CN110818971A - Sealing gasket and preparation method thereof - Google Patents
Sealing gasket and preparation method thereof Download PDFInfo
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- CN110818971A CN110818971A CN201911252124.8A CN201911252124A CN110818971A CN 110818971 A CN110818971 A CN 110818971A CN 201911252124 A CN201911252124 A CN 201911252124A CN 110818971 A CN110818971 A CN 110818971A
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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
- C08L9/06—Copolymers with styrene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D99/00—Subject matter not provided for in other groups of this subclass
- B29D99/0053—Producing sealings
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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
- C08K2201/011—Nanostructured additives
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- 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
Abstract
The invention discloses a sealing gasket which is prepared from the following components in parts by weight: 50-60 parts of styrene-butadiene rubber, 30-40 parts of epoxy acrylate rubber, 5-10 parts of oxidized paraffin, 5-10 parts of amino silicone oil, 20-25 parts of thiol group fluorosilicone acrylate polymer, 10-15 parts of graphene oxide fiber, 1-5 parts of Kevlar fiber, 1-5 parts of organic zinc surface modified zinc oxide nano fiber and 1-3 parts of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate. The invention also discloses a preparation method of the sealing gasket. The sealing gasket disclosed by the invention has the advantages of good sealing effect, simple production process, good wear resistance and corrosion resistance, excellent anti-creep and thermal aging resistance, safety and environmental protection in use and long service life.
Description
Technical Field
The invention relates to the technical field of sealing materials, in particular to a sealing gasket and a preparation method thereof.
Background
The sealing gasket is a key element for maintaining the sealing effect in the bolt flange connection, and is widely applied to process industrial devices such as pressure vessels, process equipment, power machines, connecting pipelines and the like, and the failure of the sealing gasket can bring disastrous results. It is usually made of metal or non-metal plate material, and is made up by using such processes of cutting, punching or cutting, etc. and can be used for sealing connection between pipelines and between machine parts. With the continuous development of industrial technology, increasingly stringent requirements are placed on the pressure resistance, high temperature resistance, corrosion resistance, sealing resilience and other properties of the sealing gasket, and the research on the novel sealing gasket has become a hotspot in industrial research.
The existing common sealing gasket mainly comprises a metal sealing gasket, an asbestos sealing gasket and a rubber sealing gasket. The metal sealing gasket has limited compression resilience performance and narrow application range, and the residual deformation generated after the bolt is loosened cannot ensure reliable and effective sealing pressing force and has the defect of easy corrosion. The asbestos sealing gasket pollutes the environment and is harmful to the health of human bodies, and the product has poor resistance to creep and thermal aging, poor flexibility, small compactness, poor sealing property and easy fracturing in the installation process. Rubber sealing gasket is a kind of sealing gasket that uses more and more at present, but the sealing gasket tensile strength among the prior art is lower, and creep relaxation resistance is relatively poor, and ageing resistance needs further improvement, in addition, its wearability, elasticity and mechanical properties are more and more not satisfied the demand.
The Chinese patent with patent number 200410015794.5 discloses a manufacturing and forming process method of a non-asbestos fiber reinforced latex sealing gasket plate, which comprises the steps of raw material preparation, namely preparation and formula of a plurality of raw material components such as non-asbestos fiber, rubber emulsion, a cross-linking agent, a filler, an auxiliary additive and the like, treatment of the non-asbestos fiber, preparation of the emulsion, preparation of suspension, sheet making and forming, drying and rolling vulcanization, and is characterized in that: the special raw material components are adopted, but the procedure is too complex, and the quality of the obtained sealing gasket still has problems.
