CN106700154A - Graphite sealing material and preparation method thereof - Google Patents
Graphite sealing material and preparation method thereof Download PDFInfo
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- CN106700154A CN106700154A CN201710037377.8A CN201710037377A CN106700154A CN 106700154 A CN106700154 A CN 106700154A CN 201710037377 A CN201710037377 A CN 201710037377A CN 106700154 A CN106700154 A CN 106700154A
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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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a graphite sealing material prepared from the following raw materials: 30 to 50 parts by weight of graphite, 14 to 75 parts by weight of rubber, 10 to 100 parts by weight of non-asbestos fibers, 5 to 20 parts by weight of a filler, and a rubber auxiliary agent, wherein the amount of the rubber auxiliary agent is 4% to 23% of the amount of the rubber. The graphite sealing material provided by the invention is a non-asbestos graphite sealing material, does not contain an asbestos ingredient; with use of an outstanding characteristic of the improved high temperature resistant level after graphite is combined with the rubber, with supplement of a certain proportion of the graphite and the rubber, and with addition of a specific combination and proportion of other auxiliary agents, the high temperature resistant ability of the sealing material is effectively improved, the use durability of the sealing material in a high temperature working environment is enhanced, and long-term effective sealing is ensured.
Description
Technical field
The invention belongs to encapsulant preparing technical field, more particularly to a kind of graphite sealing material and preparation method thereof.
Background technology
Encapsulant refers to just that can bear seam displacement to reach airtight, watertight purpose, and the seam such as flush mounting, building
In material.Encapsulant is almost related to all of industry and civil area, in national defence, chemical industry, coal, oil, metallurgy, friendship
Playing the role of for the aspects such as logical transport, machine building industry and Aero-Space is important.Encapsulant is divided into stream with its form
Body encapsulant, not fluid tight material, dynamic sealing and the major class of static seal four, including pump sealing, hydraulic packing, flange are close
Envelope, equipment sealing, faying face sealing and auxiliary seal etc., can be configured to liquid or paste when in use, be coated in two
Between the contact surface of part, solidify under certain conditions or sealed in non-drying putty；Can also be processed into various
The solid or hollow ring of shape seals between being arranged on the contact surface of two parts.The former claims encapsulant to be served only for two
Static seal position of the component contact face without relative motion；The latter claims encapsulant to can be not only used for static seal position, and two are can be used for again
The contact surface of part has the dynamic sealing position of relative motion.
Encapsulant typically has good physical and mechanical property, resilience is high, compression set is small, sealing can
The advantages of by, easy to process and long service life.As silicone rubber sealant energy high temperature resistant and low temperature, radiation hardness, vacuum-resistant, without dirt
Dye, it 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 encapsulant directly affects the production efficiency of mechanical body equipment, right
The service efficiency of equipment has a great impact.
Seal material has metal material (aluminium, lead, indium, stainless steel etc.), also there is nonmetallic materials (rubber, plastics, pottery
Porcelain, graphite etc.), composite (such as rubber-asbestos board, aerogel blanket-polyurethane), as commonly use sealing member material if include gold
Category spirotallic gasket, metal ring gasket, Graphite pad, metal jacketed gasket, Tetrafluoro spacer, non-asbestos pad, without asbestos washer, rubber
Glue gasket, electronic isolation pad etc..Among these, the encapsulant of asbestos component, because high-temperature resistance is strong, widely should
For plant equipment (such as：Automobile engine, motorcycle start, general purpose engine, air presses, refrigeration compressor, tube method
Orchid, valve etc.) connecting portion sealing.
But in recent years, influenceed by environmental protection condition, the use of this kind of gasket material gradually receives increasing limit
System.And relatively environment-friendly non-asbestos pad, in use, in lasting or intermittent high temperatures, meson pressure, meson burn into are pre-
In the presence of tight stress, the high-temperature resistance reduction of pad causes meson seepage, seal failure.
Therefore, a kind of non-asbestos seal material with more preferable high-temperature resistance how is found, it has also become many in the industry
One of production firm's problem demanding prompt solution.
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 graphite sealing material and preparation method thereof,
The graphite sealing material that the present invention is provided does not contain asbestos component, and with preferable high temperature resistant property.
