CN106750663B - A kind of sealing material and preparation method thereof - Google Patents

A kind of sealing material and preparation method thereof Download PDF

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Publication number
CN106750663B
CN106750663B CN201710037765.6A CN201710037765A CN106750663B CN 106750663 B CN106750663 B CN 106750663B CN 201710037765 A CN201710037765 A CN 201710037765A CN 106750663 B CN106750663 B CN 106750663B
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kneaded
rubber
sealing material
present
weight
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CN106750663A (en
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娄秀冬
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Changchun Lantian High And New Technology Sealing Material Co Ltd
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Changchun Lantian High And New Technology Sealing Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C08L9/02Copolymers with acrylonitrile
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/02Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22Component parts, details or accessories; Auxiliary operations
    • B29B7/28Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/30Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58Component parts, details or accessories; Auxiliary operations
    • B29B7/72Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K3/1006Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by the chemical nature of one of its constituents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/06Macromolecular organic compounds, e.g. prepolymers
    • C09K2200/0607Rubber or rubber derivatives
    • C09K2200/0612Butadiene-acrylonitrile rubber

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Thermal Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)

Abstract

The present invention provides a kind of sealing materials, it is made by including following raw material, the rubber of 18~28 parts by weight, the resin of 5~10 parts by weight, the vulcanization aid of 5~9 parts by weight, the anti-aging agent of 3~5 parts by weight, the filler of the fiber of 20~45 parts by weight and 25~40 parts by weight.The present invention also provides a kind of preparation methods of sealing material.The present invention starts with from the proportioning of sealing material, using specific combination of materials, it is auxiliary in the proper ratio, in conjunction with distinctive preparation process, the sealing material with preferable performance is obtained, solvent or water is not required in the sealing material process, and process environmental protection is not involved in the problems, such as solvent discharge, recovery processing and sewerage.

Description

A kind of sealing material and preparation method thereof
Technical field
The invention belongs to sealing material preparing technical fields more particularly to a kind of sealing material and preparation method thereof.
Background technology
Sealing material just refers to bear seam displacement to reach airtight, watertight and the close purpose of oil, and flush mounting, building Etc. material in seams.Sealing material is almost related to all industry and civil field, national defence, chemical industry, coal, oil, Metallurgy, communications and transportation, machine building industry and aerospace etc. have important role.Sealing material is in the form of it It is divided into fluid encapsulation material, four major class of not fluid tight material, dynamic sealing and static seal, including pump sealing, hydraulic packing, method Orchid sealing, equipment sealing, faying face sealing and auxiliary seal etc., can be configured to liquid or paste, apply when in use Between the contact surface of two components, cure or seal in non-drying putty under certain conditions;It can also be processed into Variously-shaped solid or hollow annulus seals between being mounted on the contact surface of two components.The former claims sealing material only to use In static seal position of the two component contact faces without relative motion;The latter claims sealing material to can be not only used for static seal position, and available There is the dynamic sealing position of relative motion in the contact surface of two components.
Sealing material generally have good physical and mechanical property, high resilience, compression set be small, sealing can It leans on, the advantages that easy to process and service life is long.As silicone rubber sealant energy high temperature resistant and low temperature, radiation hardness, vacuum-resistant, without dirt It contaminates, is nontoxic;Polysulfide rubber sealant has excellent resistance to aviation fuel performance, is also exactly high temperature resistant, high pressure resistant and rub resistance Etc., these are all the dominant directions for sealing industry, and the quality of sealing material directly affects the production efficiency of mechanical body equipment, right The service efficiency of equipment has a great impact.
Sealing element material has metal material (aluminium, lead, indium, stainless steel etc.), also there is nonmetallic materials (rubber, plastics, pottery Porcelain, graphite etc.), composite material (such as rubber-asbestos board, aerogel blanket-polyurethane), if common sealing member material include gold Belong to spirotallic gasket, metal ring gasket, graphite reinforced gasket, metal jacketed gasket, Tetrafluoro spacer, non-asbestos gasket, no asbestos pad Piece, rubber sheet gasket, electronic isolation gasket etc., but most commonly used is heat-resistant powder filler material.
In existing production system, the processing technology of usual rubber based elastic sealing material be mainly compressed into a method and It copies and follows the example of two kinds of techniques, process needs to use solvent or water, is related to solvent recovery processing and the problem of sewerage, and with Pay attention to day by day of the whole society for environmental protection, every profession and trade is also carrying out consistent efforts to emission reduction pollution treatment.Thus, The solvent and sewerage generated in these production processes is increasingly becoming relevant enterprise and focuses on one of matter of utmost importance solved.
Therefore, a kind of sealing material and preparation method thereof how is obtained, solvent recovery and sewage are not related in production process Discharge, is handled pollution sources from source, it has also become many production firms widely one of focus of attention in the industry.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of sealing material and preparation method thereof, this hair The sealing material process of bright offer be not required solvent or water, process environmental protection, be not related to solvent discharge, recovery processing and The problem of sewerage, and the sealing material prepared has preferable performance.