Therefore, the novel sealing gasket which has the advantages of good sealing effect, simple production process, good wear-resisting and corrosion-resisting properties, excellent anti-creep and thermal aging resistance and long service life is developed, meets the market demand, has wide market value and application prospect, and plays an important role in promoting the development of the sealing element industry.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the sealing gasket and the preparation method thereof, and the preparation method has the advantages of simple process, easy operation, easily obtained raw materials, low manufacturing cost, low dependence on equipment and suitability for large-scale production; the prepared sealing gasket overcomes the technical problems that the traditional rubber sealing gasket is low in tensile strength, poor in creep relaxation resistance, low in ageing resistance, and poor in wear resistance, elasticity and mechanical property, and the requirements cannot be met more and more, and has the advantages of being good in sealing effect, simple in production process, good in wear resistance and corrosion resistance, excellent in creep relaxation resistance and thermal aging resistance, safe and environment-friendly in use, and long in service life.
In order to achieve the aim, the invention adopts the technical scheme that the sealing gasket is prepared from the following components in parts by weight: 50-60 parts of styrene-butadiene rubber, 30-40 parts of epoxy acrylate rubber, 5-10 parts of oxidized paraffin, 5-10 parts of amino silicone oil, 20-25 parts of thiol group fluorosilicone acrylate polymer, 10-15 parts of graphene oxide fiber, 1-5 parts of Kevlar fiber, 1-5 parts of organic zinc surface modified zinc oxide nano fiber and 1-3 parts of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate.
Further, the preparation method of the thiol group fluorosilicone acrylate polymer comprises the following steps: adding 6- (4-vinylbenzyl-n-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, methyl (1-trimethylsilyl) acrylate, trifluoroethyl acrylate, trans-6-octadecenoic acid, an initiator and boron trifluoride into a high boiling point solvent, stirring and reacting for 3-5 hours at 70-80 ℃ in the atmosphere of nitrogen or inert gas, then precipitating in water, washing the precipitated product with ethanol for 3-5 times, extruding to remove ethanol, drying with a dryer, and packaging to obtain the thiol fluorosilicone acrylate polymer.
Preferably, the mass ratio of the 6- (4-vinylbenzyl-n-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, methyl (1-trimethylsilyl) acrylate, trifluoroethyl acrylate, trans-6-octadecenoic acid, initiator, boron trifluoride and high boiling point solvent is 1:1:1:0.2 (0.01-0.03):0.02 (10-15).
Preferably, the initiator is selected from one or more of azobisisobutyronitrile, azobisisoheptonitrile and potassium persulfate.
Preferably, the high boiling point solvent is selected from one or more of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone.
Preferably, the inert gas is selected from one of helium, neon and argon.
Further, the preparation method of the organic zinc surface modified zinc oxide nanofiber comprises the following steps:
i, dispersing zinc oxide nano fibers in ethanol, adding 2- (trimethoxysilyl) ethanethiol, stirring and reacting at 60-80 ℃ for 8-10 hours, centrifuging, and drying in a vacuum drying oven at 80-90 ℃ to constant weight to obtain an intermediate product;
and II, adding the intermediate product prepared in the step I and a catalyst into tetrahydrofuran, adding zinc acetylacetonate at the temperature of 90-100 ℃, stirring at a constant temperature for reaction for 15-18 hours, performing rotary centrifugation after the reaction is finished, washing with acetone for 3-5 times, and drying in a vacuum drying oven at the temperature of 75-85 ℃ to constant weight.
Preferably, the mass ratio of the zinc oxide nano-fibers, the ethanol and the 2- (trimethoxysilyl) ethanethiol in the step I is (3-5): (10-15): 1.
Preferably, the mass ratio of the intermediate product, the catalyst, the tetrahydrofuran and the zinc acetylacetonate in the step II is (2-4): 0.5-1): 6-10): 0.8.
Preferably, the catalyst is selected from one or more of n-propylamine, diethylamine, dimethylphenylphosphonium and tetrabutylammonium bromide.