The invention provides a kind of graphite sealing material, it is obtained by including following raw material：
Preferably, the rubber includes nitrile rubber, natural rubber, butadiene-styrene rubber, neoprene and hydrogenated nitrile-butadiene rubber
In one or more；
The graphite includes graphite powder；
The non-asbestos fiber includes non-asbestos organic fiber and/or non-asbestos inorfil；
Described filler includes reinforced filling；
The rubber chemicals include one or more in vulcanizing agent, accelerator, activating agent, age resistor and plasticizer.
Preferably, the rubber includes nitrile rubber, the natural rubber of 4~20 weight portions and 5~20 of 5~30 weight portions
The butadiene-styrene rubber of weight portion；
The granularity of the graphite powder is 45~550 μm；
The non-asbestos fiber includes that Fanglun slurry cake and people's dressing are fine；
Described filler includes one or more in kaolin, carbon black and white carbon；
The rubber chemicals include accounting for the vulcanizing agent of the rubber consumption 1%~5%, account for the rubber consumption 1%~5%
Accelerator, account for the activating agent of the rubber consumption 1%~8% and account for the age resistor of the rubber consumption 1%~5%.
Present invention also offers a kind of preparation method of graphite sealing material, comprise 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 is by after roll-in and vulcanization, obtaining encapsulant.
Preferably, the non-asbestos fiber includes non-asbestos organic fiber and non-asbestos inorfil；
The step 1) it is specially：
11) after non-asbestos organic fiber and graphite being carried out into shredding stirring, just mixed thing is obtained；
12) first mixed thing, rubber, rubber chemicals and solvent that above-mentioned steps are obtained are disperseed, add non-asbestos without
After machine fiber disperses again, cooling obtains mixture；
13) in the mixture for obtaining to above-mentioned steps, after adding filler mixing, add after interleaving agent mixes again, obtain
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 the one kind in gasoline, toluene, dimethylbenzene, acetone, heptane, MEK, ethyl acetate and butanone
Or it is various；
The interleaving agent includes ethanol.
Preferably, the time of the shredding stirring is 5~20min；
The scattered time is 50~180min；
The scattered time is 20~60min；
The time of the cooling is 1~30min；
The time of the mixing is 5~60min；
The time for mixing again is 5~60s.
Preferably, baking step is also included 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 invention provides a kind of graphite sealing material, it is obtained by including following raw material, the graphite of 30~50 weight portion,
The rubber of 14~75 weight portions, the non-asbestos fiber of 10~100 weight portions, the filler and rubber chemicals of 5~20 weight portions；Institute
It is the 4%~23% of rubber consumption to state the consumption of rubber chemicals.Compared with prior art, the present invention is directed to existing non-asbestos pad
Piece, in use, under conditions of lasting or intermittent high temperatures, meson pressure, meson corrosion and the effect of pre-tight stress
Under, the high-temperature resistance reduction of pad causes meson seepage, the defect of seal failure.The invention provides a kind of graphite grazing
Material, is a kind of graphite sealing material of non-asbestos, and the graphite sealing material that the present invention is provided does not contain asbestos component, using stone
Ink and rubber combine the prominent characteristic that rear high temperature resistant grade is improved, and are aided with the graphite and rubber of special ratios, then add particular combination
With other auxiliary agents of ratio, the resistance to ability of high temperature resistance of encapsulant is effectively raised, lift-off seal material is in worst hot case ring
The useful life longevity in border, it is ensured that sealing is permanently effective.
Test result indicate that, the graphite sealing material for not containing asbestos component prepared by the present invention, temperature in use reaches
260~300 DEG C, compared to 180~250 DEG C of temperature in use of common non-asbestos pad, improve 20%~44%, and with compared with
Good normal temperature and elevated-temperature seal performance, can meet or exceed the standard of correlation.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, but
It should be appreciated that these descriptions are intended merely to further illustrate the features and advantages of the present invention, rather than to invention claim
Limitation.
The all raw materials of the present invention, originate to it and are not particularly limited, commercially buying or according to people in the art
Known to member prepared by conventional method.
The all raw materials of the present invention, are not particularly limited, present invention preferably employs technical pure or superhard material work to its purity
The conventional purity that tool manufacture and hard brittle material manufacture field are used.
