CN106700154B - A kind of graphite sealing material and preparation method thereof - Google Patents
A kind of graphite sealing material and preparation method thereof Download PDFInfo
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- CN106700154B CN106700154B CN201710037377.8A CN201710037377A CN106700154B CN 106700154 B CN106700154 B CN 106700154B CN 201710037377 A CN201710037377 A CN 201710037377A CN 106700154 B CN106700154 B CN 106700154B
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- 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
- C08L9/02—Copolymers with acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L15/00—Compositions of rubber derivatives
- C08L15/005—Hydrogenated nitrile rubber
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2003/1034—Materials or components characterised by specific properties
- C09K2003/1078—Fire-resistant, heat-resistant materials
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Abstract
The present invention provides a kind of graphite sealing materials, by including that following raw material is made, the graphite of 30~50 parts by weight, the rubber of 14~75 parts by weight, the non-asbestos fiber of 10~100 parts by weight, 5~20 parts by weight filler and rubber chemicals；The dosage of the rubber chemicals is the 4%~23% of rubber consumption.Graphite sealing material provided by the invention is a kind of graphite sealing material of non-asbestos, without containing asbestos component, the prominent characteristic that rear high temperature resistant grade improves is combined using graphite and rubber, it is aided with the graphite and rubber of special ratios, again plus other of specific combination and ratio auxiliary agent, the resistance to ability of high temperature resistance of sealing material is effectively raised, lift-off seal material ensures that sealing is permanently effective in the useful life longevity of worst hot case environment.
Description
Technical field
The invention belongs to sealing material preparing technical fields more particularly to a kind of graphite sealing material and preparation method thereof.
Background technology
Sealing material refers to just that can bear seam displacement to reach airtight, watertight purpose, and seams such as flush mounting, building
In material.Sealing material is almost related to all industry and civil field, in national defence, chemical industry, coal, oil, metallurgy, friendship
Logical transport, machine building industry and aerospace etc. have important role.Sealing material is divided into stream in the form of it
Body sealing material, four major class of not fluid tight material, dynamic sealing and static seal, including pump close with sealing, hydraulic packing, flange
Envelope, equipment sealing, faying face sealing and auxiliary seal etc., can be configured to liquid or paste, be coated in two when in use
Between the contact surface of component, cures under certain conditions or seal in non-drying putty；It can also be processed into various
The solid or hollow annulus of shape seals between being mounted on the contact surface of two components.The former claims sealing material to be served only for two
Static seal position of the component contact face without relative motion；The latter claims sealing material to can be not only used for static seal position, and can be used for two
The contact surface of component has the dynamic sealing position of relative motion.
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 pad, metal jacketed gasket, Tetrafluoro spacer, non-asbestos gasket, no asbestos washer, rubber
Glue gasket, electronic isolation gasket etc..Among these, the sealing material of asbestos component is widely answered since high-temperature resistance is strong
(such as mechanical equipment：Automobile engine, motorcycle start, general purpose engine, air presses, refrigeration compressor, tube method
Orchid, valve etc.) connecting portion sealing.
But in recent years, it is influenced by environmental protection condition, the use of such gasket material gradually receives more and more limits
System.And relatively environment-friendly non-asbestos gasket, it is in use, pre- in lasting or intermittent high temperatures, meson pressure, meson burn into
Under the action of tight stress, the high-temperature resistance of gasket reduces, and causes meson to leak, seal failure.
Therefore, a kind of non-asbestos seal material with better high-temperature resistance how is found, it has also become many in the industry
One of production firm's urgent problem to be solved.
Invention content
In view of this, the technical problem to be solved in the present invention is to provide a kind of graphite sealing material and preparation method thereof,
Graphite sealing material provided by the invention does not contain asbestos component, and has preferable high temperature resistant property.
The present invention provides a kind of graphite sealing materials, by including that following raw material is made：
Preferably, the rubber includes nitrile rubber, natural rubber, butadiene-styrene rubber, neoprene and hydrogenated nitrile-butadiene rubber
In it is one or more；
The graphite includes graphite powder；
The non-asbestos fiber includes non-asbestos organic fiber and/or non-asbestos inorfil；
The filler includes reinforced filling；
The rubber chemicals include one or more in vulcanizing agent, accelerating agent, activating agent, anti-aging agent and plasticizer.
Preferably, the rubber includes the nitrile rubber of 5~30 parts by weight, the natural rubber of 4~20 parts by weight and 5~20
The butadiene-styrene rubber of parts by weight；
The granularity of the graphite powder is 45~550 μm；
The non-asbestos fiber includes that Fanglun slurry cake and artificial mine are fine；
The filler includes one or more in kaolin, carbon black and white carbon；
The rubber chemicals include the vulcanizing agent for accounting for the rubber consumption 1%~5%, account for the rubber consumption 1%~5%
Accelerating agent, account for the activating agent of the rubber consumption 1%~8% and account for the anti-aging agent of the rubber consumption 1%~5%.
The present invention also provides a kind of preparation methods of graphite sealing material, include the following steps：
1) after being mixed fiber, rubber, rubber chemicals, non-asbestos fiber and filler, masterbatch is obtained；
2) masterbatch for obtaining above-mentioned steps obtains sealing material after roll-in and vulcanization.