Further, the preparation method of the sealing gasket comprises the following steps: sequentially adding the raw materials into an internal mixer according to the formula, mixing for 7-10 minutes at 60-70 ℃, sealing and standing for 20-30 minutes, and then putting into a preforming machine for strip forming to form a glue material; and then, carrying out milling molding on the rubber material at 60-70 ℃ through an open mill, putting the molded rubber material into a mold of vulcanization equipment, carrying out vulcanization treatment, finally trimming, and inspecting the size and the appearance to obtain the finished product sealing gasket.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
the sealing gasket provided by the invention has the advantages of simple and easily-operated preparation method, easily-obtained raw materials, low manufacturing cost and low dependence on equipment, and is suitable for large-scale production.
The sealing gasket provided by the invention overcomes the technical problems that the traditional rubber sealing gasket is low in tensile strength, poor in creep relaxation resistance, low in ageing resistance, and poor in wear resistance, elasticity and mechanical property, and the requirements cannot be met more and more, and has the advantages of good sealing effect, simple production process, good wear resistance and corrosion resistance, excellent creep relaxation resistance and thermal aging resistance, safety and environmental friendliness in use, and long service life.
The sealing gasket provided by the invention adopts the blending of the modified styrene-butadiene rubber, the epoxy acrylate rubber and the thiol-based fluorosilicone acrylate polymer as a base material, combines the excellent characteristics of the modified styrene-butadiene rubber, has excellent resilience sealing property and wear resistance, and chemically reacts with an epoxy group on the epoxy acrylate rubber by adding the amino silicone oil and the oxidized paraffin to form a three-dimensional network structure, so that the material has more excellent heat resistance, wear resistance and mechanical property, and further improves the weather resistance and corrosion resistance of the material by introducing a fluorosilicone and triazole structure through reaction, and the number of double bonds on a molecular chain of the styrene-butadiene rubber is reduced due to the addition of thiol, so that the aging resistance and stability of the material are improved; the grafting of the amino silicone oil and the oxidized paraffin improves the self-lubricating property, thereby improving the wear resistance and the creep resistance of the material.
According to the sealing gasket provided by the invention, the graphene oxide fiber, the Kevlar fiber and the organic zinc surface modified zinc oxide nanofiber are added at the same time, so that a synergistic effect is achieved, the mechanical property and the sealing effect of the sealing gasket are improved, the sealing effect of the material is better due to the introduction of the nanomaterial, the amino silicone oil and the paraffin structure, the activity of the zinc oxide nanofiber is higher due to the organic zinc surface modification, and the heat conductivity, the wear resistance, the tear resistance and the tensile strength of the product are improved.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
The graphene oxide fibers used in the following embodiments of the present invention are prepared in advance, and the preparation method refers to chinese patent CN 106087114 a; the zinc oxide nano fiber is prepared in advance, and the preparation method refers to the following steps: preparation of zinc oxide nano-fiber and photocatalytic performance thereof, Shu Yan and the like, textile bulletin, 32(3), 2011; other raw materials were all purchased commercially.
Example 1
A sealing gasket is prepared from the following components in parts by weight: 50 parts of styrene-butadiene rubber, 30 parts of epoxy acrylate rubber, 5 parts of oxidized paraffin, 5 parts of amino silicone oil, 20 parts of thiol group fluorosilicone acrylate polymer, 10 parts of graphene oxide fiber, 1 part of Kevlar fiber, 1 part of organic zinc surface modified zinc oxide nano fiber and 1 part of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate.
The preparation method of the thiol group fluorosilicone acrylate polymer comprises the following steps: adding 1kg of 6- (4-vinylbenzyl-n-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, 1kg of methyl (1-trimethylsilyl) acrylate, 1kg of trifluoroethyl acrylate, 0.2kg of trans-6-octadecenoic acid, 0.01kg of azodiisobutyronitrile and 0.02kg of boron trifluoride into 10kg of dimethyl sulfoxide, stirring and reacting for 3 hours at 70 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated product with ethanol for 3 times, extruding to remove the ethanol, drying with a dryer, and packaging to obtain the thiol fluorosilicone acrylate polymer.