The invention provides a kind of graphite sealing material, it is obtained by including following raw material：
The present invention is not particularly limited to the graphite, with graphite material well known to those skilled in the art, ability
Field technique personnel can be selected and be adjusted according to practical condition, product quality and use 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
Invention is not particularly limited to the granularity of the graphite, with the granularity of graphite powder well known to those skilled in the art, ability
Field technique personnel can be selected and be adjusted according to practical condition, product quality and use requirement, of the present invention
The granularity of graphite is preferably 45~550 μm, most preferably more preferably 100~450 μm, 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. 325 mesh~200 mesh,
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. 120 mesh~30 mesh, most preferably more preferably 220~450 μm, 320~350 μm.This
The addition of the graphite is invented for 30~50 weight portions, preferably 32~48 weight portions, more preferably 34~46 weight portions, most
Preferably 36~44 weight portions.
The present invention is not particularly limited to the rubber, with elastomeric material well known to those skilled in the art, ability
Field technique personnel can be selected and be adjusted according to practical condition, product quality and use requirement, of the present invention
Rubber preferably includes 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
Elect nitrile rubber, natural rubber and butadiene-styrene rubber as.Nitrile rubber of the present invention includes PNBR.
The addition of rubber of the present invention be 14~75 weight portions, preferably 24~65 weight portions, more preferably 34~
55 weight portions, most preferably 40~50 weight portions.Specifically chosen and its corresponding addition of the present invention to the elastomeric 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 be with root
Selected and adjusted according to practical condition, product quality and use requirement, the addition of nitrile rubber of the present invention
Preferably 5~30 weight portions, more preferably 10~25 weight portions, most preferably 15~20 weight portions；Natural rubber of the present invention
The addition of glue is preferably 4~20 weight portions, most preferably more preferably 6~18 weight portions, 10~24 weight portions；Institute of the present invention
The addition for stating butadiene-styrene rubber is preferably 5~20 weight portions, most preferably more preferably 8~17 weight portions, 11~14 weight portions.
The present invention is not particularly limited to the non-asbestos fiber, with fibrous non-stone 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 use 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 is not limited especially the specifically chosen of the non-asbestos organic fiber
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 use requirement are selected and 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 to the specifically chosen of non-asbestos inorfil
There is especially 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 use requirement are selected and adjusted, and non-asbestos inorfil of the present invention is preferably
Non-asbestos type manually sinters the artificial inorganic reinforcing fiber of manufacture, and more preferably people's dressing is fine.
The addition of non-asbestos fiber of the present invention be 10~100 weight portions, preferably 20~90 weight portions, more preferably
It is 30~80 weight portions, most preferably 50~60 weight portions.The present invention is to the specifically chosen and its corresponding of the non-asbestos fiber
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 be adjusted according to practical condition, product quality and use requirement, and non-asbestos of the present invention has
The addition of machine fiber is preferably 10~40 weight portions, most preferably more preferably 15~35 weight portions, 20~30 weight portions；This
The addition for inventing the non-asbestos inorfil is preferably 10~60 weight portions, more preferably 20~50 weight portions, most preferably
It is 30~40 weight portions.
The present invention is not particularly limited to described filler, with the filler for encapsulant well known to those skilled in the art
, those skilled in the art can be selected and be adjusted according to practical condition, product quality and use requirement, this
Invention described filler preferably includes reinforced filling, more specifically preferably includes 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 weight portions, preferably 7~18 weights
Amount part, most preferably more preferably 9~16 weight portions, 11~14 weight portions.