The present invention provides a kind of sealing materials, are made by including following raw material:
Preferably, the rubber includes nitrile rubber, isoprene rubber, butadiene-styrene rubber, natural rubber and acrylic rubber In one or more;
The vulcanization aid includes two kinds in Sulfur, peroxide, 2-steryl benzothiazole, zinc oxide and magnesia It is or a variety of;
The resin includes one kind or more in epoxy resin, ABS resin, phenolic resin, polyester resin and polyamide -66 Kind.
Preferably, the anti-aging agent includes tetramethylthiuram disulfide, 2,6-di-tert-butyl p-cresol stabilizer, prevents always One or more in agent 4010, antioxidant 4010NA and anti-aging agent RD;
The fiber is included in poly(p-phenylene terephthalamide), cellulose fibre, carbon fiber, glass fibre and ore deposit fibre It is one or more;
The filler includes barium sulfate, mica, vermiculite, fumed silica, kaolin, precipitated calcium carbonate, barite With the one or more in wollastonite.
The present invention also provides a kind of preparation method of sealing material, by comprising the following steps:
1) after rubber, fiber, resin, vulcanization aid, anti-aging agent, fiber and filler being carried out mixing mixing, mixed Object;
2) mixture that above-mentioned steps obtain is kneaded by mill with after roll-in, obtains semi-finished product;
3) semi-finished product for obtaining above-mentioned steps obtain sealing material after over cure.
Preferably, the rubber is the sheet rubber after mastication;
The temperature of the mastication is 40~50 DEG C;The thickness of the sheet rubber is less than or equal to 5mm;
The fiber passes through the fiber of silane coupling agent processing for surface;
The silane coupling agent includes vinyltriethoxysilane, the vinyltrimethoxysilane, (β-first of vinyl three Oxygroup ethyoxyl) one or more in silane and γ-(2,3- glycidoxy) propyl trimethoxy silicane;
The temperature that the mixing is kneaded is 50~70 DEG C;The time that the mixing is kneaded is 10~15min.
Preferably, the step 1) is specially:
Rubber and resin are put into mixer to be kneaded for the first time, add vulcanization aid and after anti-aging agent is kneaded again, After putting into fiber and filler progress third time mixing, mixture is obtained.
Preferably, the time being kneaded for the first time is 1~1.5min;
The time being kneaded again is 1~1.5min;
The time that the third time is kneaded is 8~12min.
Preferably, the pass that the mill is kneaded is 4~6 times;
The temperature that the mill is kneaded is 40~50 DEG C;
The preliminary roller linear velocity that the mill is kneaded is 23~24mm/min;
The roller gap that the mill is kneaded is 3~4mm.
Preferably, the temperature of the roll-in is 40~60 DEG C;
The roller speed of the roll-in is 23~24mm/min;
The roller gap of the roll-in is the 90%~95% of sealing material thickness.
Preferably, the pressure of the vulcanization is 8~10MPa;
The temperature of the vulcanization is 140~150 DEG C;
The time of the vulcanization is 18~22min.
The present invention provides a kind of sealing materials, are made by including following raw material, the rubber of 18~28 parts by weight, 5~10 The resin of parts by weight, the vulcanization aid of 5~9 parts by weight, the anti-aging agent of 3~5 parts by weight, 20~45 parts by weight fiber and The filler of 25~40 parts by weight.The present invention also provides a kind of preparation methods of sealing material.Compared with prior art, it is of the invention For the problem that in existing heat-resistant powder filler sealing material production process, existing solvent recovery and sewerage, from sealing The proportioning of material is started with, using specific combination of materials, it is auxiliary in the proper ratio, in conjunction with distinctive preparation process, obtain Solvent or water is not required in sealing material with preferable performance, the sealing material process, and process environmental protection is not related to molten The problem of agent discharge, recovery processing and sewerage.
The experimental results showed that sealing material prepared by the present invention, properties can meet or more than corresponding close in the industry The examination criteria of closure material, can be close to corresponding professional standard QC/T684-2013.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still It should be appreciated that these descriptions are intended merely to the feature and advantage further illustrated the present invention rather than to invention claim Limitation.
All raw materials of the present invention, are not particularly limited its source, buying on the market or according to people in the art Known to member prepared by conventional method.
All raw materials of the present invention, are not particularly limited its purity, present invention preferably employs technical pure or sealing material systems The conventional purity that the field of making uses.
The present invention provides a kind of sealing materials, are made by including following raw material:
The rubber is not particularly limited in the present invention, with rubber material well known to those skilled in the art, ability Field technique personnel can make choice and adjust according to practical condition, product quality and requirement, of the present invention Rubber preferably includes the one or more in nitrile rubber, isoprene rubber, butadiene-styrene rubber, natural rubber and acrylic rubber, More preferably nitrile rubber, isoprene rubber, butadiene-styrene rubber, natural rubber or acrylic rubber are most preferably nitrile rubber, day Two or more in T PNR and butadiene-styrene rubber.The addition of rubber of the present invention is 18~28 parts by weight, is preferably 19 ~27 parts by weight, more preferably 20~26 parts by weight are most preferably 22~24 parts by weight.