Preferably, the non-asbestos fiber includes non-asbestos organic fiber and non-asbestos inorfil；
The step 1) is specially：
11) after non-asbestos organic fiber and graphite being carried out shredding stirring, just mixed object is obtained；
12) first mixed object, rubber, rubber chemicals and solvent that above-mentioned steps obtain are disperseed, add non-asbestos without
After machine fiber disperses again, cooling obtains mixture；
13) it in the mixture obtained to above-mentioned steps, after filler mixing is added, adds after interleaving agent mixes again, obtains
To master batch.
Preferably, the rubber is the sheet rubber after breaking glue and mastication；
The temperature of the mastication is 40~50 DEG C；
The pass of the mastication is 1~3 time；
The solvent includes one kind in gasoline, toluene, dimethylbenzene, acetone, heptane, methyl ethyl ketone, ethyl acetate and butanone
Or it is a variety of；
The interleaving agent includes ethyl alcohol.
Preferably, the time of the shredding stirring is 5~20min；
The time of the dispersion is 50~180min；
The time of the dispersion is 20~60min；
The time of the cooling is 1~30min；
The time of the mixing is 5~60min；
The time mixed again is 5~60s.
Preferably, further include baking step before the vulcanization；
The temperature of the drying is 60~100 DEG C；
The time of the drying is 4~10h.
Preferably, the pressure of the vulcanization is 10~16MPa；
The temperature of the vulcanization is 143~155 DEG C；
The time of the vulcanization is 6~20min.
Preferably, the temperature of the roll-in is 80~200 DEG C；
The line pressure of the roll-in is 4~16t；
The steam pressure of the roll-in is 0.1~0.5MPa.
The present invention provides a kind of graphite sealing materials, by including that following raw material is made, the graphite of 30~50 parts by weight,
The filler and rubber chemicals of the rubber of 14~75 parts by weight, the non-asbestos fiber of 10~100 parts by weight, 5~20 parts by weight；Institute
The dosage for stating rubber chemicals is the 4%~23% of rubber consumption.Compared with prior art, the present invention is directed to existing non-asbestos pad
Piece, in use, under conditions of continuing or intermittent high temperatures, meson pressure, meson corrosion and the effect of pre-tight stress
Under, the high-temperature resistance of gasket reduces, and causes meson to leak, the defect of seal failure.The present invention provides a kind of graphite grazings
Material, is a kind of graphite sealing material of non-asbestos, and graphite sealing material provided by the invention does not contain asbestos component, utilizes stone
Ink and rubber combine the prominent characteristic that rear high temperature resistant grade improves, and are aided with the graphite and rubber of special ratios, then add specific combination
With other auxiliary agents of ratio, the resistance to ability of high temperature resistance of sealing material is effectively raised, lift-off seal material is in worst hot case ring
The useful life longevity in border ensures that sealing is permanently effective.
The experimental results showed that the graphite sealing material without containing asbestos component prepared by the present invention, temperature in use reach
260~300 DEG C, compare the temperature in use of 180~250 DEG C of common non-asbestos gasket, improve 20%~44%, and with compared with
Good room temperature and elevated-temperature seal performance, can meet or exceed relevant standard.
Specific implementation mode
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
It is prepared by conventional method known to member.
All raw materials of the present invention, are not particularly limited its purity, and present invention preferably employs technical pure or superhard material works
The conventional purity that tool manufacture and hard brittle material manufacture field use.
The present invention provides a kind of graphite sealing materials, by including that following raw material is made：
The graphite is not particularly limited in the present invention, with graphite material well known to those skilled in the art, ability
Field technique personnel can select and adjust according to practical condition, product quality and requirement, of the present invention
Graphite is preferably amorphous graphite and/or crystalline flake graphite, more preferably amorphous graphite (amorphous graphite powder) or crystalline flake graphite.This
The granularity of the graphite is not particularly limited in invention, with the granularity of graphite powder well known to those skilled in the art, ability
Field technique personnel can select and adjust according to practical condition, product quality and requirement, of the present invention
The granularity of graphite is preferably 45~550 μm, more preferably 100~450 μm, most preferably 200~350 μm.Specifically, of the invention
When the graphite is preferably amorphous graphite, the granularity of the amorphous graphite is preferably 45~75 μm, i.e. the mesh of 325 mesh~200,
More preferably 50~70 μm, most preferably 55~65 μm.When graphite of the present invention is preferably crystalline flake graphite, the crystalline flake graphite
Granularity be preferably 120~550 μm, i.e. the mesh of 120 mesh~30, more preferably 220~450 μm, most preferably 320~350 μm.This
Invent the graphite addition be 30~50 parts by weight, preferably 32~48 parts by weight, more preferably 34~46 parts by weight, most
Preferably 36~44 parts by weight.
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 select and adjust according to practical condition, product quality and requirement, of the present invention
Rubber preferably include it is one or more in nitrile rubber, natural rubber, butadiene-styrene rubber, neoprene and hydrogenated nitrile-butadiene rubber,
Two or more more preferably in nitrile rubber, natural rubber, butadiene-styrene rubber, neoprene and hydrogenated nitrile-butadiene rubber, it is optimal
It is selected as nitrile rubber, natural rubber and butadiene-styrene rubber.Nitrile rubber of the present invention includes powder nitrile rubber.