The present invention is not particularly limited to the rubber chemicals, with well known to those skilled in the art for elastomeric material
Rubber chemicals, those skilled in the art can be selected according to practical condition, product quality and use requirement
And adjustment, rubber chemicals of the present invention preferably include the one kind in vulcanizing agent, accelerator, activating agent, age resistor and plasticizer
Or it is various, one or more more preferably in vulcanizing agent, accelerator, activating agent, age resistor and plasticizer, most preferably vulcanize
Agent, accelerator, activating agent, age resistor 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 present invention is not particularly limited to the specifically chosen and its corresponding addition of the rubber chemicals, with this area skill
Conventional selection and addition known to art personnel, those skilled in the art can be according to practical condition, product qualities
And use requirement is selected and adjusted, the addition of vulcanizing agent of the present invention is preferably 1%~5%, more preferably 2%
~4%, most preferably 2.5%~3.5%；The addition of accelerator of the present invention is preferably 1%~5%, more preferably 2%
~4%, most preferably 2.5%~3.5%；The addition of activating agent of the present invention is preferably 1%~8%, more preferably 2%
~7%, more preferably 3%~6%, most preferably 4%~5%；The addition of age resistor of the present invention is preferably 1%~
5%, more preferably 2%~4%, most preferably 2.5%~3.5%.
Present invention also offers a kind of preparation method of graphite sealing material, comprise 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 is by after roll-in and vulcanization, obtaining encapsulant.
Raw material in selection and optimum principle, with foregoing graphites encapsulant of the present invention to the raw material in above-mentioned preparation method
Selection and optimum principle can carry out correspondence, this is no longer going to repeat them.
The present invention is not particularly limited to the pretreatment process of rubber in the preparation process, 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
Ask and selected and adjusted, rubber of the present invention is preferably the sheet rubber after breaking glue and mastication.
The present invention is not particularly limited to the detailed process and parameter of the broken glue, with well known to those skilled in the art broken
Glue process and parameter, those skilled in the art can be carried out according to practical condition, product quality and use requirement
Selection and adjustment.The present invention is not particularly limited to the detailed process and parameter of the mastication, is known with those skilled in the art
Mastication process and parameter, those skilled in the art can be according to practical condition, product quality and use requirement
Selected and adjusted, the roller temperature of the temperature of mastication of the present invention, i.e. 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, it is also possible to preferably 2 times.
The present invention is not particularly limited to the specific equipment of the broken glue and mastication, with well known to those skilled in the art normal
Rule equipment, those skilled in the art can be selected according to practical condition, product quality and use requirement and
The equipment of adjustment, broken glue of the present invention and mastication is preferably opening rubber mixing machine.
The present invention is not particularly limited to the specific steps of the mixing, and those skilled in the art can be according to actual production
Situation, product quality and use requirement are selected and adjusted, and the present invention is the uniformity for ensureing to mix, and improves the property of product
Can, the step 1) it is specially：
11) after non-asbestos organic fiber and graphite being carried out into shredding stirring, just mixed thing is obtained；
12) first mixed thing, rubber, rubber chemicals and solvent that above-mentioned steps are obtained are disperseed, add non-asbestos without
After machine fiber disperses again, cooling obtains mixture；
13) in the mixture for obtaining to above-mentioned steps, after adding filler mixing, add after interleaving agent mixes again, obtain
To master batch.
The equipment and parameter that the present invention is used above-mentioned steps are not particularly limited, with well known to those skilled in the art
The process and parameter of the conventional stirring of such product, those skilled in the art can be according to practical condition, product matter
Amount and use requirement selected and adjusted, step 1 of the present invention) used by equipment be preferably ploughshare mixer.This
Invent the step 1) used by mixing parametric, main oar rotating speed is preferably 80~120r/min, more preferably 85~115r/min,
Most preferably 90~110r/min；The knife oar 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 thing is obtained.
The present invention is the degree of scatter of raising fiber, for the mechanism that organic fiber is reunited, using graphite elder generation and non-asbestos
Organic fiber mixing shredding, effectively solves non-asbestos organic fiber due to static reason, the problem for causing to reunite.The present invention
Detailed process and parameter to shredding stirring are not particularly limited, with the mistake that shredding well known to those skilled in the art is stirred
Journey and parameter, those skilled in the art can be selected according to practical condition, product quality and use requirement
And adjustment, time of shredding of the present invention stirring be preferably 5~20min, more preferably 8~18min, most preferably 10~
15min。
Then the present invention is disperseed first mixed thing, rubber, rubber chemicals and solvent that above-mentioned steps are obtained, is added non-
After asbestos inorfil disperses again, cooling obtains mixture.
