CN105803781B - A kind of lubricant and preparation method for carbon fiber sizing agent - Google Patents

A kind of lubricant and preparation method for carbon fiber sizing agent Download PDF

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CN105803781B
CN105803781B CN201610265465.9A CN201610265465A CN105803781B CN 105803781 B CN105803781 B CN 105803781B CN 201610265465 A CN201610265465 A CN 201610265465A CN 105803781 B CN105803781 B CN 105803781B
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dispersion liquid
tungsten disulfide
polyacrylic acid
acid modified
lubricant
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CN105803781A (en
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叶明新
沈剑锋
李娜
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Fudan University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/22Compounds containing sulfur, selenium or tellurium
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M161/00Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188Monocarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/065Sulfides; Selenides; Tellurides
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/041Siloxanes with specific structure containing aliphatic substituents
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40Fibres of carbon
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/40Reduced friction resistance, lubricant properties; Sizing compositions

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention relates to a kind of lubricant and preparation method for carbon fiber sizing agent, the lubricant includes polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid, dispersant, silicone oil and higher fatty acids;The polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid is dispersion liquid of the nanoscale twins tungsten disulfide dispersion liquid after polyacrylic acid modified;The preparation method first passes through 1) configuration isopropanol water solution, adds the tungsten disulfide that crystallite dimension is less than 100 microns, forms dispersion liquid;2) after ultrasound, standing, centrifugation obtains upper strata dispersion liquid;3) polyacrylic acid modified processing obtains polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid, then mixed according to matching principle with dispersant, silicone oil and higher fatty acids, the lubricant by using polyacrylic acid modified preparation nanoscale twins tungsten disulfide dispersion liquid, it can be used for preparing the sizing agent with specific use, part optimization fiber and its composite material interface performance and macro property.