The addition of rubber of the present invention be 14~75 parts by weight, preferably 24~65 parts by weight, more preferably 34~
55 parts by weight, most preferably 40~50 parts by weight.Specific choice and its corresponding addition of the present invention to the rubber material
It is not particularly limited, with conventional selection well known to those skilled in the art and addition, those skilled in the art can root
It is selected and is adjusted according to practical condition, product quality and requirement, the addition of nitrile rubber of the present invention
Preferably 5~30 parts by weight, more preferably 10~25 parts by weight, most preferably 15~20 parts by weight；Natural rubber of the present invention
The addition of glue is preferably 4~20 parts by weight, more preferably 6~18 parts by weight, most preferably 10~24 parts by weight；Institute of the present invention
The addition for stating butadiene-styrene rubber is preferably 5~20 parts by weight, more preferably 8~17 parts by weight, most preferably 11~14 parts by weight.
The non-asbestos fiber is not particularly limited in the present invention, with the non-stone of threadiness well known to those skilled in the art
Cotton material, those skilled in the art can be selected according to practical condition, product quality and requirement and
Adjustment, non-asbestos fiber of the present invention preferably includes non-asbestos organic fiber and/or non-asbestos inorfil, more preferably non-
Asbestos organic fiber and non-asbestos inorfil.The present invention does not limit the specific choice of the non-asbestos organic fiber especially
System, with non-asbestos organic fiber well known to those skilled in the art, those skilled in the art can be according to actual production feelings
Condition, product quality and requirement are selected and are adjusted, and non-asbestos organic fiber of the present invention is preferably non-asbestos
The artificial enhancing organic fiber of type, more preferably Fanglun slurry cake.The present invention does not have the specific choice of the non-asbestos inorfil
There is special limitation, with non-asbestos inorfil well known to those skilled in the art, those skilled in the art can be according to reality
The border condition of production, product quality and requirement are selected and are adjusted, and non-asbestos inorfil of the present invention is preferably
Non-asbestos type is manually sintered the artificial inorganic reinforcing fiber of manufacture, and more preferably artificial mine is fine.
The addition of non-asbestos fiber of the present invention be 10~100 parts by weight, preferably 20~90 parts by weight, more preferably
For 30~80 parts by weight, most preferably 50~60 parts by weight.The present invention is to the specific choice of the non-asbestos fiber and its corresponding
Addition be not particularly limited, with conventional selection well known to those skilled in the art and addition, people in the art
Member can be selected and adjusted according to practical condition, product quality and requirement, and non-asbestos of the present invention has
The addition of machine fiber is preferably 10~40 parts by weight, more preferably 15~35 parts by weight, most preferably 20~30 parts by weight；This
The addition for inventing the non-asbestos inorfil is preferably 10~60 parts by weight, more preferably 20~50 parts by weight, most preferably
For 30~40 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 select and adjust according to practical condition, product quality and requirement, this
Invent the filler and preferably include reinforced filling, more specifically preferably include it is one or more in kaolin, carbon black and white carbon,
More preferably kaolin, carbon black or white carbon.The addition of filler of the present invention is 5~20 parts by weight, preferably 7~18 weights
Measure part, more preferably 9~16 parts by weight, most preferably 11~14 parts by weight.
The rubber chemicals are not particularly limited in the present invention, with well known to those skilled in the art for rubber material
Rubber chemicals, those skilled in the art can select according to practical condition, product quality and requirement
And adjustment, rubber chemicals of the present invention preferably include one kind in vulcanizing agent, accelerating agent, activating agent, anti-aging agent and plasticizer
Or it is a variety of, it is more preferably one or more in vulcanizing agent, accelerating agent, activating agent, anti-aging agent and plasticizer, most preferably vulcanize
Agent, accelerating agent, activating agent, anti-aging agent or plasticizer.The addition of filler of the present invention is the 4%~23% of rubber consumption,
Preferably 7%~20%, more preferably 10%~17%, most preferably 12%~15%.
The specific choice of the rubber chemicals and its corresponding addition is not particularly limited in the present invention, with this field skill
Conventional selection and addition known to art personnel, those skilled in the art can be according to practical condition, product qualities
And requirement is selected and is adjusted, and the addition of vulcanizing agent of the present invention is preferably 1%~5%, and more preferably 2%
~4%, most preferably 2.5%~3.5%；The addition of accelerating agent of the present invention is preferably 1%~5%, and more preferably 2%
~4%, most preferably 2.5%~3.5%；The addition of activating agent of the present invention is preferably 1%~8%, and more preferably 2%
~7%, more preferably 3%~6%, most preferably 4%~5%；The addition of anti-aging agent of the present invention is preferably 1%~
5%, more preferably 2%~4%, most preferably 2.5%~3.5%.
The present invention also provides a kind of preparation methods of graphite sealing material, include the following steps：
1) after being mixed fiber, rubber, rubber chemicals, non-asbestos fiber and filler, masterbatch is obtained；
2) masterbatch for obtaining above-mentioned steps obtains sealing material after roll-in and vulcanization.
Selection and optimum principle of the present invention to the raw material in above-mentioned preparation method, with raw material in foregoing graphites sealing material
Selection and optimum principle can be corresponded to, this is no longer going to repeat them.