The present invention is not particularly limited to the solvent, and the solvent with solvent rubber well known to those skilled in the art is
Can, those skilled in the art can be selected and be adjusted, this hair according to practical condition, product quality and use requirement
It is bright be improve rubber degree of scatter, improve product performance, solvent of the present invention preferably include gasoline, toluene, dimethylbenzene,
One or more in acetone, heptane, MEK, ethyl acetate and butanone, more preferably gasoline, toluene, dimethylbenzene, acetone,
Heptane, MEK, ethyl acetate or butanone, most preferably gasoline or toluene.
The present invention is not particularly limited to the scattered detailed process and parameter, with well known to those skilled in the art point
Scattered process and parameter, those skilled in the art can enter according to practical condition, product quality and use requirement
Row selection and adjustment, the present invention are to improve the degree of scatter of mixture, improve the performance of product, scattered time of the present invention
Preferably 50~180min, more preferably 70~160min, most preferably 90~140min.
The present invention is not particularly limited to the detailed process scattered again and parameter, is known with those skilled in the art
Scattered process and parameter, those skilled in the art can according to practical condition, product quality and using will
Ask and selected and adjusted, the present invention is the degree of scatter of raising mixture, improve the performance of product, it is of the present invention to divide again
The scattered time is preferably 20~60min, most preferably more preferably 30~50min, 35~45min.
The present invention is not particularly limited to the detailed process and parameter of the cooling, with drop well known to those skilled in the art
The process and parameter of temperature, those skilled in the art can enter according to practical condition, product quality and use requirement
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 of the invention last mixture obtained to above-mentioned steps, after adding filler mixing, add interleaving agent and mix again
After conjunction, master batch is obtained.
The present invention is not particularly limited to the interleaving agent, and those skilled in the art can be according to practical condition, product
Quality and use requirement are selected and adjusted, and the present invention is the degree of scatter of raising master batch, improves the performance of finished product material,
Interleaving agent of the present invention preferably includes ethanol.
The present invention is not particularly limited to the detailed process and parameter of the mixing, with well known to those skilled in the art point
Scattered process and parameter, those skilled in the art can enter according to practical condition, product quality and use requirement
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 present invention is not particularly limited to the detailed process for mixing again and parameter, is known with those skilled in the art
Scattered process and parameter, those skilled in the art can according to practical condition, product quality and using will
Ask and selected and adjusted, the present invention is the degree of scatter of raising mixture, improve the performance of product, it is of the present invention to mix again
The time of conjunction is preferably 5~60s, most preferably more preferably 15~50s, 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 last masterbatch for obtaining above-mentioned steps of the invention is by after roll-in and vulcanization, obtaining encapsulant.
The present invention is not particularly limited to the concrete technology of the roll-in, 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 requirement
Selected and adjusted, roll-in of the present invention is preferably and is rolled into Zhang Gong's skill.
The present invention is not particularly limited to the equipment of the roll-in, with such technique central roll well known to those skilled in the art
Pressure equipment, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement
Whole, the equipment of roll-in of the present invention is preferably roll squeezer.The present invention is not particularly limited to the actual temp of the roll-in, 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 adjusted, and the temperature of roll-in of the present invention is preferably 80~200 DEG C, more excellent
Elect 90~190 DEG C, most preferably 100~180 DEG C as.The present invention is not particularly limited to the line pressure of the roll-in, 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 adjusted, and the line pressure of roll squeezer of the present invention is preferably 4~16t, more preferably
It is 6~14t, most preferably 8~12t.The present invention is not particularly limited to the steam pressure of the roll-in, 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
Ask 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
It is 0.2~0.4MPa, most preferably 0.25~0.35MPa.
The present invention is the integrality and operability of raising preparation process, and solvent recovery step is also included after the roll-in.
The present invention is not particularly limited to the concrete technology to the solvent recovery, with 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
Ask and selected and adjusted, solvent recovery of the present invention is preferably charcoal absorption recovery process.
The present invention is not particularly limited to the concrete technology of the vulcanization, 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 requirement
Selected and adjusted.