Description

A kind of lubricant and preparation method for carbon fiber sizing agent
Technical field
The present invention relates to technical field of composite materials, more particularly to a kind of lubricant and preparation for carbon fiber sizing agent Method, particularly a kind of polyacrylic acid modified nanoscale twins tungsten disulfide base lubricating agent for carbon fiber sizing agent.
Background technology
Carbon fiber has a series of excellent properties such as high specific strength, high ratio modulus and is widely used, but because of carbon fiber Poor toughness, rub is poor, in production and process, and meeting snag broken end makes opening unclear, is easily produced through mechanical friction The phenomenon such as lousiness and single wire fracture, makes its intensity decreases.In fiber production process, solution can be very good by starching above-mentioned Problem, starching has become a very important link in fiber production process.With carbon fibre composite industry not Disconnected development, also improves constantly to the performance requirement of sizing agent, is gradually evolved into strengthen from simple protection carbon fiber Carbon fibre composite interface binding intensity, improves composite materials property, i.e., from universal sizing agent to functional form starching Agent develops.
Auxiliary agent in sizing agent can be good at improving the stability of sizing agent in use, and lubricant is to help One kind in agent, it is possible to increase the lubricating ability of material, effectively prevents from bonding between fiber, and lubricant common at present has The unstability of composition and the shortcoming of poor compatibility, therefore profit for prepare carbon fiber sizing agent of the research and development with superperformance Lubrication prescription is significant.
The content of the invention
In view of above-mentioned analysis, the present invention is intended to provide a kind of lubricant and preparation method for carbon fiber sizing agent, The lubricant uses polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid, can be effective as on specific use carbon fiber Slurry agent composition is used, hence it is evident that improve the lubrication and processing characteristics of product.
The purpose of the present invention is mainly achieved through the following technical solutions:
The present invention provides a kind of lubricant for carbon fiber sizing agent, including polyacrylic acid modified nanoscale twins curing Tungsten dispersion liquid, dispersant, silicone oil and higher fatty acids;
Wherein described polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid passes through for nanoscale twins tungsten disulfide dispersion liquid Dispersion liquid after polyacrylic acid modified;Wherein described polyacrylic acid modified mode is effectively to shell polyacrylic acid situ-formed graft From nanoscale twins tungsten disulfide surface.
Further, the parts by weight of the polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid are 1-32, described point The parts by weight of powder are 1-5, and the parts by weight of the silicone oil are 60-90, and the parts by weight of the higher fatty acids are 1-3.
Further, the dispersant include Solulan5, Solulan98, Solulan16, Solulan25 and More than one or both of Solulan97.
Further, the silicone oil includes unsubstituted dimethyl silicone polymer or by the alkyl with 2-20 carbon atom Substituted dimethyl silicone polymer;It is described by the alkyl-substituted dimethyl silicone polymer with 2-20 carbon atom at 25 DEG C Viscosity be 2-100mm2/s。
Further, the higher fatty acids includes laurate, myristic acid, lignin with 12-24 carbon atom It is more than one or both of acid, palmitic acid, oleic acid.
Another aspect of the present invention also provides a kind of preparation method of the lubricant for carbon fiber sizing agent, by polyacrylic acid The configuration of modified Nano lamella tungsten disulfide dispersion liquid is formed, the system of the polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid Preparation Method comprises the following steps:
1) mixed liquor of isopropyl alcohol and water is configured, wherein volume ratio of the isopropanol in the mixed liquor is 30%- 70%, the tungsten disulfide that crystallite dimension is less than 100 microns is added, the dispersion liquid that tungsten disulfide concentration is 10mg/mL is formed;
2) by step 1) gained dispersion liquid carry out ultrasound, stand after, centrifugation obtain upper strata dispersion liquid, by sheet curing Tungsten is efficiently peeled off, and then removes bulky grain, unstripped part;
3) by step 2) the polyacrylic acid modified processing of gained dispersion liquid progress:Acrylic acid and ammonium persulfate are added, reaction is obtained Obtain polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid.
Further, above-mentioned preparation method also includes:Weigh a certain amount of polyacrylic acid modified nanoscale twins curing Tungsten dispersion liquid is mixed according to matching principle with dispersant, silicone oil and higher fatty acids at 40-80 DEG C, uses ultrasonic disperse 1-6h.
Further, step 2) ultrasonic power be 100W, sonication treatment time is 1-8h, and time of repose is 4-12h, Centrifugal rotational speed is 2000-6000rpm.
