CN116462924A - Low-temperature-resistant fluorine rubber and preparation method thereof - Google Patents
Low-temperature-resistant fluorine rubber and preparation method thereof Download PDFInfo
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 36
- 239000011737 fluorine Substances 0.000 title claims abstract description 36
- 239000006229 carbon black Substances 0.000 claims abstract description 66
- 229920001973 fluoroelastomer Polymers 0.000 claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 32
- 239000000945 filler Substances 0.000 claims abstract description 29
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 27
- 239000013543 active substance Substances 0.000 claims abstract description 23
- ZBSKZKPSSKTLNE-UHFFFAOYSA-N 4-methylpent-3-enoxysilane Chemical compound CC(=CCCO[SiH3])C ZBSKZKPSSKTLNE-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000314 lubricant Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004014 plasticizer Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims description 44
- 239000002245 particle Substances 0.000 claims description 34
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 18
- 239000011787 zinc oxide Substances 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 15
- 230000003712 anti-aging effect Effects 0.000 claims description 10
- 239000001913 cellulose Substances 0.000 claims description 9
- 229920002678 cellulose Polymers 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- JEWCZPTVOYXPGG-UHFFFAOYSA-N ethenyl-ethoxy-dimethylsilane Chemical compound CCO[Si](C)(C)C=C JEWCZPTVOYXPGG-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 6
- 229960002447 thiram Drugs 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- 150000003751 zinc Chemical class 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical group C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application relates to the technical field of rubber materials, and particularly discloses a low-temperature-resistant fluorine rubber and a preparation method thereof. The low-temperature-resistant fluorine rubber comprises the following raw materials in parts by weight: 50-70 parts of fluororubber, 30-50 parts of ethylene propylene diene monomer rubber, 10-20 parts of modified filler, 2-5 parts of active agent, 1-2 parts of flow aid, 0.5-1.5 parts of release agent, 55-65 parts of reinforcing agent, 10-15 parts of lubricant, 10-15 parts of plasticizer, 2-5 parts of vulcanizing agent and 4-5 parts of accelerator; the raw materials of the modified filler comprise dimethylvinylethoxysilane, ethanol and white carbon black. In the application, fluororubber and ethylene propylene diene monomer rubber are blended, and the dimethyl vinyl ethoxy silane is used for modifying the white carbon black, so that the white carbon black can be uniformly dispersed in the system, and the low temperature resistance of the fluororubber is improved.
Description
Technical Field
The application relates to the technical field of rubber materials, in particular to low-temperature-resistant fluorine rubber and a preparation method thereof.
Background
Fluororubber is a synthetic polymer elastomer containing fluorine atoms on carbon atoms of a main chain or a side chain, and introduction of fluorine atoms imparts excellent heat resistance, oxidation resistance, oil resistance, corrosion resistance and aging resistance to rubber. However, the low temperature resistance of fluororubber is poor, and the fluororubber can only reach about-20 ℃ at most, so that the fluororubber cannot be used in various fields with high reliability requirements such as automobiles, aviation and the like.
Disclosure of Invention
In order to improve the low temperature resistance of fluororubber, the application provides low temperature resistant fluororubber and a preparation method thereof.
In a first aspect, the application provides a low temperature resistant fluorine gum, which adopts the following technical scheme:
the low-temperature-resistant fluorine rubber comprises the following raw materials in parts by weight: 50 to 70 parts of fluororubber, 30 to 50 parts of ethylene propylene diene monomer rubber, 10 to 20 parts of modified filler, 2 to 5 parts of active agent, 1 to 2 parts of flow aid, 0.5 to 1.5 parts of release agent, 55 to 65 parts of reinforcing agent, 10 to 15 parts of lubricant, 10 to 15 parts of plasticizer, 2 to 5 parts of vulcanizing agent and 4 to 5 parts of accelerator; the raw materials of the modified filler comprise dimethylvinylethoxysilane, ethanol and white carbon black.
By adopting the technical scheme, the fluororubber and the ethylene propylene diene monomer are blended, so that the prepared fluororubber has the low temperature resistance of the ethylene propylene diene monomer; the white carbon black is modified by using the dimethylvinylethoxysilane, so that the white carbon black can be uniformly dispersed in a system, and the low temperature resistance of the fluororubber is improved under the cooperation of the ethylene propylene diene monomer rubber and the white carbon black.
In a specific embodiment, the method of preparing the modified filler comprises the steps of:
uniformly stirring and mixing dimethylvinylethoxysilane, ethanol and water to obtain a modified liquid; and stirring the white carbon black, spraying the modified liquid on the white carbon black in the stirring process, and drying to obtain the modified filler.
By adopting the technical scheme, the dimethyl vinyl ethoxy silane is firstly dissolved in the ethanol and then sprayed on the white carbon black, so that the white carbon black is modified, and the modified filler is obtained.
In a specific embodiment, the weight ratio of the dimethylvinylethoxysilane to the white carbon black is 1: (60-70).
By adopting the technical scheme, the proportion of the dimethylvinylethoxysilane to the white carbon black is further limited, so that the dimethylvinylethoxysilane can better coat the white carbon black, and the modification effect on the white carbon black is improved.
In a specific embodiment, the weight ratio of the ethylene propylene diene monomer rubber to the fluororubber is 1: (1.4-1.6).
By adopting the technical scheme, the proportion of the ethylene propylene diene monomer rubber and the fluororubber is further limited, so that the prepared fluororubber has good low temperature resistance and high temperature resistance.
In a specific embodiment, the active agent comprises a mixture of zinc oxide and SA.
By adopting the technical scheme, zinc oxide and SA can react to generate zinc salt, which is beneficial to promoting the vulcanization of rubber.