The pretreatment process of rubber in the preparation process is not particularly limited in the present invention, ripe with those skilled in the art
The rubber pre-treatment step known, those skilled in the art can want according to practical condition, product quality and use
It asks and is selected and adjusted, rubber of the present invention is preferably the sheet rubber after breaking glue and mastication.
The detailed process and parameter of the broken glue is not particularly limited in the present invention, with well known to those skilled in the art broken
Glue process and parameter, those skilled in the art can carry out according to practical condition, product quality and requirement
Selection and adjustment.The detailed process and parameter of the mastication is not particularly limited in the present invention, with known to those skilled in the art
Mastication process and parameter, those skilled in the art can be according to practical condition, product quality and requirement
It is selected and is adjusted, the temperature of mastication of the present invention, the i.e. roller temperature of opening rubber mixing machine, preferably 40~50 DEG C,
More preferably 42~48 DEG C, most preferably 44~46 DEG C；The pass of the mastication is preferably 1~3 time, can also be preferably 2 times.
The specific equipment of the broken glue and mastication is not particularly limited in the present invention, with well known to those skilled in the art normal
Advise equipment, those skilled in the art can be selected according to practical condition, product quality and requirement and
Adjustment, the equipment of broken glue and mastication of the present invention is preferably opening rubber mixing machine.
The specific steps of the mixing are not particularly limited in the present invention, and those skilled in the art can be according to actual production
Situation, product quality and requirement are selected and are adjusted, and the present invention is to ensure mixed uniformity, improves the property of product
Can, the step 1) is specially：
11) after non-asbestos organic fiber and graphite being carried out shredding stirring, just mixed object is obtained；
12) first mixed object, rubber, rubber chemicals and solvent that above-mentioned steps obtain are disperseed, add non-asbestos without
After machine fiber disperses again, cooling obtains mixture；
13) it in the mixture obtained to above-mentioned steps, after filler mixing is added, adds after interleaving agent mixes again, obtains
To master batch.
Equipment used in above-mentioned steps and parameter is not particularly limited in the present invention, with well known to those skilled in the art
The process and parameter that such product commonly stirs, those skilled in the art can be according to practical condition, product matter
Amount and requirement are selected and are adjusted, and the equipment used in step 1) of the present invention is preferably ploughshare blender.This
The mixing parametric used in the step 1) is invented, main paddle rotating speed is preferably 80~120r/min, more preferably 85~115r/min,
Most preferably 90~110r/min；The knife paddle rotating speed is preferably 1000~3000r/min, more preferably 1300~2700r/
Min, most preferably 1600~2400r/min.
After non-asbestos organic fiber and graphite are carried out shredding stirring by the present invention first, just mixed object is obtained.
The present invention is to improve the degree of scatter of fiber, for the mechanism that organic fiber is reunited, using graphite elder generation and non-asbestos
Organic fiber mixing shredding, effective solution non-asbestos organic fiber is due to static reason, the problem of causing to reunite.The present invention
The detailed process and parameter of shredding stirring are not particularly limited, the mistake stirred with shredding well known to those skilled in the art
Journey and parameter, those skilled in the art can select according to practical condition, product quality and requirement
And adjustment, the time of shredding stirring of the present invention is preferably 5~20min, more preferably 8~18min, most preferably 10~
15min。
Then the present invention disperses first mixed object, rubber, rubber chemicals and solvent that above-mentioned steps obtain, add non-
After asbestos inorfil disperses again, cooling obtains mixture.
The solvent is not particularly limited in the present invention, and the solvent with solvent rubber well known to those skilled in the art is
Can, those skilled in the art can select and adjust, this hair according to practical condition, product quality and requirement
It is bright to improve the performance of product to improve the degree of scatter of rubber, solvent of the present invention preferably include gasoline, toluene, dimethylbenzene,
It is one or more in acetone, heptane, methyl ethyl ketone, ethyl acetate and butanone, more preferably gasoline, toluene, dimethylbenzene, acetone,
Heptane, methyl ethyl ketone, ethyl acetate or butanone, most preferably gasoline or toluene.
The detailed process and parameter of the dispersion is not particularly limited in the present invention, with well known to those skilled in the art point
Scattered process and parameter, those skilled in the art can according to practical condition, product quality and requirement into
Row selection and adjustment, the present invention are to improve the degree of scatter of mixture, improve the performance of product, the time of dispersion of the present invention
Preferably 50~180min, more preferably 70~160min, most preferably 90~140min.
The detailed process disperseed again and parameter is not particularly limited in the present invention, with known to those skilled in the art
Dispersion process and parameter, those skilled in the art can want according to practical condition, product quality and use
It asks and is selected and adjusted, the present invention is to improve the degree of scatter of mixture, improves the performance of product, of the present invention to divide again
The scattered time is preferably 20~60min, more preferably 30~50min, most preferably 35~45min.
The detailed process and parameter of the cooling is not particularly limited in the present invention, with drop well known to those skilled in the art
Temperature process and parameter, those skilled in the art can according to practical condition, product quality and requirement into
Row selection and adjustment, the present invention are to improve the degree of scatter of mixture, improve the performance of product, the time of cooling of the present invention
Preferably 1~30min, more preferably 5~25min, most preferably 10~20min.