The preparation method of the organic zinc surface modified zinc oxide nanofiber comprises the following steps:
i, dispersing 3kg of zinc oxide nano fiber in 10kg of ethanol, then adding 1kg of 2- (trimethoxysilyl) ethanethiol, stirring and reacting for 8 hours at 60 ℃, centrifuging, and drying in a vacuum drying oven at 80 ℃ to constant weight to obtain an intermediate product;
II, adding 2kg of the intermediate product prepared in the step I and 0.5kg of n-propylamine into 6kg of tetrahydrofuran, adding 0.8kg of zinc acetylacetonate at 90 ℃, stirring at a constant temperature for reaction for 15 hours, performing rotary centrifugation after the reaction is finished, washing for 3 times by using acetone, and drying in a vacuum drying oven at 75 ℃ to constant weight.
The preparation method of the sealing gasket comprises the following steps: sequentially adding the raw materials into an internal mixer according to the formula, mixing for 7 minutes at 60 ℃, sealing and standing for 20 minutes, and then putting into a preforming machine for strip forming to form a gel material; and then carrying out open milling molding on the rubber material at 60 ℃ through an open mill, putting the molded rubber material into a mold of vulcanization equipment, carrying out vulcanization treatment, finally trimming, and inspecting the size and the appearance to obtain the finished product sealing gasket.
Example 2
A sealing gasket is prepared from the following components in parts by weight: 53 parts of styrene-butadiene rubber, 33 parts of epoxy acrylate rubber, 6 parts of oxidized paraffin, 6 parts of amino silicone oil, 21 parts of thiol group fluorosilicone acrylate polymer, 11 parts of graphene oxide fiber, 2 parts of Kevlar fiber, 2 parts of organic zinc surface modified zinc oxide nano fiber and 2 parts of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate.
The preparation method of the thiol group fluorosilicone acrylate polymer comprises the following steps: adding 1kg of 6- (4-vinylbenzyl-N-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, 1kg of methyl (1-trimethylsilyl) acrylate, 1kg of trifluoroethyl acrylate, 0.2kg of trans-6-octadecenoic acid, 0.015kg of azodiisoheptanonitrile and 0.02kg of boron trifluoride into 11.5kg of N, N-dimethylformamide, stirring and reacting for 3.5 hours at 73 ℃ under the atmosphere of helium, then precipitating in water, washing the precipitated product with ethanol for 4 times, then extruding to remove the ethanol, drying with a dryer, and packaging to obtain the thiol group fluorosilicone acrylate polymer.
The preparation method of the organic zinc surface modified zinc oxide nanofiber comprises the following steps:
dispersing 3.5kg of zinc oxide nano fiber in 12kg of ethanol, then adding 1kg of 2- (trimethoxysilyl) ethanethiol, stirring and reacting for 8.5 hours at 65 ℃, centrifuging, and drying in a vacuum drying oven at 83 ℃ to constant weight to obtain an intermediate product;
II, adding 2.5kg of intermediate product obtained in the step I and 0.7kg of diethylamine into 7.5kg of tetrahydrofuran, adding 0.8kg of zinc acetylacetonate at 93 ℃, stirring at constant temperature for reaction for 16 hours, carrying out rotary centrifugation after the reaction is finished, washing with acetone for 4 times, and then placing in a vacuum drying oven for drying at 78 ℃ to constant weight.
The preparation method of the sealing gasket comprises the following steps: sequentially adding the raw materials into an internal mixer according to the formula, mixing for 8 minutes at 63 ℃, sealing and standing for 23 minutes, and then putting into a preforming machine for strip forming to form a gel material; and then, carrying out open milling molding on the rubber material at 63 ℃ through an open mill, putting the molded rubber material into a mold of vulcanization equipment, carrying out vulcanization treatment, finally trimming, and inspecting the size and the appearance to obtain the finished product sealing gasket.