Further, step 3) acrylic acid and ammonium persulfate addition weight ratio be 10:1-200:1, propylene The weight ratio of acid and tungsten disulfide is 5:1-25:1, temperature is 40-80 DEG C, and the reaction time is 4-96h.
Further, step 3) acrylic acid and ammonium persulfate addition weight ratio be 100:1, acrylic acid and two The weight ratio of tungsten sulfide is 10:1, temperature is 60 DEG C, and the reaction time is 48h.
The present invention has the beneficial effect that:
Lubricant of the present invention can be effective as specific use carbon fiber sizing agent composition and use, and can solve the problem that common at present Lubricant composition unstability and the shortcoming of poor compatibility, hence it is evident that improve product lubrication and processing characteristics, it is of the invention Preparation method is simple to operate, and cost is low, in actual applications can be by changing the proportioning of component in lubricant, applied to difference The sizing agent matrix of species, can play a very good protection in the preparation process of carbon fiber, glass fibre etc., while right The mechanical property of composite increases.The lubricant of this functional form can partly optimize fiber and its composite material interface Performance and macro property.
Other features and advantages of the present invention will be illustrated in the following description, also, the partial change from specification Obtain it is clear that or being understood by implementing the present invention.The purpose of the present invention and other advantages can be by the explanations write Specifically noted structure is realized and obtained in book, claims and accompanying drawing.
Brief description of the drawings
Accompanying drawing is only used for showing the purpose of specific embodiment, and is not considered as limitation of the present invention, in whole accompanying drawing In, identical reference symbol represents identical part.
Fig. 1 is the stereoscan photograph of lubricant in embodiment 1;
Fig. 2 is the stereoscan photograph of lubricant in embodiment 3.
Embodiment
The preferred embodiments of the present invention are specifically described below in conjunction with the accompanying drawings, wherein, accompanying drawing constitutes the application part, and It is used for the principle for explaining the present invention together with embodiments of the present invention.
Embodiment 1
The present embodiment provides a kind of polyacrylic acid modified nanoscale twins tungsten disulfide base for carbon fiber sizing agent and lubricated Agent and preparation method, wherein preparation method comprise the following steps:
(1) mixed solution of configuration water and isopropanol, the wherein volume ratio of isopropanol are 30%, add Average crystallite The tungsten disulfide that 50 microns of size, the concentration of tungsten disulfide is 10mg/mL, is mixed to form dispersion liquid;
(2) dispersion liquid obtained step (1) is ultrasonically treated, and ultrasonic power is 100W, and ultrasonic time is 1 hour;Ultrasound After the completion of stand 8 hours;Then centrifugation obtains upper strata dispersion liquid under 4000rpm rotating speeds;
(3) dispersion liquid for obtaining step (2) is modified processing:It is 10 that weight ratio is added at 40 DEG C:1 propylene Acid and ammonium persulfate, the wherein weight ratio of acrylic acid and tungsten disulfide are 10:1, reaction 96h obtains polyacrylic acid modified receive Rice lamella tungsten disulfide dispersion liquid;
(4) at 70 DEG C, above-mentioned 210 grams and 20 grams dispersants of polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid are taken Solulan16,760 grams of viscositys are 5mm2/ s unsubstituted dimethyl silicone polymer and 10 grams have 12-24 carbon atom Laurate ultrasonic disperse 6 hours under 100W ultrasonic powers, obtain lubricant.
Polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid of the lubricant obtained in this example including 21 parts by weight, The dispersant Solulan16 of 2 parts by weight, the unsubstituted dimethyl silicone polymer of 76 parts by weight and 1 parts by weight have a 12-24 The laurate of individual carbon atom.
The stereoscan photograph of the lubricant is as shown in Figure 1.
Embodiment 2
The present embodiment provides a kind of polyacrylic acid modified nanoscale twins tungsten disulfide base for carbon fiber sizing agent and lubricated Agent and preparation method, wherein preparation method comprise the following steps:
(1) mixed solution of configuration water and isopropanol, the wherein volume ratio of isopropanol are 50%, add Average crystallite The tungsten disulfide that 80 microns of size, the concentration of tungsten disulfide is 10mg/mL, is mixed to form dispersion liquid;
(2) dispersion liquid obtained step (1) is ultrasonically treated, and ultrasonic power is 100W, and ultrasonic time is 8 hours;Ultrasound After the completion of stand 4 hours;Then centrifugation obtains upper strata dispersion liquid under 6000rpm rotating speeds;
(3) dispersion liquid for obtaining step (2) is modified processing:It is 80 that weight ratio is added at 80 DEG C:1 propylene Acid and ammonium persulfate, the wherein weight ratio of acrylic acid and tungsten disulfide are 5:1, reaction 48h obtains polyacrylic acid modified receive Rice lamella tungsten disulfide dispersion liquid;