In the mixture that the present invention is finally obtained to above-mentioned steps, after filler mixing is added, adds interleaving agent and mix again
After conjunction, master batch is obtained.
The interleaving agent is not particularly limited in the present invention, and those skilled in the art can be according to practical condition, production
Quality and requirement are selected and are adjusted, and the present invention is to improve the degree of scatter of master batch, improves the performance of finished product material,
Interleaving agent of the present invention preferably includes ethyl alcohol.
The detailed process and parameter of the mixing is not particularly limited in the present invention, with well known to those skilled in the art point
Scattered process and parameter, those skilled in the art can according to practical condition, product quality and requirement into
Row selection and adjustment, the present invention are to improve the degree of scatter of mixture, improve the performance of product, the time of mixing of the present invention
Preferably 5~60min, more preferably 15~50min, most preferably 25~40min.
The detailed process mixed again and parameter is not particularly limited in the present invention, with known to those skilled in the art
Dispersion process and parameter, those skilled in the art can want according to practical condition, product quality and use
It asks and is selected and adjusted, the present invention is to improve the degree of scatter of mixture, improves the performance of product, of the present invention to mix again
The time of conjunction is preferably 5~60s, more preferably 15~50s, most preferably 25~40s.
Above-mentioned steps of the present invention provide the specific steps of raw material mixing, composition and respective spy of the present invention for raw material
Point, creative improves production technology, it is proposed that it is above-mentioned in batches, mixing dispersing technology step by step.
The masterbatch that the present invention finally obtains above-mentioned steps obtains sealing material after roll-in and vulcanization.
The concrete technology of the roll-in is not particularly limited in the present invention, with such technique well known to those skilled in the art
Middle conventional rolling process, those skilled in the art can be according to practical condition, product requirement and quality requirements
It is selected and is adjusted, roll-in of the present invention is preferably rolled into Zhang Gong's skill.
The equipment of the roll-in is not particularly limited in the present invention, with such technique central roll well known to those skilled in the art
Press equipment, those skilled in the art that can select and adjust according to practical condition, product requirement and quality requirement
Whole, the equipment of roll-in of the present invention is preferably roll squeezer.The actual temp of the roll-in is not particularly limited in the present invention, with
Roll temperature in such technique well known to those skilled in the art, those skilled in the art can be according to actual production feelings
Condition, product requirement and quality requirement are selected and are adjusted, and the temperature of roll-in of the present invention is preferably 80~200 DEG C, more excellent
It is selected as 90~190 DEG C, most preferably 100~180 DEG C.The line pressure of the roll-in is not particularly limited in the present invention, with ability
Rolling-line pressure in such technique known to field technique personnel, those skilled in the art can according to practical condition,
Product requirement and quality requirement are selected and are adjusted, and the line pressure of roll squeezer of the present invention is preferably 4~16t, more preferably
For 6~14t, most preferably 8~12t.The steam pressure of the roll-in is not particularly limited in the present invention, with people in the art
Roll-in steam pressure in such technique known to member, those skilled in the art can want according to practical condition, product
It asks and quality requirement is selected and adjusted, the steam pressure of roll squeezer of the present invention is preferably 0.1~0.5MPa, more preferably
For 0.2~0.4MPa, most preferably 0.25~0.35MPa.
The present invention is to improve the integrality and operability of preparation process, further includes solvent recovery step after the roll-in.
The concrete technology to the solvent recovery is not particularly limited in the present invention, in such technique well known to those skilled in the art
Conventional solvent recovery process, those skilled in the art can want according to practical condition, product requirement and quality
It asks and is selected and adjusted, solvent recovery of the present invention is preferably activated carbon adsorption recovery process.
The concrete technology of the vulcanization is not particularly limited in the present invention, with such technique well known to those skilled in the art
Middle conventional sulfuration process, those skilled in the art can be according to practical condition, product requirement and quality requirements
It is selected and is adjusted.
The equipment of the vulcanization is not particularly limited in the present invention, with sulphur in such technique well known to those skilled in the art
Change equipment, those skilled in the art can select and adjust according to practical condition, product requirement and quality requirement
Whole, the equipment of vulcanization of the present invention is preferably vulcanizing press.The present invention does not limit the actual temp of the vulcanization especially
System, with curing temperature in such technique well known to those skilled in the art, those skilled in the art can be according to practical life
Production situation, product requirement and quality requirement are selected and are adjusted, and the temperature of vulcanization of the present invention is preferably 143~155 DEG C,
More preferably 145~153 DEG C, most preferably 147~151 DEG C.The pressure of the vulcanization is not particularly limited in the present invention, with this
Sulfide stress in such technique known to field technology personnel, those skilled in the art can according to practical condition,
Product requirement and quality requirement are selected and are adjusted, and the line pressure of vulcanization of the present invention is preferably 10~16MPa, more preferably
For 11~15MPa, most preferably 12~14MPa.The time of the vulcanization is not particularly limited in the present invention, with art technology
Vulcanization time in such technique known to personnel, those skilled in the art can be according to practical condition, product requirements
And quality requirement is selected and is adjusted, the time of vulcanization of the present invention is preferably 6~20min, more preferably 8~18min,
Most preferably 10~15min.