Example 3
A sealing gasket is prepared from the following components in parts by weight: 55 parts of styrene-butadiene rubber, 35 parts of epoxy acrylate rubber, 8 parts of oxidized paraffin, 8 parts of amino silicone oil, 23 parts of thiol group fluorosilicone acrylate polymer, 13 parts of graphene oxide fiber, 3 parts of Kevlar fiber, 3 parts of organic zinc surface modified zinc oxide nano fiber and 2 parts of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate.
The preparation method of the thiol group fluorosilicone acrylate polymer comprises the following steps: adding 1kg of 6- (4-vinylbenzyl-N-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, 1kg of methyl (1-trimethylsilyl) acrylate, 1kg of trifluoroethyl acrylate, 0.2kg of trans-6-octadecenoic acid, 0.02kg of potassium persulfate and 0.02kg of boron trifluoride into 13kg of N-methylpyrrolidone, stirring and reacting for 4 hours at 75 ℃ under a neon atmosphere, then precipitating in water, washing the precipitated product with ethanol for 4 times, extruding to remove the ethanol, drying with a dryer, and packaging to obtain the thiol group fluorosilicone acrylate polymer.
The preparation method of the organic zinc surface modified zinc oxide nanofiber comprises the following steps:
i, dispersing 4kg of zinc oxide nano fiber in 13kg of ethanol, then adding 1kg of 2- (trimethoxysilyl) ethanethiol, stirring and reacting for 9 hours at 70 ℃, centrifuging, and drying in a vacuum drying oven at 85 ℃ to constant weight to obtain an intermediate product;
II, adding 3kg of intermediate product obtained in the step I and 0.8kg of dimethylphenylphosphine into 8.5kg of tetrahydrofuran, adding 0.8kg of zinc acetylacetonate at 95 ℃, stirring at constant temperature for reaction for 17 hours, performing rotary centrifugation after the reaction is finished, washing with acetone for 4 times, and drying in a vacuum drying oven at 79 ℃ to constant weight.
The preparation method of the sealing gasket comprises the following steps: sequentially adding the raw materials into an internal mixer according to the formula, mixing for 8 minutes at 65 ℃, sealing and standing for 25 minutes, and then putting into a preforming machine for strip forming to form a gel material; and then, carrying out milling molding on the rubber material at 65 ℃ through an open mill, putting the molded rubber material into a mold of vulcanization equipment, carrying out vulcanization treatment, finally trimming, and inspecting the size and the appearance to obtain the finished product sealing gasket.
Example 4
A sealing gasket is prepared from the following components in parts by weight: 58 parts of styrene-butadiene rubber, 38 parts of epoxy acrylate rubber, 9 parts of oxidized paraffin, 9 parts of amino silicone oil, 24 parts of thiol group fluorosilicone acrylate polymer, 14 parts of graphene oxide fiber, 4 parts of Kevlar fiber, 5 parts of organic zinc surface modified zinc oxide nano fiber and 2 parts of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate.
The preparation method of the thiol group fluorosilicone acrylate polymer comprises the following steps: adding 1kg of 6- (4-vinylbenzyl-n-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, 1kg of methyl (1-trimethylsilyl) acrylate, 1kg of trifluoroethyl acrylate, 0.2kg of trans-6-octadecenoic acid, 0.025kg of an initiator and 0.02kg of boron trifluoride into 14.5kg of a high boiling point solvent, stirring and reacting for 4.5 hours at 78 ℃ under an argon atmosphere, then precipitating in water, washing the precipitated product with ethanol for 5 times, extruding to remove the ethanol, drying with a dryer, and packaging to obtain the thiol group fluorosilicone acrylate polymer; the initiator is a mixture formed by mixing azodiisobutyronitrile, azodiisoheptonitrile and potassium persulfate according to the mass ratio of 2:1: 3; the high-boiling-point solvent is a mixture formed by mixing dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone according to the mass ratio of 1:3: 1.