The present invention is not particularly limited to the equipment of the vulcanization, with sulphur in such technique well known to those skilled in the art
Change equipment, those skilled in the art can be selected and be adjusted 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 is not limited especially the actual temp of the vulcanization
System, with curing temperature in such technique well known to those skilled in the art, those skilled in the art can be according to actual life
Product situation, product requirement and quality requirement are selected and 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 present invention is not particularly limited to the pressure of the vulcanization, with this
Sulfide stress in such technique known to art personnel, those skilled in the art can according to practical condition,
Product requirement and quality requirement are selected and adjusted, and the line pressure of vulcanization of the present invention is preferably 10~16MPa, more preferably
It is 11~15MPa, most preferably 12~14MPa.The present invention is not particularly limited to the time of the vulcanization, with art technology
Cure time in such technique known to personnel, those skilled in the art can be according to practical condition, product requirement
And quality requirement is selected and 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 the integrality and operability of raising preparation process, and baking step is also included 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 be selected according to practical condition, product requirement and quality requirement
Select and adjust, 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, most preferably more preferably 5~9h, 6~8h；This hair
The equipment of the bright drying is preferably drying hole.
Above-mentioned steps of the present invention provide a kind of graphite sealing material and preparation method thereof, the graphite grazing that the present invention is provided
Material does not contain asbestos component, and the prominent characteristic that rear high temperature resistant grade is improved is combined using graphite and rubber, is aided with special ratios
Graphite and rubber, then add other auxiliary agents of particular combination and ratio, and, the present invention for material different qualities, with reference to
The selection of composition and ratio, using hybrid technique in batches step by step, in conjunction with Zhang Gong's skill and other techniques are rolled into, prepares
The graphite sealing material is obtained.Graphite sealing material prepared by the present invention, the high temperature resistance for effectively raising encapsulant is resistance to
Ability, useful life longevity of the lift-off seal material in worst hot case environment, it is ensured that sealing is permanently effective, solves existing asbestos
The environmental protection of class sealed material is not up to standard, rather than the poor problem of sealed material resistance to elevated temperatures.
Test result indicate that, the graphite sealing material for not containing asbestos component prepared by the present invention, temperature in use reaches
260~300 DEG C, compared to 180~250 DEG C of temperature in use of common non-asbestos pad, improve 20%~44%, and with compared with
Good normal temperature and elevated-temperature seal performance, can meet or exceed the standard of correlation.
In order to further illustrate the present invention, a kind of encapsulant to present invention offer and its preparation with reference to embodiments
Method has been described in detail, but it is to be understood that these embodiments are that reality is carried out under premised on technical solution of the present invention
Apply, give detailed implementation method and specific operating process, simply to further illustrate the features and advantages of 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 |
| Accelerator | 0.90 |
| Zinc oxide | 1.80 |
| Plasticizer | 0.50 |
| Age resistor | 0.80 |
| It is total | 4.96 |
| White carbon | 10.00 |
| Kaolin | 13.00 |
| Graphite powder | 45.00 |
| People's dressing is fine | 44.00 |
| Fanglun slurry cake | 10 |
| It is total | 122.00 |
| Amount to | 154.96 |
| Toluene | 85L |
| Alcohol | 22L |
Preparation process：
Operation 1：The mastication of nitrile rubber
By the consumption of formula regulation, 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 standby.
Operation 2：Dispensing
By the consumption that regulation is formulated in table 1, rubber chemicals (tolerance+0.005kg) are weighed：Cosan, accelerator, oxidation
Zinc, plasticizer, age resistor.It is standby；
By other raw material types in table 1, the consumption (tolerance+0.2kg) of regulation is weighed.
Operation 3：Stir material
Equipment：Ploughshare mixer；Rotating speed：Main slurry 105r/min, knife slurry 1800r/min；
Whipping step：
1st step：Add Fanglun slurry cake, graphite powder；Mixing time 8min；
2nd step：Add nitrile rubber, rubber chemicals, kaolin, toluene；Mixing time 58min；
3rd step：Add people's dressing fine；Mixing time：20min；
4th step：Cooling；Temperature fall time：5min；
5th step：Add white carbon；Mixing time 30min；
6th step：Add alcohol；Mixing time 30s；
7th step：Discharging, loads container, standby.