The present invention is to improve the integrality and operability of preparation process, further includes baking step before the vulcanization.This hair
The bright concrete technology to the baking step is not particularly limited, with conventional in such technique well known to those skilled in the art
Baking step, those skilled in the art can select according to practical condition, product requirement and quality requirement
It selects and adjusts, the temperature of baking step of the present invention is preferably 60~100 DEG C, more preferably 70~90 DEG C, most preferably 75
~85 DEG C；The time of baking step of the present invention is preferably 4~10h, more preferably 5~9h, most preferably 6~8h；This hair
The equipment of the bright drying preferably dries hole.
Above-mentioned steps of the present invention provide a kind of graphite sealing material and preparation method thereof, graphite grazing provided by the invention
Material does not contain asbestos component, combines the prominent characteristic that rear high temperature resistant grade improves using graphite and rubber, is aided with special ratios
Graphite and rubber, then add specific combination and ratio other auxiliary agents, moreover, the present invention be directed to material different characteristics, in conjunction with
The selection of ingredient and ratio is prepared using hybrid technique in batches step by step in conjunction with Zhang Gong's skill and other techniques is rolled into
The graphite sealing material is obtained.Graphite sealing material prepared by the present invention, the high temperature resistance for effectively raising sealing material are resistance to
Ability, lift-off seal material ensure that sealing is permanently effective, solve existing asbestos in the useful life longevity of worst hot case environment
The environmental protection of class sealed material is not up to standard rather than the problem of sealed material high temperature resistance difference.
The experimental results showed that the graphite sealing material without containing asbestos component prepared by the present invention, temperature in use reach
260~300 DEG C, compare the temperature in use of 180~250 DEG C of common non-asbestos gasket, improve 20%~44%, and with compared with
Good room temperature and elevated-temperature seal performance, can meet or exceed relevant standard.
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 only 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
Graphite grazing lining plank I type factory formulas, referring to table 1.
Table 1
| Thickness：0.25~3.00mm | Graphite grazing lining plank I types |
| Raw material title | Actual amount (kg) |
| Nitrile rubber | 28.00 |
| It is total | 28.00 |
| Sofril | 0.96 |
| Accelerating agent | 0.90 |
| Zinc oxide | 1.80 |
| Plasticizer | 0.50 |
| Anti-aging agent | 0.80 |
| It is total | 4.96 |
| White carbon | 10.00 |
| Kaolin | 13.00 |
| Graphite powder | 45.00 |
| Artificial mine is fine | 44.00 |
| Fanglun slurry cake | 10 |
| It is total | 122.00 |
| It amounts to | 154.96 |
| Toluene | 85L |
| Alcohol | 22L |
Preparation process：
Process 1：The mastication of nitrile rubber
By dosage as defined in formula, nitrile rubber (tolerance+0.2kg) is weighed；
By the nitrile rubber after weighing, the mastication 2 times on the rubber mixing machine that roller temperature is 42 DEG C, it is thin it is logical after break into film
Shape, it is spare.
Process 2：Dispensing
By defined dosage is formulated in table 1, rubber chemicals (tolerance+0.005kg) are weighed：Cosan, accelerating agent, oxidation
Zinc, plasticizer, anti-aging agent.It is spare；
By other raw material types in table 1, defined dosage (tolerance+0.2kg) is weighed.
Process 3：Material mixing
Equipment：Ploughshare blender；Rotating speed：Main slurry 105r/min, knife starch 1800r/min；
Whipping step：
1st step：Fanglun slurry cake, graphite powder is added；Mixing time 8min；
2nd step：Nitrile rubber, rubber chemicals, kaolin, toluene is added；Mixing time 58min；
3rd step：It is fine that artificial mine is added；Mixing time：20min；
4th step：Cooling；Temperature fall time：5min；
5th step：White carbon is added；Mixing time 30min；
6th step：Alcohol is added；Mixing time 30s；
7th step：Discharging is packed into container, spare.
Process 4：It is rolled into and opens
Equipment：509 at a machine；
Cheng Zhangji steam pressures are 0.30MPa；
Cheng Zhangji roller temperatures are 130 DEG C；
Roller line pressure is 12t；
Processing thickness is 2.0mm planks, material quantity 30kg；
Process 5：Vulcanization
Equipment：Dry hole, vulcanizing press；
(1) plank is put into drying hole and is dried, paragraph 1 vulcanization；Temperature：70 DEG C, the time：8h；
(2) it will be placed on vulcanizing press by the plank of paragraph 1 vulcanization, carry out the 2nd section of vulcanization；Temperature：149℃；Pressure
Power：12MPa；Time：10min.
Plank after over cure is finished product plank, i.e. graphite grazing lining plank.
Performance detection is carried out to graphite grazing lining plank prepared by the embodiment of the present invention 1.
Detecting instrument：(1) insulating box；(2) instron；(3) compression rebound tester；(4) creep relaxation rate
Tester；(5) gas tightness tester；(6) oil seal testing machine.
Referring to table 2, table 2 is the performance data of graphite grazing lining plank prepared by embodiment 1.
Table 2
Embodiment 2
Graphite grazing lining plank II type factory formulas, referring to table 3.