The preparation method of the organic zinc surface modified zinc oxide nanofiber comprises the following steps:
i, dispersing 4.5kg of zinc oxide nano fiber in 14.5kg of ethanol, then adding 1kg of 2- (trimethoxysilyl) ethanethiol, stirring and reacting for 9.5 hours at 75 ℃, centrifuging, placing in a vacuum drying oven at 89 ℃, and drying to constant weight to obtain an intermediate product;
II, adding 3.5kg of the intermediate product prepared in the step I and 0.9kg of catalyst into 9.5kg of tetrahydrofuran, adding 0.8kg of zinc acetylacetonate at the temperature of 99 ℃, stirring at a constant temperature for reacting for 17.5 hours, performing rotary centrifugation after the reaction is finished, washing for 5 times by using acetone, and then placing in a vacuum drying oven for drying at 83 ℃ to constant weight; the catalyst is a mixture formed by mixing n-propylamine, diethylamine, dimethylphenyl phosphorus and tetrabutylammonium bromide according to a mass ratio of 4:2:3: 1.
The preparation method of the sealing gasket comprises the following steps: sequentially adding the raw materials into an internal mixer according to the formula, mixing for 9 minutes at 69 ℃, sealing and standing for 29 minutes, and then putting into a preforming machine for strip forming to form a gel material; and then, carrying out open milling molding on the rubber material at 69 ℃ through an open mill, putting the molded rubber material into a mold of vulcanization equipment, carrying out vulcanization treatment, finally trimming, and inspecting the size and the appearance to obtain the finished product sealing gasket.
Example 5
A sealing gasket is prepared from the following components in parts by weight: 60 parts of styrene-butadiene rubber, 40 parts of epoxy acrylate rubber, 10 parts of oxidized paraffin, 10 parts of amino silicone oil, 25 parts of thiol group fluorosilicone acrylate polymer, 15 parts of graphene oxide fiber, 5 parts of Kevlar fiber, 5 parts of organic zinc surface modified zinc oxide nano fiber and 3 parts of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate.
The preparation method of the thiol group fluorosilicone acrylate polymer comprises the following steps: adding 1kg of 6- (4-vinylbenzyl-N-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, 1kg of methyl (1-trimethylsilyl) acrylate, 1kg of trifluoroethyl acrylate, 0.2kg of trans-6-octadecenoic acid, 0.03kg of azodiisobutyronitrile and 0.02kg of boron trifluoride into 15kg of N, N-dimethylformamide, stirring and reacting for 5 hours at 80 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated product with ethanol for 5 times, extruding to remove the ethanol, drying with a dryer, and packaging to obtain the thiol group fluorosilicone acrylate polymer.
The preparation method of the organic zinc surface modified zinc oxide nanofiber comprises the following steps:
i, dispersing 5kg of zinc oxide nano fiber in 15kg of ethanol, then adding 1kg of 2- (trimethoxysilyl) ethanethiol, stirring and reacting for 10 hours at 80 ℃, centrifuging, and drying in a vacuum drying oven at 90 ℃ to constant weight to obtain an intermediate product;
II, adding 4kg of the intermediate product prepared in the step I and 1kg of tetrabutylammonium bromide into 10kg of tetrahydrofuran, adding 0.8kg of zinc acetylacetonate at 100 ℃, stirring at a constant temperature for reacting for 18 hours, performing rotary centrifugation after the reaction is finished, washing for 5 times by using acetone, and then placing in a vacuum drying oven for drying at 85 ℃ to constant weight.
The preparation method of the sealing gasket comprises the following steps: sequentially adding the raw materials into an internal mixer according to the formula, mixing for 10 minutes at 70 ℃, sealing and standing for 30 minutes, and then putting into a preforming machine for strip forming to form a gel material; and then, carrying out refining molding on the rubber material at 70 ℃ through an open mill, putting the molded rubber material into a mold of vulcanization equipment, carrying out vulcanization treatment, finally trimming, and inspecting the size and the appearance to obtain the finished product sealing gasket.