Operation 4：It is rolled into and opens
Equipment：509 one-tenth machines；
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 sheet materials, and material quantity is 30kg；
Operation 5：Vulcanization
Equipment：Drying hole, vulcanizing press；
(1) sheet material is put into drying hole and is dried, the 1st section of vulcanization；Temperature：70 DEG C, time：8h；
(2) will be placed on vulcanizing press by the sheet material of the 1st section of vulcanization, carry out the 2nd section of vulcanization；Temperature：149℃；Pressure
Power：12MPa；Time：10min.
It is finished product sheet material, i.e. graphite grazing lining plank through the sheet material after over cure.
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 test instrument；(4) creep relaxation rate
Test instrument；(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 |
| Accelerator | 0.94 |
| Zinc oxide | 1.50 |
| Plasticizer | 0.90 |
| Age resistor | 0.60 |
| It is total | 5.05 |
| White carbon | 12.00 |
| Carbon black | 5.00 |
| Graphite powder | 50.00 |
| People's dressing is fine | 36.00 |
| Fanglun slurry cake | 15.00 |
| It is total | 118.00 |
| Amount to | 155.05 |
| Toluene | 98L |
| Alcohol | 43L |
Preparation process：
Operation 1：The mastication of hydrogenated nitrile-butadiene rubber
By the consumption of formula regulation, 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 standby.
Operation 2：Dispensing
By the consumption that regulation is formulated in table 1, rubber chemicals (tolerance+0.005kg) are weighed：Cosan, accelerator, oxidation
Zinc, plasticizer, age resistor.It is standby；
By other raw material types in table 1, the consumption (tolerance+0.2kg) of regulation is weighed.
Operation 3：Stir material
Equipment：Ploughshare mixer；Rotating speed：Main slurry 100r/min, knife slurry 1850r/min；
Whipping step：
1st step：Add Fanglun slurry cake, graphite powder；Mixing time 15min；
2nd step：Add nitrile rubber, rubber chemicals, kaolin, carbon black, toluene；Mixing time 62min；
3rd step：Add people's dressing fine；Mixing time：25min；
4th step：Cooling；Temperature fall time：10min；
5th step：Add white carbon；Mixing time 40min；
6th step：Add alcohol；Mixing time 50s；
7th step：Discharging, loads container, standby.
Operation 4：It is rolled into and opens
Equipment：509 one-tenth machines；
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 sheet materials, and material quantity is 8.5kg；
Operation 5：Vulcanization
Equipment：Drying hole, vulcanizing press；
(1) sheet material is put into drying hole and is dried, the 1st section of vulcanization；Temperature：60 DEG C, time：9h；
(2) will be placed on vulcanizing press by the sheet material of the 1st section of vulcanization, carry out the 2nd section of vulcanization；Temperature：145℃；Pressure
Power：15MPa；Time：12min.
It is finished product sheet material, i.e. graphite grazing lining plank through the sheet material after over cure.
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 test instrument；(4) creep relaxation rate
Test instrument；(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：
Operation 1：Dispensing
By the consumption that regulation is formulated in table 1, PNBR (tolerance+0.2kg) is weighed.It is standby；
By the consumption that regulation is formulated in table 1, rubber chemicals (tolerance+0.005kg) are weighed：Cosan, accelerator, oxidation
Zinc, plasticizer, age resistor.It is standby；
By other raw material types in table 1, the consumption (tolerance+0.2kg) of regulation is weighed.
Operation 2：Stir material
Equipment：Ploughshare mixer；Rotating speed：Main slurry 110r/min, knife slurry 1900r/min；
Whipping step：
1st step：Add Fanglun slurry cake, graphite powder；Mixing time 20min；
2nd step：Add nitrile rubber, rubber chemicals, kaolin, carbon black, toluene；Mixing time 68min；
3rd step：Add people's dressing fine；Mixing time：30min；
4th step：Cooling；Temperature fall time：7min；
5th step：Add white carbon；Mixing time 35min；
6th step：Add alcohol；Mixing time 40s；
7th step：Discharging, loads container, standby.
Operation 3：It is rolled into and opens
Equipment：509 one-tenth machines；
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 sheet materials, and material quantity is 8.5kg；
Operation 4：Vulcanization
Equipment：Drying hole, vulcanizing press；
(1) sheet material is put into drying hole and is dried, the 1st section of vulcanization；Temperature：75 DEG C, time：6h；
(2) will be placed on vulcanizing press by the sheet material of the 1st section of vulcanization, carry out the 2nd section of vulcanization；Temperature：147℃；Pressure
Power：15MPa；Time：15min.