The resin is not particularly limited in the present invention, with resin material well known to those skilled in the art, ability Field technique personnel can make choice and adjust according to practical condition, product quality and requirement, of the present invention Resin preferably includes the one or more in epoxy resin, ABS resin, phenolic resin, polyester resin and polyamide -66, more excellent Elect epoxy resin, ABS resin, phenolic resin, polyester resin or polyamide -66 as.The addition of resin of the present invention for 5~ 10 parts by weight are preferably 6~9 parts by weight, and more preferably 6.5~8.5 parts by weight are most preferably 7~8 parts by weight.
The vulcanization aid is not particularly limited in the present invention, with vulcanization aid well known to those skilled in the art, Those skilled in the art can make choice and adjust according to practical condition, product quality and requirement, the present invention The vulcanization aid preferably includes two kinds or more in Sulfur, peroxide, 2-steryl benzothiazole, zinc oxide and magnesia Kind, two kinds be more preferably in Sulfur, peroxide, 2-steryl benzothiazole, zinc oxide and magnesia.Sulphur of the present invention Change the addition of auxiliary agent as 5~9 parts by weight, be preferably 5.5~8.5 parts by weight, more preferably 6~8 parts by weight are most preferably 6.5~8.5 parts by weight.
The anti-aging agent is not particularly limited in the present invention, with anti-aging agent well known to those skilled in the art, ability Field technique personnel can make choice and adjust according to practical condition, product quality and requirement, of the present invention Anti-aging agent preferably includes tetramethylthiuram disulfide, 2,6-di-tert-butyl p-cresol stabilizer, antioxidant 4010, anti-aging agent One or more in 4010NA and anti-aging agent RD, more preferably tetramethylthiuram disulfide, 2,6-di-tert-butyl p-cresol Stabilizer, antioxidant 4010, antioxidant 4010NA or anti-aging agent RD.The addition of anti-aging agent of the present invention is 3~5 weight Part, it is preferably 3.3~4.8 parts by weight, more preferably 3.5~4.5 parts by weight are most preferably 3.7~4.3 parts by weight.
The fiber is not particularly limited in the present invention, is with the fine material of sealing material use well known to those skilled in the art Can, those skilled in the art can make choice and adjust, this hair according to practical condition, product quality and requirement The bright fiber preferably includes one in poly(p-phenylene terephthalamide), cellulose fibre, carbon fiber, glass fibre and ore deposit fibre Kind is a variety of, and more preferably poly(p-phenylene terephthalamide), cellulose fibre, carbon fiber, glass fibre or ore deposit are fine.The present invention The addition of the fiber is 20~45 parts by weight, is preferably 25~40 parts by weight, more preferably 28~38 parts by weight, most preferably For 30~35 parts by weight.
The filler is not particularly limited in the present invention, with the filler well known to those skilled in the art for sealing material , those skilled in the art can make choice and adjust according to practical condition, product quality and requirement, this It invents the filler and preferably includes barium sulfate, mica, vermiculite, fumed silica, kaolin, precipitated calcium carbonate, barite With the one or more in wollastonite, more preferably including barium sulfate, mica, vermiculite, fumed silica, kaolin, light Matter calcium carbonate, barite or wollastonite.The addition of filler of the present invention is 25~40 parts by weight, is preferably 27~38 weight Part, more preferably 30~35 parts by weight are most preferably 31~34 parts by weight.
The present invention also provides a kind of preparation methods of sealing material, comprise the following steps:
1) after rubber, fiber, resin, vulcanization aid, anti-aging agent, fiber and filler being carried out mixing mixing, mixed Object;
2) mixture that above-mentioned steps obtain is kneaded by mill with after roll-in, obtains semi-finished product;
3) semi-finished product for obtaining above-mentioned steps obtain sealing material after over cure.
Selection and optimum principle of the present invention to the raw material in above-mentioned preparation method, the choosing with raw material in aforementioned seal material Selecting can be corresponded to optimum principle, and this is no longer going to repeat them.
After rubber, fiber, resin, vulcanization aid, anti-aging agent, fiber and filler are carried out mixing mixing by the present invention first, Obtain mixture.
The present invention ensures the integrality and operability of technique, the rubber is preferably to improve the comprehensive performance of product Sheet rubber after mastication.
The mastication process of rubber in the preparation process is not particularly limited in the present invention, with known to those skilled in the art Rubber mastication step, those skilled in the art can according to practical condition, product quality and requirement into Row selection and adjustment.The design parameter of the mastication is not particularly limited in the present invention, with element well known to those skilled in the art Procedure parameter is refined, those skilled in the art can be selected according to practical condition, product quality and requirement It selects and adjusts, the temperature of mastication of the present invention is preferably 40~50 DEG C, more preferably 41~49 DEG C, more preferably 43~47 DEG C, it is most preferably 44~46 DEG C.
