8, carbon fiber 10, Silane coupling agent KH550 0.1, oxidation Zinc 00.5, stearic acid 0.15, antioxidant MB 0.1, SOCl2, tetrahydrofuran, ethanol, appropriate hexamethylene.
A kind of preparation method of the oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping, its feature exist In carrying out according to the following steps：
A. polycaprolactone diols and graphite are mixed into 1h, is warmed up to 100-110 DEG C of vacuum dehydration 1h, is cooled to 40-50 After DEG C, quick stirring is lower to add antioxidant TNP, UV absorbent UV-9, toluene di-isocyanate(TDI), reacts at 70-80 DEG C 1h, vacuum defoamation 1h, are again heated to 80-90 DEG C, add dimethythiotoluene diamine, stir rapidly, mixture is placed in 105-115 DEG C, preheating, gel；
B. in multi-walled carbon nano-tubes with 20:1 adds SOCl2And dimethylformamide, in 60-70 DEG C of water-bath, constant temperature adds Thermal agitation 2h, is mixed with ethylenediamine, under 160-170 DEG C of oil bath of constant temperature stirs 1h, with tetrahydrofuran and washing with alcohol 3 times, mistake Filter, it is after filter cake is vacuum dried 2h at 80-90 DEG C, stand-by；
C. by dodecylbenzene sodium sulfonate, nickel naphthenate, triisobutyl aluminium mixing, in 70-80 DEG C of heated at constant temperature magnetic agitation, After reaction 2h, add boron trifluoride etherate, octanal, Silicon chloride. to carry out coupling 1h, with washing with alcohol 5 times, filter, will Product is air-dried prior in fume hood, then is placed in 70-80 DEG C of vacuum drying oven, is dried to constant weight；
D. butadiene is mixed with naphthenic oil, adds the cyclohexane solution of dcpd resin, be put into water bath with thermostatic control, heated To 70-80 DEG C of polymerization temperature, the catalyst prepared in c is added thereto with needle tubing, stirring makes which fully mix, temperature stabilization For 60-70 DEG C of stirring, 4h is oil-filled completes, then by oil-extended butadiene rubber glue Jing after vapor cohesion, on 110-120 DEG C of cylinder Rolling is dry；
E. first carbon fiber is placed in 300-320 DEG C of Muffle furnace is dried and take out after 1h, Silane coupling agent KH550 is dissolved in ethanol, Stir, add the carbon fiber of high temperature modified mistake, after stirring, be put into 60-70 DEG C of stirred in water bath 1h, pour in container After drying, in being put into 70-80 DEG C of baking oven, 3h is dried；
F. by resulting material in a, b, d, e and other residual componentss mix homogeneously, add double screw extruder
It is interior, in 240-260 DEG C, 90-120r/min melt blendings, extruding pelletization, that is, obtain a kind of use of modified carbon fiber doping In the oil resistant resistant material of high-pressure oil pipe.
A kind of property of the oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping prepared by above-described embodiment Energy testing result is as follows：
Tensile strength 86MPa, fault growth rate 175%；
Thermal aging test (160 DEG C, 200h)：Tensile strength rate of change 10.2%, elongation at break rate of change 11.5%；
Resistance to mineral oil tests (80 DEG C, 200h)：Tensile strength rate of change 11.6%, elongation at break rate of change 12.4%.

Claims (2)

1. the oil resistant resistant material for high-pressure oil pipe that a kind of modified carbon fiber adulterates, it is characterised in that by following weight The raw material of part is obtained：
Butadiene（Polymer grade）20-28, naphthenic oil 12-20, nickel naphthenate 3-7, triisobutyl aluminium 4-8, three
Fluorination diethyl etherate 3-7, octanal 2-4, polycaprolactone diols 2-4, graphite 1-2, antioxidant TNP 0.5-1.5, UV absorbent UV-9 0.1-0.3, toluene di-isocyanate(TDI) 1-3, dimethythiotoluene diamine 1-3, multi-walled carbon nano-tubes 1- 2, dimethylformamide 1-2, ethylenediamine 1-2, dodecylbenzene sodium sulfonate 2-4, Silicon chloride. 1-2, dcpd resin 3- 5, nylon 5-8, carbon fiber 5-10, Silane coupling agent KH550 0.05-0.1, Zinc Oxide 0.25-0.5, stearic acid 0.05-0.15, Antioxidant MB 0.05-0.1, SOCl2, tetrahydrofuran, ethanol, appropriate hexamethylene.
2. the system of the oil resistant resistant material for high-pressure oil pipe of a kind of modified carbon fiber doping according to claim 1 Preparation Method, it is characterised in that carry out according to the following steps：
A. polycaprolactone diols and graphite are mixed into 1-2h, is warmed up to 100-140 DEG C of vacuum dehydration 1-2h, is cooled to After 40-50 DEG C, quick stirring is lower to add antioxidant TNP, UV absorbent UV-9, toluene di-isocyanate(TDI), at 70-90 DEG C Reaction 1-3h, vacuum defoamation 1-2h, are again heated to 80-90 DEG C, add dimethythiotoluene diamine, stir rapidly, will be mixed Compound is placed in 105-115 DEG C, preheating, gel；
B. in multi-walled carbon nano-tubes with 20:1-2 adds SOCl2And dimethylformamide, in 60-90 DEG C of water-bath, constant temperature adds Thermal agitation 2-4h, is mixed with ethylenediamine, under 130-170 DEG C of oil bath of constant temperature stirs 1-2h, with tetrahydrofuran and washing with alcohol 3-5 It is secondary, filter, it is after filter cake is vacuum dried 2-5h at 70-90 DEG C, stand-by；
C. by dodecylbenzene sodium sulfonate, nickel naphthenate, triisobutyl aluminium mixing, in 50-90 DEG C of heated at constant temperature magnetic agitation, After reaction 2-3h, boron trifluoride etherate, octanal, Silicon chloride. is added to carry out coupling 1-2h, with washing with alcohol 3-5 time, Filter, product is air-dried prior in fume hood, then be placed in 50-80 DEG C of vacuum drying oven, it is dried to constant weight；
D. butadiene is mixed with naphthenic oil, adds the cyclohexane solution of dcpd resin, be put into water bath with thermostatic control, heated To 70-90 DEG C of polymerization temperature, gained catalyst in c is added thereto with needle tubing, stirring makes which fully mix, and temperature stabilization is 2-4h is oil-filled completes for 60-80 DEG C of stirring, then by oil-extended butadiene rubber glue Jing after vapor cohesion, on 110-140 DEG C of cylinder Rolling is dry；
E. first carbon fiber is placed in 250-350 DEG C of Muffle furnace is dried and take out after 1-2h, Silane coupling agent KH550 is dissolved in into ethanol In, stir, add the carbon fiber of high temperature modified mistake, after stirring, be put into 60-80 DEG C of stirred in water bath 1-2h, pour into After drying in container, in being put into 60-90 DEG C of baking oven, 3-5h is dried；
F. by resulting material in a, b, d, e and other residual componentss mix homogeneously, add double screw extruder
It is interior, in 230-260 DEG C, 50-120r/min melt blendings, extruding pelletization, that is, obtain a kind of use of modified carbon fiber doping In the oil resistant resistant material of high-pressure oil pipe.
CN201610913640.0A 2016-10-20 2016-10-20 A kind of oil resistant resistant material for high-pressure oil pipe of modified carbon fiber doping and preparation method thereof Withdrawn CN106543497A (en)

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Application publication date: 20170329