It is finished product sheet material, i.e. graphite grazing lining plank through the sheet material after over cure.
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 test instrument；(4) creep relaxation rate
Test instrument；(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 for providing the present invention above and preparation method thereof is described in detail, used herein
Specific case is set forth to principle of the invention and implementation method, and the explanation of above example is only intended to help and understands
The method of the present invention and its core concept, including best mode, and also cause that any person skilled in the art can be real
The present invention is trampled, including is manufactured and is used any device or system, and the method for implementing any combination.It should be pointed out that for this skill
For the those of ordinary skill in art field, under the premise without departing from the principles of the invention, some changing can also be carried out to the present invention
Enter and modify, these are improved and modification is 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
Applying example has the structural element for being not different from claim character express, or if they include the word with claim
Equivalent structural elements of the statement without essence difference, then these other embodiments also should be comprising within the scope of the claims.
Claims (10)
1. a kind of graphite sealing material, it is characterised in that be obtained by including following raw material：
2. graphite sealing material according to claim 1, it is characterised in that the rubber includes nitrile rubber, natural rubber
One or more in glue, butadiene-styrene rubber, neoprene and hydrogenated nitrile-butadiene rubber；
The graphite includes amorphous graphite and/or crystalline flake graphite；
The non-asbestos fiber includes non-asbestos organic fiber and/or non-asbestos inorfil；
Described filler includes reinforced filling；
The rubber chemicals include one or more in vulcanizing agent, accelerator, activating agent, age resistor and plasticizer.
3. graphite sealing material according to claim 2, it is characterised in that the rubber includes the fourth of 5~30 weight portions
The butadiene-styrene rubber of nitrile rubber, the natural rubber of 4~20 weight portions and 5~20 weight portions；
The granularity of the graphite is 45~550 μm；
The non-asbestos fiber includes that Fanglun slurry cake and people's dressing are fine；
Described filler includes one or more in kaolin, carbon black and white carbon；
The rubber chemicals include accounting for the vulcanizing agent of the rubber consumption 1%~5%, accounting for the rush of the rubber consumption 1%~5%
Enter agent, account for the activating agent of the rubber consumption 1%~8% and account for the age resistor of the rubber consumption 1%~5%.
4. a kind of preparation method of graphite sealing material, it is characterised in that comprise 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 is by after roll-in and vulcanization, obtaining encapsulant.
5. preparation method according to claim 4, it is characterised in that the non-asbestos fiber includes non-asbestos organic fiber
With non-asbestos inorfil；
The step 1) it is specially：
11) after non-asbestos organic fiber and graphite being carried out into shredding stirring, just mixed thing is obtained；
12) first mixed thing, rubber, rubber chemicals and solvent that above-mentioned steps are obtained are disperseed, is added the inorganic fibre of non-asbestos
After dimension is disperseed again, cooling obtains mixture；
13) in the mixture for obtaining to above-mentioned steps, after adding filler mixing, add after interleaving agent mixes again, obtain mother
Grain.
6. preparation method according to claim 5, it is characterised 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 the one kind or many in gasoline, toluene, dimethylbenzene, acetone, heptane, MEK, ethyl acetate and butanone
Kind；
The interleaving agent includes ethanol.
7. the preparation method according to claim 5 or 6, it is characterised in that the time of the shredding stirring is 5~20min；
The scattered time is 50~180min；
The scattered time is 20~60min；
The time of the cooling is 1~30min；
The time of the mixing is 5~60min；
The time for mixing again is 5~60s.
8. preparation method according to claim 4, it is characterised in that also include baking step before the vulcanization；
The temperature of the drying is 60~100 DEG C；
The time of the drying is 4~10h.
9. preparation method according to claim 8, it is characterised 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.
10. preparation method according to claim 8 or claim 9, it is characterised 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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| CN108953608A (en) * | 2018-08-24 | 2018-12-07 | 宁波灏印燃气用具有限公司 | A kind of graphite-based composite seal 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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| CN106700154B (en) | 2018-11-06 |
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