Comparative example 1
This example provides a gasket seal formulation and method of preparation similar to example 1 except that no mercaptofluorosilicone acrylate polymer is added.
Comparative example 2
This example provides a gasket seal formulation and method of manufacture similar to example 1, except that no epoxy acrylate rubber is added.
Comparative example 3
This example provides a gasket seal similar in formulation and preparation to example 1 except that no graphene oxide fibers were added.
Comparative example 4
This example provides a gasket seal, the formulation and preparation method of which are similar to those of example 1, except that zinc oxide nanofibers are used to replace organic zinc surface modified zinc oxide nanofibers.
Comparative example 5
This example provides a gasket seal formulation and method of preparation similar to example 1 except that no aminosilicone is added.
Comparative example 6
This example provides a sealing gasket, the formulation and preparation method of which are the same as those of embodiment 1 of the Chinese patent CN 106867448A.
The performance of the gaskets prepared in examples 1-5 and comparative examples 1-6 was tested, and the test methods and results are shown in table 1.
TABLE 1
| Item | Rebound resilience | Tensile strength | High temperature resistance | Hot air aging | Leakage rate |
| Unit of | ％ | KN/mm | ℃ | h | mg/m.s |
| Test standard | ASTMF36 | ASTMD412 | EN344 | GB/T2941 | DNIN28091 |
| Example 1 | 79.3 | 25.5 | 345 | 352 | 2.3 |
| Example 2 | 79.5 | 25.7 | 347 | 355 | 2.2 |
| Example 3 | 79.7 | 25.9 | 349 | 357 | 2.0 |
| Example 4 | 79.8 | 26.1 | 351 | 359 | 1.8 |
| Example 5 | 80.1 | 26.3 | 353 | 362 | 1.6 |
| Comparative example 1 | 69.5 | 19.2 | 302 | 326 | 3.2 |
| Comparative example 2 | 68.6 | 19.1 | 305 | 328 | 3.3 |
| Comparative example 3 | 66.9 | 20.0 | 305 | 325 | 2.9 |
| Comparative example 4 | 67.3 | 19.5 | 299 | 330 | 3.0 |
| Comparative example 5 | 69.9 | 19.1 | 303 | 329 | 3.2 |
| Comparative example 6 | 60.0 | 13.3 | 280 | 320 | 4.0 |
As can be seen from table 1, the sealing gasket disclosed in the embodiment of the present invention has more excellent sealing resilience, high temperature resistance, aging resistance, and tensile property, compared to the sealing gasket in the prior art.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A sealing gasket is characterized by being prepared from the following components in parts by weight: 50-60 parts of styrene-butadiene rubber, 30-40 parts of epoxy acrylate rubber, 5-10 parts of oxidized paraffin, 5-10 parts of amino silicone oil, 20-25 parts of thiol group fluorosilicone acrylate polymer, 10-15 parts of graphene oxide fiber, 1-5 parts of Kevlar fiber, 1-5 parts of organic zinc surface modified zinc oxide nano fiber and 1-3 parts of bis (3-trimethoxysilylpropyl) (E) -butyl-2-enedioate.
2. A gasket seal according to claim 1, wherein said preparation method of said thiol-fluorosilicone acrylate polymer comprises the steps of: adding 6- (4-vinylbenzyl-n-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, methyl (1-trimethylsilyl) acrylate, trifluoroethyl acrylate, trans-6-octadecenoic acid, an initiator and boron trifluoride into a high boiling point solvent, stirring and reacting for 3-5 hours at 70-80 ℃ in the atmosphere of nitrogen or inert gas, then precipitating in water, washing the precipitated product with ethanol for 3-5 times, extruding to remove ethanol, drying with a dryer, and packaging to obtain the thiol fluorosilicone acrylate polymer.