The design parameter of the sheet rubber is not particularly limited in the present invention, before rubber well known to those skilled in the art Parameter that treated, those skilled in the art can carry out according to practical condition, product quality and requirement Selection and adjustment, the thickness of sheet rubber of the present invention are less than or equal to 5mm, more preferably less than or equal to 4.5mm, more preferably less than etc. In 4mm.
The equipment of the mastication is not particularly limited in the present invention, is with conventional equipment well known to those skilled in the art Can, those skilled in the art can make choice and adjust, this hair according to practical condition, product quality and requirement The equipment of the bright mastication is preferably opening rubber mixing machine.
The present invention ensures the integrality and operability of technique, the fiber is preferably to improve the comprehensive performance of product The fiber of silane coupling agent processing is passed through on surface.
The processing procedure of the silane coupling agent is not particularly limited in the present invention, with fibre well known to those skilled in the art The technique of dimension table surface treatment, those skilled in the art can be according to practical condition, product quality and requirements It makes choice and adjusts.The specific choice of the silane coupling agent is not particularly limited in the present invention, with those skilled in the art The well known silane coupling agent for Fiber strength, those skilled in the art can be according to practical condition, productions Quality and requirement make choice and adjust, and silane coupling agent of the present invention preferably includes vinyl triethoxyl silicon Alkane, vinyltrimethoxysilane, ('beta '-methoxy ethyoxyl) silane of vinyl three and γ-(2,3- glycidoxy) propyl three One or more in methoxy silane, more preferably vinyltriethoxysilane, vinyltrimethoxysilane, vinyl Three ('beta '-methoxy ethyoxyl) silane or γ-(2,3- glycidoxy) propyl trimethoxy silicane.
The design parameter that the present invention is kneaded the mixing is not particularly limited, with routine well known to those skilled in the art Mixing be kneaded parameter, those skilled in the art can according to practical condition, product quality and requirement into Row selection and adjustment, the temperature that mixing of the present invention is kneaded is preferably 50~70 DEG C, more preferably 52~68 DEG C, more preferably 55~65 DEG C, be most preferably 57~63 DEG C;The time that mixing of the present invention is kneaded is preferably 10~15min, and more preferably 11 ~14min is most preferably 12~13min.
The equipment that the present invention is kneaded the mixing is not particularly limited, with conventional mixing well known to those skilled in the art Mixing facilities, those skilled in the art can make choice according to practical condition, product quality and requirement And adjustment, the equipment that mixing of the present invention is kneaded is preferably mixer.
The present invention is further ensured that the comprehensive performance of product, pin of the present invention to ensure the integrality and operability of technique Composition to raw material and it is respective the characteristics of, creative improves production technology, it is proposed that in batches, mixing step by step is kneaded Technique, the step 1) are particularly preferred as:
Rubber and resin are put into mixer to be kneaded for the first time, add vulcanization aid and after anti-aging agent is kneaded again, After putting into fiber and filler progress third time mixing, mixture is obtained.
The design parameter being kneaded for the first time is not particularly limited in the present invention, and those skilled in the art can be according to reality The condition of production, product quality and requirement make choice and adjust, and time of the present invention for being kneaded for the first time is preferably 1~ 1.5min, more preferably 1.1~1.4min are most preferably 1.2~1.3min.
The design parameter being kneaded again is not particularly limited in the present invention, and those skilled in the art can be according to reality The condition of production, product quality and requirement make choice and adjust, and time of the present invention for being kneaded again is preferably 1~ 1.5min, more preferably 1.1~1.4min are most preferably 1.2~1.3min.
The design parameter that the present invention is kneaded the third time is not particularly limited, and those skilled in the art can be according to reality The border condition of production, product quality and requirement make choice and adjust, and the time that third time of the present invention is kneaded is preferred It is most preferably 9~11min for 8~12min, more preferably 8.5~11.5min.
Then the mixture that above-mentioned steps obtain is kneaded by mill with after roll-in by the present invention, obtain semi-finished product.
The equipment that the present invention is kneaded the mill is not particularly limited, with conventional mill well known to those skilled in the art Mixing facilities, those skilled in the art can make choice according to practical condition, product quality and requirement And adjustment, the equipment that mill of the present invention is kneaded is preferably open mill.
The design parameter that the present invention is kneaded the mill is not particularly limited, with routine well known to those skilled in the art Mill be kneaded parameter, those skilled in the art can according to practical condition, product quality and requirement into Row selection and adjustment, the temperature that mill of the present invention is kneaded is preferably 40~50 DEG C, more preferably 41~49 DEG C, more preferably 43~47 DEG C, be most preferably 44~46 DEG C;The preliminary roller linear velocity of preliminary roller linear velocity, i.e. open mill that mill of the present invention is kneaded Preferably 23~24mm/min, more preferably 23.2~23.8mm/min are most preferably 23.4~23.6mm/min.Institute of the present invention The roller gap of mill mixing is stated, i.e. the roller gap of open mill is preferably 3~4mm, more preferably 3.2~3.8mm, is most preferably 3.4~3.6mm.