Table 3
| Thickness：0.25~3.00mm | Graphite grazing lining plank II types |
| Raw material title | Actual amount (kg) |
| Hydrogenated nitrile-butadiene rubber | 32.00 |
| It is total | 32.00 |
| Sofril | 1.11 |
| Accelerating agent | 0.94 |
| Zinc oxide | 1.50 |
| Plasticizer | 0.90 |
| Anti-aging agent | 0.60 |
| It is total | 5.05 |
| White carbon | 12.00 |
| Carbon black | 5.00 |
| Graphite powder | 50.00 |
| Artificial mine is fine | 36.00 |
| Fanglun slurry cake | 15.00 |
| It is total | 118.00 |
| It amounts to | 155.05 |
| Toluene | 98L |
| Alcohol | 43L |
Preparation process：
Process 1：The mastication of hydrogenated nitrile-butadiene rubber
By dosage as defined in formula, hydrogenated nitrile-butadiene rubber (tolerance+0.2kg) is weighed；
By the hydrogenated nitrile-butadiene rubber after weighing, the mastication 2 times on the rubber mixing machine that roller temperature is 45 DEG C, it is thin it is logical after break into glue
Sheet, it is spare.
Process 2：Dispensing
By defined dosage is formulated in table 1, rubber chemicals (tolerance+0.005kg) are weighed：Cosan, accelerating agent, oxidation
Zinc, plasticizer, anti-aging agent.It is spare；
By other raw material types in table 1, defined dosage (tolerance+0.2kg) is weighed.
Process 3：Material mixing
Equipment：Ploughshare blender；Rotating speed：Main slurry 100r/min, knife starch 1850r/min；
Whipping step：
1st step：Fanglun slurry cake, graphite powder is added；Mixing time 15min；
2nd step：Nitrile rubber, rubber chemicals, kaolin, carbon black, toluene is added；Mixing time 62min；
3rd step：It is fine that artificial mine is added；Mixing time：25min；
4th step：Cooling；Temperature fall time：10min；
5th step：White carbon is added；Mixing time 40min；
6th step：Alcohol is added；Mixing time 50s；
7th step：Discharging is packed into container, spare.
Process 4：It is rolled into and opens
Equipment：509 at a machine；
Cheng Zhangji steam pressures are 0.25MPa；
Cheng Zhangji roller temperatures are 120 DEG C；
Roller line pressure is 13t；
Processing thickness is 0.5mm planks, material quantity 8.5kg；
Process 5：Vulcanization
Equipment：Dry hole, vulcanizing press；
(1) plank is put into drying hole and is dried, paragraph 1 vulcanization；Temperature：60 DEG C, the time：9h；
(2) it will be placed on vulcanizing press by the plank of paragraph 1 vulcanization, carry out the 2nd section of vulcanization；Temperature：145℃；Pressure
Power：15MPa；Time：12min.
Plank after over cure is finished product plank, i.e. graphite grazing lining plank.
Performance detection is carried out to graphite grazing lining plank prepared by the embodiment of the present invention 2.
Detecting instrument：(1) insulating box；(2) instron；(3) compression rebound tester；(4) creep relaxation rate
Tester；(5) gas tightness tester；(6) oil seal testing machine.
Referring to table 4, table 4 is the performance data of graphite grazing lining plank prepared by embodiment 2.
Table 4
Embodiment 3
Graphite grazing lining plank type III factory formula, referring to table 5.
Table 5
Preparation process：
Process 1：Dispensing
By defined dosage is formulated in table 1, powder nitrile rubber (tolerance+0.2kg) is weighed.It is spare；
By defined dosage is formulated in table 1, rubber chemicals (tolerance+0.005kg) are weighed：Cosan, accelerating agent, oxidation
Zinc, plasticizer, anti-aging agent.It is spare；
By other raw material types in table 1, defined dosage (tolerance+0.2kg) is weighed.
Process 2：Material mixing
Equipment：Ploughshare blender；Rotating speed：Main slurry 110r/min, knife starch 1900r/min；
Whipping step：
1st step：Fanglun slurry cake, graphite powder is added；Mixing time 20min；
2nd step：Nitrile rubber, rubber chemicals, kaolin, carbon black, toluene is added；Mixing time 68min；
3rd step：It is fine that artificial mine is added；Mixing time：30min；
4th step：Cooling；Temperature fall time：7min；
5th step：White carbon is added；Mixing time 35min；
6th step：Alcohol is added；Mixing time 40s；
7th step：Discharging is packed into container, spare.
Process 3：It is rolled into and opens
Equipment：509 at a machine；
Cheng Zhangji steam pressures are 0.35MPa；
Cheng Zhangji roller temperatures are 140 DEG C；
Roller line pressure is 16t；
Processing thickness is 0.5mm planks, material quantity 8.5kg；
Process 4：Vulcanization
Equipment：Dry hole, vulcanizing press；
(1) plank is put into drying hole and is dried, paragraph 1 vulcanization；Temperature：75 DEG C, the time：6h；
(2) it will be placed on vulcanizing press by the plank of paragraph 1 vulcanization, carry out the 2nd section of vulcanization；Temperature：147℃；Pressure
Power：15MPa；Time：15min.
Plank after over cure is finished product plank, i.e. graphite grazing lining plank.