(4) at 60 DEG C, above-mentioned 170 grams and 40 grams dispersants of polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid are taken Solulan25,770 grams of viscositys are 20mm2/ s by the alkyl-substituted dimethyl silicone polymer with 2-20 carbon atom and 20 grams of ultrasonic disperse 4 hours under 100W ultrasonic powers of the myristic acid with 12-24 carbon atom, obtain lubricant.
Polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid of the lubricant obtained in this example including 17 parts by weight, The dispersant Solulan25 of 4 parts by weight, 77 parts by weight by the alkyl-substituted polydimethylsiloxanes with 2-20 carbon atom The myristic acid with 12-24 carbon atom of alkane and 2 parts by weight.
Embodiment 3
The present embodiment provides a kind of polyacrylic acid modified nanoscale twins tungsten disulfide base for carbon fiber sizing agent and lubricated Agent and preparation method, wherein preparation method comprise the following steps:
(1) mixed solution of configuration water and isopropanol, the wherein volume ratio of isopropanol are 70%, add Average crystallite The tungsten disulfide that 50 microns of size, the concentration of tungsten disulfide is 10mg/mL, is mixed to form dispersion liquid;
(2) dispersion liquid obtained step (1) is ultrasonically treated, and ultrasonic power is 100W, and ultrasonic time is 8 hours;Ultrasound After the completion of stand 8 hours;Then centrifugation obtains upper strata dispersion liquid under 2000rpm rotating speeds;
(3) dispersion liquid for obtaining step (2) is modified processing:It is 200 that weight ratio is added at 60 DEG C:The third of 1 The weight ratio of olefin(e) acid and ammonium persulfate, wherein acrylic acid and tungsten disulfide is 20:1, reaction 4h obtains polyacrylic acid modified Nanoscale twins tungsten disulfide dispersion liquid;
(4) at 80 DEG C, above-mentioned 320 grams and 50 grams dispersants of polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid are taken Solulan5,600 grams of viscositys are 50mm2/ s unsubstituted dimethyl silicone polymer and 30 grams have 12-24 carbon atom Palmitic acid ultrasonic disperse 3 hours under 100W ultrasonic powers, obtain lubricant.
Polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid of the lubricant obtained in this example including 32 parts by weight, The dispersant Solulan5 of 5 parts by weight, the unsubstituted dimethyl silicone polymer of 60 parts by weight and 3 parts by weight have a 12-24 The palmitic acid of individual carbon atom.
The stereoscan photograph of the lubricant is as shown in Figure 2.
Embodiment 4
The present embodiment provides a kind of polyacrylic acid modified nanoscale twins tungsten disulfide base for carbon fiber sizing agent and lubricated Agent and preparation method, wherein preparation method comprise the following steps:
(1) mixed solution of configuration water and isopropanol, the wherein volume ratio of isopropanol are 60%, add Average crystallite The tungsten disulfide that 80 microns of size, the concentration of tungsten disulfide is 10mg/mL, is mixed to form dispersion liquid;
(2) dispersion liquid obtained step (1) is ultrasonically treated, and ultrasonic power is 100W, and ultrasonic time is 4 hours;Ultrasound After the completion of stand 12 hours;Then centrifugation obtains upper strata dispersion liquid under 5000rpm rotating speeds;
(3) dispersion liquid for obtaining step (2) is modified processing:It is 200 that weight ratio is added at 80 DEG C:The third of 1 The weight ratio of olefin(e) acid and ammonium persulfate, wherein acrylic acid and tungsten disulfide is 15:1, reaction 4h obtains polyacrylic acid modified Nanoscale twins tungsten disulfide dispersion liquid;
(4) at 50 DEG C, above-mentioned 20 grams and 50 grams dispersants of polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid are taken Solulan97,900 grams of viscositys are 70mm2/ s unsubstituted dimethyl silicone polymer and 30 grams have 12-24 carbon atom Oleic acid ultrasonic disperse 3 hours under 100W ultrasonic powers, obtain lubricant.
The lubricant obtained in this example includes the polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid of 2 parts by weight, 5 The dispersant Solulan97 of parts by weight, the unsubstituted dimethyl silicone polymer of 90 parts by weight and 3 parts by weight have a 12-24 The oleic acid of individual carbon atom.
The fibre abrasion number of times coated using the lubricant in embodiment 1-4 is as shown in table 1, this hair it can be seen from table Bright lubricant adds fiber abrasion resistance after polyacrylic acid modified, with good lubrication.
The fibre abrasion number of times that table 1 is coated using the lubricant in embodiment 1-4
Condition Abrasion resistance Amplitude of variation (%)
Blank (unmodified) 304 -
Embodiment 1 598 97
Embodiment 2 573 88
Embodiment 3 581 91
Embodiment 4 602 98
In summary, the embodiments of the invention provide a kind of polyacrylic acid modified nanoscale twins for carbon fiber sizing agent Tungsten disulfide base softening agent and preparation method, the lubricant can be effective as specific use carbon fiber sizing agent composition and use, It is obviously improved the lubrication and processing characteristics of product.Fiber and its composite material interface performance and macro property can partly be optimized; Preparation method is simple to operate, and cost is low.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in, It should all be included within the scope of the present invention.