The present invention is to improve the comprehensive performance of product, ensures the integrality and operability of technique, what the mill was kneaded Pass is 4~6 times, more preferably 4~5 times, so as to ensure that mixture can be uniformly dispersed preferably.
The equipment of the roll-in is not particularly limited in the present invention, and those skilled in the art can be according to actual production feelings Condition, product quality and requirement make choice and adjust, and the equipment of roll-in of the present invention is particularly preferably open mill.
The design parameter of the roll-in is not particularly limited in the present invention, with regular roll well known to those skilled in the art Parameter, those skilled in the art can be made choice according to practical condition, product quality and requirement and Adjustment, the temperature of roll-in of the present invention is preferably 40~60 DEG C, more preferably 42~58 DEG C, more preferably 44~56 DEG C, most Preferably 46~54 DEG C.The roller speed of the roller speed of roll-in of the present invention, i.e. open mill is preferably 23~24mm/min, more preferably 23.2~23.8mm/min is most preferably 23.4~23.6mm/min.The roller in the roller gap, i.e. open mill of roll-in of the present invention Gap is preferably sealing material, i.e. the 90%~95% of final product thickness, and more preferably 91%~94%, it is most preferably 92% ~93%.
The semi-finished product that the present invention finally obtains above-mentioned steps obtain sealing material after over cure.
The design parameter of the vulcanization is not particularly limited in the present invention, with vulcanization well known to those skilled in the art Parameter, those skilled in the art can be made choice according to practical condition, product quality and requirement and Adjustment, the temperature of vulcanization of the present invention is preferably 140~150 DEG C, more preferably 141~149 DEG C, more preferably 143~147 DEG C, it is most preferably 144~146 DEG C.The pressure of vulcanization of the present invention is preferably 8~10MPa, more preferable 8.3~9.7MPa, most Preferably 8.6~9.4MPa.
The equipment of the vulcanization is not particularly limited in the present invention, and those skilled in the art can be according to actual production feelings Condition, product quality and requirement make choice and adjust, and the equipment of vulcanization of the present invention is preferably vulcanizing press.
The present invention provides a kind of sealing materials and preparation method thereof.The present invention starts with from the proportioning of sealing material, uses Specific combination of materials, it is auxiliary in the proper ratio, in conjunction with distinctive preparation process, obtained the sealing material with preferable performance Solvent or water is not required in material, the sealing material process, and process environmental protection is not related to solvent discharge, recovery processing and row The problem of sewage.
The experimental results showed that sealing material prepared by the present invention, properties can meet or more than corresponding close in the industry The examination criteria of closure material, can be close to corresponding professional standard QC/T684-2013.
In order to further illustrate the present invention, with reference to embodiments to a kind of sealing material provided by the invention and its preparation Method is described in detail, but it is to be understood that these embodiments are carried out in fact lower based on the technical solution of the present invention It applies, gives detailed embodiment and specific operating process, be simply the feature and advantage further illustrated the present invention, and It is not limiting to the claimed invention, protection scope of the present invention is also not necessarily limited to following embodiments.
Embodiment 1
1st, it is formulated, referring to table 1, table 1 is the composition of raw materials of the embodiment of the present invention 1.
Table 1
2nd, technical process
2.1 materials prepare
(1) drying glue:Summer, when natural gum drying 24 is small, nitrile rubber does not have to drying;Winter, when natural gum drying 68 is small, fourth When nitrile glue drying 30 is small.It is 80 DEG C~100 DEG C to dry hole temperature.
(2) dispensing:By formula and technological requirement, 0~50 gram of material precision weighs for 0.2 gram of balance;50~ The pan scale that 1000 grams of material precision is 5 grams weighs;The platform balance that 1000 grams or more of material precision is 200 grams weighs. Load weighted material is individually placed by following classification.
2.2 mastication
4.5kg nitrile rubber, 2.8kg natural gums are put into mastication in the open mill of roller spacing about 4mm, roller temperature must not exceed 50 DEG C, rubber is pressed into thin slice by squeezing 3 times repeatedly, is cooled to room temperature.
2.3 mixing
1.2min is kneaded for the first time by being added in by the nitrile rubber of mastication, natural gum and phenolic resin in mixer, is added Sulphur, 2-steryl benzothiazole, zinc oxide, magnesia, 2,6-di-tert-butyl p-cresol and 4010NA are kneaded 1.5min, finally Add in poly(p-phenylene terephthalamide), glass fibre, mica, precipitated silica and resin cure auxiliary agent, mica, leech Mixing 10min is carried out in stone, aramid fiber, paper release silicone and wollastonite input mixer.Mixer thermometric instrument displays temperature 50 DEG C~60 DEG C.
2.4 mills are kneaded
Open mill is preheated to 40 DEG C, roller gap is adjusted to 3.5mm, and it is enterprising that the material come out from mixer is placed on open mill Row is fully kneaded 4 times~5 times.Temperature is not permitted more than 50 DEG C in mixing process, and the preliminary roller linear velocity of open mill is 23mm/min.