Performance detection is carried out to graphite grazing lining plank prepared by the embodiment of the present invention 3.
Detecting instrument：(1) insulating box；(2) instron；(3) compression rebound tester；(4) creep relaxation rate
Tester；(5) gas tightness tester；(6) oil seal testing machine.
Referring to table 6, table 6 is the performance data of graphite grazing lining plank prepared by embodiment 3.
Table 6
A kind of gasket seal provided by the invention and preparation method thereof is described in detail above, it is used herein
Principle and implementation of the present invention are described for specific case, and the explanation of above example is only intended to help to understand
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 manufactures and use any device or system, and implements the method for any combination.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 also fall within the protection scope of the claims of the present invention.The range 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
Applying example has the structural element for being not different from claim character express, or if they include the word with claim
The equivalent structural elements without essence difference are stated, then these other embodiments should also be included in the scope of the claims.
Claims (8)
1. a kind of preparation method of graphite sealing material, which is characterized in that include the following steps：
1）After graphite, rubber, rubber chemicals, non-asbestos fiber and filler are mixed, masterbatch is obtained；
Above-mentioned proportioning is：
30 ~ 50 parts by weight of graphite；
The graphite includes amorphous graphite and/or crystalline flake graphite；
14 ~ 75 parts by weight of rubber；
10 ~ 100 parts by weight of non-asbestos fiber；
The non-asbestos fiber includes non-asbestos organic fiber and non-asbestos inorfil；
5 ~ 20 parts by weight of reinforced filling；
The reinforced filling includes one or more in kaolin, carbon black and white carbon；
The 4% ~ 23% of rubber chemicals rubber consumption；
The step 1）Specially：
11）After non-asbestos organic fiber and graphite are carried out shredding stirring, just mixed object is obtained；
12）First mixed object, rubber, rubber chemicals and solvent that above-mentioned steps obtain are disperseed, the inorganic fibre of non-asbestos is added
After dimension is disperseed again, cooling obtains mixture；
13）In the mixture obtained to above-mentioned steps, after reinforced filling mixing is added, adds after interleaving agent mixes again, obtain
To master batch；
2）The masterbatch that above-mentioned steps are obtained obtains sealing material after roll-in and vulcanization.
2. preparation method according to claim 1, which is characterized in that the rubber includes nitrile rubber, natural rubber, fourth
It is one or more in benzene rubber, neoprene and hydrogenated nitrile-butadiene rubber；
The rubber chemicals include one or more in vulcanizing agent, accelerating agent, activating agent, anti-aging agent and plasticizer.
3. preparation method according to claim 2, which is characterized in that the rubber includes the butyronitrile rubber of 5 ~ 30 parts by weight
The butadiene-styrene rubber of glue, the natural rubber of 4 ~ 20 parts by weight and 5 ~ 20 parts by weight；
The granularity of the graphite is 45 ~ 550 μm；
The non-asbestos fiber includes that Fanglun slurry cake and artificial mine are fine；
The rubber chemicals include account for the vulcanizing agent of the rubber consumption 1% ~ 5%, the accelerating agent for accounting for the rubber consumption 1% ~ 5%,
It accounts for the activating agent of the rubber consumption 1% ~ 8% and accounts for the anti-aging agent of the rubber consumption 1% ~ 5%.
4. preparation method according to claim 1, which is characterized in that the rubber is the rubber after breaking glue and mastication
Piece；
The temperature of the mastication is 40 ~ 50 DEG C；
The pass of the mastication is 1 ~ 3 time；
The solvent includes one kind or more in gasoline, toluene, dimethylbenzene, acetone, heptane, methyl ethyl ketone, ethyl acetate and butanone
Kind；
The interleaving agent includes ethyl alcohol.
5. preparation method according to claim 1, which is characterized in that the time of the shredding stirring is 5 ~ 20min；
The time of the dispersion is 50 ~ 180min；
The time disperseed again is 20 ~ 60min；
The time of the cooling is 1 ~ 30min；
The time of the mixing is 5 ~ 60min；
The time mixed again is 5 ~ 60s.
6. preparation method according to claim 1, which is characterized in that further include baking step before the vulcanization；
The temperature of the drying is 60 ~ 100 DEG C；
The time of the drying is 4 ~ 10h.
7. preparation method according to claim 6, which is characterized in that the pressure of the vulcanization is 10 ~ 16MPa；
The temperature of the vulcanization is 143 ~ 155 DEG C；
The time of the vulcanization is 6 ~ 20min.
8. the preparation method described according to claim 6 or 7, which is characterized in that the temperature of the roll-in is 80 ~ 200 DEG C；
The line pressure of the roll-in is 4 ~ 16t；
The steam pressure of the roll-in is 0.1 ~ 0.5MPa.
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| CN108299786A (en) * | 2018-01-11 | 2018-07-20 | 山东润银生物化工股份有限公司 | A kind of high temperature resistant self-lubricating sealing material and preparation method thereof |
| CN108953608B (en) * | 2018-08-24 | 2021-02-26 | 灏印(宁波)波纹管技术有限公司 | Graphite-based composite sealing element and preparation method thereof |
| CN109778590A (en) * | 2019-01-11 | 2019-05-21 | 浙江理工大学 | A kind of modified expanded graphite composite seal preparation method |
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