Claims (10)

1. a kind of lubricant for carbon fiber sizing agent, it is characterised in that including polyacrylic acid modified nanoscale twins curing Tungsten dispersion liquid, dispersant, silicone oil and higher fatty acids;
Wherein described polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid is nanoscale twins tungsten disulfide dispersion liquid through poly- third The modified dispersion liquid of olefin(e) acid;Wherein described polyacrylic acid modified mode is by ammonium persulfate initiator that polyacrylic acid is in situ It is grafted on the nanoscale twins tungsten disulfide surface being effectively peeled off.
2. it is used for the lubricant of carbon fiber sizing agent according to claim 1, it is characterised in that described polyacrylic acid modified to receive The parts by weight of rice lamella tungsten disulfide dispersion liquid are 1-32, and the parts by weight of the dispersant are 1-5, and the parts by weight of the silicone oil are 60-90, the parts by weight of the higher fatty acids are 1-3.
3. the lubricant according to claim 1 or claim 2 for carbon fiber sizing agent, it is characterised in that the dispersant includes It is more than Solulan5, Solulan98, Solulan16, one or both of Solulan25 and Solulan97.
4. it is used for the lubricant of carbon fiber sizing agent according to claim 1 or 2 is any, it is characterised in that the silicone oil bag Include unsubstituted dimethyl silicone polymer or by the alkyl-substituted dimethyl silicone polymer with 2-20 carbon atom;25℃ When, the viscosity by the alkyl-substituted dimethyl silicone polymer with 2-20 carbon atom is 2-100mm2/s。
5. it is used for the lubricant of carbon fiber sizing agent according to claim 1-2 is any, it is characterised in that the higher aliphatic Acid include one or both of the laurate with 12-24 carbon atom, myristic acid, lignin acid, palmitic acid, oleic acid with On.
6. a kind of preparation method for the lubricant for being used for carbon fiber sizing agent as described in claim 1-5 is any, it is characterised in that Formed by the configuration of polyacrylic acid modified nanoscale twins tungsten disulfide dispersion liquid, the polyacrylic acid modified nanoscale twins tungsten disulfide The preparation method of dispersion liquid comprises the following steps:
1) mixed liquor of isopropyl alcohol and water is configured, wherein volume ratio of the isopropanol in the mixed liquor is 30%-70%, then The tungsten disulfide that crystallite dimension is less than 100 microns is added, the dispersion liquid that tungsten disulfide concentration is 10mg/mL is formed;
2) by step 1) gained dispersion liquid carry out ultrasound, stand after, centrifugation obtain upper strata dispersion liquid;
3) by step 2) the polyacrylic acid modified processing of gained dispersion liquid progress:Acrylic acid and ammonium persulfate are added, reaction is gathered Acrylic acid modified nanoscale twins tungsten disulfide dispersion liquid.
7. preparation method according to claim 6, it is characterised in that also include:Weigh a certain amount of described polyacrylic acid modified Nanoscale twins tungsten disulfide dispersion liquid is mixed according to matching principle with dispersant, silicone oil and higher fatty acids at 40-80 DEG C, is used Ultrasonic disperse 1-6h.
8. preparation method according to claim 6, it is characterised in that step 2) ultrasonic power is 100W, ultrasonically treated Time is 1-8h, and time of repose is 4-12h, and centrifugal rotational speed is 2000-6000rpm.
9. preparation method according to claim 6, it is characterised in that step 3) the addition weight of the acrylic acid and ammonium persulfate It is 10 to measure part ratio:1-200:1, the weight ratio of acrylic acid and tungsten disulfide is 5:1-25:1, temperature is 40-80 DEG C, instead It is 4-96h between seasonable.
10. preparation method according to claim 6, it is characterised in that step 3) addition of the acrylic acid and ammonium persulfate Weight ratio is 100:1, the weight ratio of acrylic acid and tungsten disulfide is 10:1, temperature is 60 DEG C, and the reaction time is 48h。
CN201610265465.9A 2016-04-26 2016-04-26 A kind of lubricant and preparation method for carbon fiber sizing agent Expired - Fee Related CN105803781B (en)

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CN108587729B (en) * 2018-04-13 2022-02-18 李立强 Modified nano tungsten disulfide lubricating oil additive and preparation method thereof
CN113999495B (en) * 2021-11-16 2023-07-07 嘉兴学院 Structural-function-integrated carbon fiber/epoxy composite material and preparation method thereof

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