2.5 making sheet
Open mill is preheated to 50 DEG C, roller gap is adjusted to 0.90mm (the sealing lining backing plate of production 1.0mm), from mixing The thick blanks that open mill comes out are placed on progress roll-in on the open mill of making sheet and go out plate.Temperature is not permitted more than 60 in mixing process DEG C, the preliminary roller linear velocity of open mill is 23mm/min.
2.6 cut-parts
The plate of different size is cut on request.Vulcanization is gone to according to actual conditions or rushes base.
2.7 rush base
Blank is gone out according to the concrete shape of gasket, blank profile uniformly goes out greatly 3~5 millimeters than finished product gasket profile.
2.8 vulcanization
Blank is put on vulcanizing press, vulcanizes 20min under conditions of 148 DEG C of temperature, pressure is 8.5MPa, then Vulcanizer is opened, the plate after vulcanization is taken out, obtains sealing material.
The sealing material prepared to the embodiment of the present invention 1 is detected.Referring to table 2, table 2 is prepared for the embodiment of the present invention 1 Sealing material detection data and in the industry corresponding sealing material examination criteria comparison.
Table 2
With reference to People's Republic of China (PRC) automobile industry standard QC/T684-2013《Motorcycle and light motorcycle engine are used Gasket seal technical conditions》" physical performance index of filled rubber gasket " refers to the physical property of this product as defined in middle table 7 Mark project and technology requirement are close.Product provided by the present invention has reached the requirement of professional standard.
Embodiment 2
1st, it is formulated, referring to table 3, table 3 is the composition of raw materials of the embodiment of the present invention 2.
Table 3
Sequence number Raw material title Weight (Kg) Percentage (%)
1 Nitrile rubber 4.5 15
2 Natural rubber 2.8 7
3 Phenolic resin 2.4 6
4 Sulphur 0.45 1.5
5 2-steryl benzothiazole 0.45 1.5
6 Zinc oxide 1.6 4
7 Magnesia 0.4 1
8 2,6-di-tert-butyl p-cresol 0.8 2
9 4010NA 0.8 2
10 Poly(p-phenylene terephthalamide) 2 5
11 Glass fibre 8 20
12 Mica 8 20
13 Precipitated silica 2 5
14 Wollastonite 4 10
It is total 40 100
2nd, technical process
2.1 materials prepare
(1) drying glue:Summer, when natural gum drying 24 is small, nitrile rubber does not have to drying;Winter, when natural gum drying 68 is small, fourth When nitrile glue drying 30 is small.It is 80 DEG C~100 DEG C to dry hole temperature.
(2) dispensing:By formula and technological requirement, 0~50 gram of material precision weighs for 0.2 gram of balance;50~ The pan scale that 1000 grams of material precision is 5 grams weighs;The platform balance that 1000 grams or more of material precision is 200 grams weighs. Load weighted material is individually placed by following classification.
2.2 mastication
4.5kg nitrile rubber, 2.8kg natural gums are put into mastication in the open mill of roller spacing about 4mm, roller temperature must not exceed 50 DEG C, rubber is pressed into thin slice by squeezing 3 times repeatedly, is cooled to room temperature.
2.3 mixing
1.3min is kneaded for the first time by being added in by the nitrile rubber of mastication, natural gum and phenolic resin in mixer, is added Sulphur, 2-steryl benzothiazole, zinc oxide, magnesia, 2,6-di-tert-butyl p-cresol and 4010NA are kneaded 1.3min, finally Add in poly(p-phenylene terephthalamide), glass fibre, mica, precipitated silica and resin cure auxiliary agent, mica, leech Mixing 10.5min is carried out in stone, aramid fiber, paper release silicone and wollastonite input mixer.Mixer thermometric instrument display temperature 50 DEG C~60 DEG C of degree.
2.4 mills are kneaded
Open mill is preheated to 40 DEG C, roller gap is adjusted to 3.5mm, and it is enterprising that the material come out from mixer is placed on open mill Row is fully kneaded 4 times~5 times.Temperature is not permitted more than 50 DEG C in mixing process, and the preliminary roller linear velocity of open mill is 23mm/min.
2.5 making sheet
Open mill is preheated to 50 DEG C, roller gap is adjusted to 0.90mm (the sealing lining backing plate of production 1.0mm), from mixing The thick blanks that open mill comes out are placed on progress roll-in on the open mill of making sheet and go out plate.Temperature is not permitted more than 60 in mixing process DEG C, the preliminary roller linear velocity of open mill is 23mm/min.
2.6 cut-parts
The plate of different size is cut on request.Vulcanization is gone to according to actual conditions or rushes base.
2.7 rush base
Blank is gone out according to the concrete shape of gasket, blank profile uniformly goes out greatly 3~5 millimeters than finished product gasket profile.
2.8 vulcanization
Blank is put on vulcanizing press, vulcanizes 20min under conditions of 145 DEG C of temperature, pressure is 8.5MPa, then Vulcanizer is opened, the plate after vulcanization is taken out, obtains gasket seal.
The gasket seal prepared to the embodiment of the present invention 2 is detected.Referring to table 4, table 4 is prepared for the embodiment of the present invention 2 Gasket seal detection data and in the industry corresponding sealing material examination criteria comparison.