3. A sealing gasket according to claim 2, wherein the mass ratio of 6- (4-vinylbenzyl-n-propyl) amino-1, 3, 5-triazine-2, 4-dithiol, methyl (1-trimethylsilyl) acrylate, trifluoroethyl acrylate, trans-6-octadecenoic acid, initiator, boron trifluoride and high boiling point solvent is 1:1:1:0.2 (0.01-0.03):0.02 (10-15).
4. A sealing gasket according to claim 2, wherein said initiator is selected from one or more of azobisisobutyronitrile, azobisisoheptonitrile, and potassium persulfate; the high boiling point solvent is selected from one or more of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone; the inert gas is selected from helium, neon and argon.
5. The gasket seal of claim 1, wherein the preparation method of the organic zinc surface modified zinc oxide nanofiber comprises the following steps:
i, dispersing zinc oxide nano fibers in ethanol, adding 2- (trimethoxysilyl) ethanethiol, stirring and reacting at 60-80 ℃ for 8-10 hours, centrifuging, and drying in a vacuum drying oven at 80-90 ℃ to constant weight to obtain an intermediate product;
and II, adding the intermediate product prepared in the step I and a catalyst into tetrahydrofuran, adding zinc acetylacetonate at the temperature of 90-100 ℃, stirring at a constant temperature for reaction for 15-18 hours, performing rotary centrifugation after the reaction is finished, washing with acetone for 3-5 times, and drying in a vacuum drying oven at the temperature of 75-85 ℃ to constant weight.
6. A sealing gasket according to claim 5, wherein the mass ratio of said zinc oxide nanofibers, ethanol, and 2- (trimethoxysilyl) ethanethiol in step I is (3-5): (10-15): 1.
7. A sealing gasket according to claim 5, wherein in step II the mass ratio of the intermediate product, the catalyst, the tetrahydrofuran and the zinc acetylacetonate is (2-4): 0.5-1): 6-10): 0.8.
8. A sealing gasket according to claim 5, wherein said catalyst is selected from one or more of n-propylamine, diethylamine, dimethylphenylphosphine, tetrabutylammonium bromide.
9. A gasket seal according to any of claims 1 to 8, wherein said gasket seal is prepared by a process comprising the steps of: sequentially adding the raw materials into an internal mixer according to the formula, mixing for 7-10 minutes at 60-70 ℃, sealing and standing for 20-30 minutes, and then putting into a preforming machine for strip forming to form a glue material; and then, carrying out milling molding on the rubber material at 60-70 ℃ through an open mill, putting the molded rubber material into a mold of vulcanization equipment, carrying out vulcanization treatment, finally trimming, and inspecting the size and the appearance to obtain the finished product sealing gasket.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911252124.8A CN110818971A (en) | 2019-12-09 | 2019-12-09 | Sealing gasket and preparation method thereof |
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| CN201911252124.8A CN110818971A (en) | 2019-12-09 | 2019-12-09 | Sealing gasket and preparation method thereof |
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| CN110818971A true CN110818971A (en) | 2020-02-21 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114316492A (en) * | 2022-01-19 | 2022-04-12 | 慈溪埃弗龙密封件有限公司 | Long-life toothed plate reinforced high-strength graphite gasket and preparation method thereof |
| CN114805963A (en) * | 2021-06-26 | 2022-07-29 | 上海西尔福斯特密封件有限公司 | Environment-friendly nontoxic sealing gasket and preparation method thereof |
-
2019
- 2019-12-09 CN CN201911252124.8A patent/CN110818971A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805963A (en) * | 2021-06-26 | 2022-07-29 | 上海西尔福斯特密封件有限公司 | Environment-friendly nontoxic sealing gasket and preparation method thereof |
| CN114805963B (en) * | 2021-06-26 | 2024-02-09 | 上海西尔福斯特密封件有限公司 | Environment-friendly nontoxic sealing gasket and preparation method thereof |
| CN114316492A (en) * | 2022-01-19 | 2022-04-12 | 慈溪埃弗龙密封件有限公司 | Long-life toothed plate reinforced high-strength graphite gasket and preparation method thereof |
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