Table 4
With reference to People's Republic of China (PRC) automobile industry standard QC/T684-2013《Motorcycle and light motorcycle engine are used Gasket seal technical conditions》" physical performance index of filled rubber gasket " refers to the physical property of this product as defined in middle table 7 Mark project and technology requirement are close.Product provided by the present invention has reached the requirement of professional standard.
Embodiment 3
1st, it is formulated, referring to table 5, table 5 is the composition of raw materials of the embodiment of the present invention 3.
Table 5
2nd, technical process
2.1 materials prepare
(1) drying glue:Summer, when natural gum drying 24 is small, nitrile rubber does not have to drying;Winter, when natural gum drying 68 is small, fourth When nitrile glue drying 30 is small.It is 80 DEG C~100 DEG C to dry hole temperature.
(2) dispensing:By formula and technological requirement, 0~50 gram of material precision weighs for 0.2 gram of balance;50~ The pan scale that 1000 grams of material precision is 5 grams weighs;The platform balance that 1000 grams or more of material precision is 200 grams weighs. Load weighted material is individually placed by following classification.
2.2 mastication
4.5kg nitrile rubber, 2.8kg natural gums are put into mastication in the open mill of roller spacing about 3.8mm, roller temperature must not exceed 50 DEG C, rubber is pressed into thin slice by squeezing 3 times repeatedly, is cooled to room temperature.
2.3 mixing
1.2min is kneaded for the first time by being added in by the nitrile rubber of mastication, natural gum and epoxy resin in mixer, is added Sulphur, 2-steryl benzothiazole, zinc oxide, magnesia, 2,6-di-tert-butyl p-cresol and 4010NA are kneaded 1.2min, finally Add in poly(p-phenylene terephthalamide), glass fibre, mica, precipitated silica and resin cure auxiliary agent, mica, leech Mixing 11min is carried out in stone, aramid fiber, paper release silicone and wollastonite input mixer.Mixer thermometric instrument displays temperature 50 DEG C~60 DEG C.
2.4 mills are kneaded
Open mill is preheated to 40 DEG C, roller gap is adjusted to 3.5mm, and it is enterprising that the material come out from mixer is placed on open mill Row is fully kneaded 4 times~5 times.Temperature is not permitted more than 50 DEG C in mixing process, and the preliminary roller linear velocity of open mill is 23mm/min.
2.5 making sheet
Open mill is preheated to 50 DEG C, roller gap is adjusted to 0.90mm (the sealing lining backing plate of production 1.0mm), from mixing The thick blanks that open mill comes out are placed on progress roll-in on the open mill of making sheet and go out plate.Temperature is not permitted more than 60 in mixing process DEG C, the preliminary roller linear velocity of open mill is 23mm/min.
2.6 cut-parts
The plate of different size is cut on request.Vulcanization is gone to according to actual conditions or rushes base.
2.7 rush base
Blank is gone out according to the concrete shape of gasket, blank profile uniformly goes out greatly 3~5 millimeters than finished product gasket profile.
2.8 vulcanization
Blank is put on vulcanizing press, vulcanizes 20min under conditions of 146 DEG C of temperature, pressure is 8.5MPa, then Vulcanizer is opened, takes out the plate after vulcanization, the plate after vulcanization is taken out, obtains sealing material.
The sealing material prepared to the embodiment of the present invention 3 is detected.Referring to table 6, table 6 is prepared for the embodiment of the present invention 3 Sealing material detection data and in the industry corresponding sealing material examination criteria comparison.
Table 6
With reference to People's Republic of China (PRC) automobile industry standard QC/T684-2013《Motorcycle and light motorcycle engine are used Gasket seal technical conditions》" physical performance index of filled rubber gasket " refers to the physical property of this product as defined in middle table 7 Mark project and technology requirement are close.Product provided by the present invention has reached the requirement of professional standard.
A kind of gasket seal provided by the invention and preparation method thereof is described in detail above, it is used herein Specific case is set forth the principle of the present invention and embodiment, to understand the explanation of above example is only intended to helping The method and its core concept of the present invention, including best mode, and but also any person skilled in the art can be real The present invention is trampled, including manufacturing and using any device or system and the method for any combination of implementation.It should be pointed out that for this skill For the those of ordinary skill in art field, without departing from the principle of the present invention, several change can also be carried out to the present invention Into and modification, these improvement and modification are also fallen into the protection domain of the claims in the present invention.The scope of patent protection of the present invention Be defined by the claims, and may include those skilled in the art it is conceivable that other embodiment.If these other realities Example is applied with the structural element for being not different from claim character express or if they include the word with claim State the equivalent structural elements without essence difference, then these other embodiments should also be included in the range of claim.

Claims (10)

1. a kind of sealing material, which is characterized in that be made by including following raw material:
18 ~ 28 parts by weight of rubber;
5 ~ 10 parts by weight of resin;
5 ~ 9 parts by weight of vulcanization aid;
3 ~ 5 parts by weight of anti-aging agent;
20 ~ 45 parts by weight of fiber;
25 ~ 40 parts by weight of filler;
Without solvent or water in process.
2. sealing material according to claim 1, which is characterized in that the rubber includes nitrile rubber, isoprene rubber, fourth One or more in benzene rubber, natural rubber and acrylic rubber;
The vulcanization aid includes two kinds or more in Sulfur, peroxide, 2-steryl benzothiazole, zinc oxide and magnesia Kind;
The resin includes the one or more in epoxy resin, ABS resin, phenolic resin, polyester resin and polyamide -66.
3. sealing material according to claim 1, which is characterized in that it is blue that the anti-aging agent includes the tetramethyl autumn One or more in nurse, 2,6-di-tert-butyl p-cresol stabilizer, antioxidant 4010, antioxidant 4010NA and anti-aging agent RD;
The fiber includes one kind in poly(p-phenylene terephthalamide), cellulose fibre, carbon fiber, glass fibre and ore deposit fibre It is or a variety of;
The filler includes barium sulfate, mica, vermiculite, fumed silica, kaolin, precipitated calcium carbonate, barite and silicon One or more in lime stone.
4. a kind of preparation method of sealing material, which is characterized in that by comprising the following steps:
1)After rubber, resin, vulcanization aid, anti-aging agent, fiber and filler are carried out mixing mixing, mixture is obtained;
2)The mixture that above-mentioned steps obtain is kneaded by mill with after roll-in, obtains semi-finished product;
3)The semi-finished product that above-mentioned steps are obtained obtain sealing material after over cure.
5. preparation method according to claim 4, which is characterized in that the rubber is the sheet rubber after mastication;
The temperature of the mastication is 40 ~ 50 DEG C;The thickness of the sheet rubber is less than or equal to 5mm;
The fiber passes through the fiber of silane coupling agent processing for surface;
The silane coupling agent includes vinyltriethoxysilane, vinyltrimethoxysilane, vinyl three('beta '-methoxy Ethyoxyl)Silane and γ-(2,3- glycidoxies)One or more in propyl trimethoxy silicane;
The temperature that the mixing is kneaded is 50 ~ 70 DEG C;The time that the mixing is kneaded is 10 ~ 15min.
6. preparation method according to claim 4, which is characterized in that the step 1)Specially:
Rubber and resin are put into mixer to be kneaded for the first time, add vulcanization aid and after anti-aging agent is kneaded again, input After fiber and filler carry out third time mixing, mixture is obtained.
7. preparation method according to claim 6, which is characterized in that the time being kneaded for the first time is 1 ~ 1.5min;
The time being kneaded again is 1 ~ 1.5min;
The time that the third time is kneaded is 8 ~ 12min.
8. preparation method according to claim 4, which is characterized in that the pass that the mill is kneaded is 4 ~ 6 times;
The temperature that the mill is kneaded is 40 ~ 50 DEG C;
The preliminary roller linear velocity that the mill is kneaded is 23 ~ 24mm/min;
The roller gap that the mill is kneaded is 3 ~ 4mm.
9. preparation method according to claim 4, which is characterized in that the temperature of the roll-in is 40 ~ 60 DEG C;
The roller speed of the roll-in is 23 ~ 24mm/min;
The roller gap of the roll-in is the 90% ~ 95% of sealing material thickness.
10. according to the preparation method described in claim 4 ~ 9 any one, which is characterized in that the pressure of the vulcanization for 8 ~ 10MPa;
The temperature of the vulcanization is 140 ~ 150 DEG C;
The time of the vulcanization is 18 ~ 22min.
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CN108164773A (en) * 2017-12-20 2018-06-15 合肥市易远新材料有限公司 A kind of preparation method of the capacitor rubber of resistance to hot-seal
CN108178894A (en) * 2017-12-20 2018-06-19 合肥市易远新材料有限公司 A kind of High-temperature-rescapacitor capacitor seals rubber
CN109233115B (en) * 2018-08-29 2021-07-06 三斯达(江苏)环保科技有限公司 Rubber composition with high wear resistance, preparation method and application thereof
CN108929470B (en) * 2018-08-29 2020-12-11 三斯达(江苏)环保科技有限公司 Anti-aging rubber composition and preparation method thereof
CN109438782A (en) * 2018-11-01 2019-03-08 宁国华祥汽车零部件有限公司 A kind of preparation method for the piston seal rubber that ageing-resistant effect is good
CN109897241B (en) * 2019-03-12 2021-03-12 青岛科技大学 Rubber material for gas pressure regulator and preparation process of rubber
CN109897243A (en) * 2019-04-08 2019-06-18 中国农业大学 A kind of composite material suitable for doing harvest corn machine cylinder spike-tooth
CN113527774A (en) * 2020-04-16 2021-10-22 上海弗兆实业有限公司 Processing technology of rubber sealing ring
CN115650632B (en) * 2022-10-26 2023-10-31 河北慈宏新材料科技有限公司 High-resistance Wen Zhidan-based composite sealing gasket and preparation method thereof

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