In a specific embodiment, the reinforcing agent comprises a mixture of large particle carbon black, small particle carbon black, cellulose.
By adopting the technical scheme, the small-particle carbon black has smaller particle size, better dispersion performance and better reinforcing effect, but the prepared rubber has poor pressure change performance; the large-particle carbon black has larger particle size, so that the pressure change performance of the rubber can be improved; the addition of cellulose can improve the wear resistance and high temperature resistance of rubber.
In a specific embodiment, the starting materials for the fluororubber further comprise 0.1 to 1 part by weight of an anti-aging agent and 5 to 7 parts by weight of an anti-wear agent.
By adopting the technical scheme, the anti-aging agent and the anti-wear agent are added, so that the anti-aging performance and the wear resistance of the prepared rubber can be further improved.
In a second aspect, the preparation method of the low-temperature-resistant fluorine rubber provided by the application adopts the following technical scheme:
the preparation method of the low-temperature-resistant fluorine rubber comprises the following steps:
plasticating and mixing fluororubber and ethylene propylene diene monomer rubber to obtain a mixture A;
adding part of modified filler, an active agent, a flow aid, a release agent, part of reinforcing agent, a lubricant, an anti-aging agent and an anti-wear agent into the mixture A, and mixing to 90-110 ℃ to obtain a mixture B;
adding the rest modified filler, the rest reinforcing agent and the plasticizer into the mixture B, and mixing to 120-130 ℃ to obtain a rubber compound;
and adding a vulcanizing agent and an accelerator into the rubber compound, vulcanizing, and cooling to obtain the low-temperature-resistant fluorine rubber.
By adopting the technical scheme, the fluorine rubber with good low temperature resistance is prepared by using the method.
In summary, the present application includes at least one of the following beneficial technical effects:
1. in the method, fluororubber and ethylene propylene diene monomer are blended, so that the prepared fluororubber has low temperature resistance of the ethylene propylene diene monomer; the white carbon black is modified by using the dimethylvinylethoxysilane, so that the white carbon black can be uniformly dispersed in a system, and the low temperature resistance of the fluororubber is improved under the cooperation of the ethylene propylene diene monomer rubber and the white carbon black;
2. the small-particle carbon black has smaller particle size, better dispersion performance and better reinforcing effect, but the prepared rubber has poor pressure change performance; the large-particle carbon black has larger particle size, so that the pressure change performance of the rubber can be improved;
3. according to the method, fluororubber and ethylene propylene diene monomer rubber are plasticated and mixed firstly, then modified filler, an active agent, a flow aid, a release agent, a part of reinforcing agent, a lubricant, an anti-aging agent and an antiwear agent are added, mixing is carried out, then the rest modified filler, the rest reinforcing agent and a plasticizer are added, finally a vulcanizing machine and an accelerator are added, vulcanization is carried out, and cooling is carried out, so that the fluororubber with better low temperature resistance is obtained.
Detailed Description
The present application is described in further detail below with reference to examples.
All the starting materials in the examples are commercially available. Wherein white carbon CAS number: 10279-57-9; the fluororubber model is FA100S; the ethylene propylene diene monomer rubber model is IP4520; SA is SA-40 active agent; the flow aid is a mixture of two flow aids of model WS-280 and WB212, and the weight ratio is 1:2; the model of the release agent is 935P; the small particle carbon black model is N330; the model of the large-particle carbon black is N990; the cellulose model is KCW250; the type of the wear-resistant agent is F5A; the plasticizer is paraffin oil P5110.
Preparation example
Preparation example 1
Preparation example 1 provides a preparation method of modified filler, which comprises the following steps:
uniformly stirring and mixing dimethylvinylethoxysilane, ethanol and water to obtain a modified liquid; adding white carbon black into a high-speed mixer, spraying a modifying liquid on the white carbon black in the stirring process, stirring for 0.5h after the spraying is finished, and drying for 2h at 50 ℃ to obtain a modified filler; wherein the weight ratio of the dimethylvinylethoxysilane, ethanol and water in the modified liquid is 5:18:2; the weight ratio of the dimethylvinylethoxysilane to the white carbon black is 1:55.
preparation example 2
Preparation example 2 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to white carbon black is 1:60; the remaining steps are identical to those of preparation 1.
Preparation example 3
Preparation example 3 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to white carbon black is 1: 65. The remaining steps are identical to those of preparation 1.
Preparation example 4
Preparation example 4 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to white carbon black is 1:70; the remaining steps are identical to those of preparation 1.
Preparation example 5
Preparation example 5 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to white carbon black is 1:75; the remaining steps are identical to those of preparation 1.
Examples
Example 1
Embodiment 1 provides a preparation method of low temperature resistant fluorine rubber, which comprises the following steps:
putting 50kg of fluororubber and 30kg of ethylene propylene diene monomer into an internal mixer, plasticating and mixing for 45s to obtain a mixture A;
adding 5kg of modified filler, 2kg of active agent, 1kg of flow aid, 0.5kg of release agent, part of reinforcing agent and 10kg of lubricant in preparation example 1 into the mixture A, and mixing to 100 ℃ to obtain a mixture B; wherein the lubricant is advanced graphite AO; the partial reinforcing agent is 17.5kg of small-particle carbon black, 7kg of large-particle carbon black and 6kg of cellulose; the active agent comprises a mixture of zinc oxide and SA, and the weight ratio of the zinc oxide to the SA is 6:1, a step of;
adding 5kg of modified filler, the rest of reinforcing agent and 10kg of plasticizer in preparation example 1 into the mixture B, and mixing to 125 ℃ to obtain a rubber compound; the rest reinforcing agent is 17.5kg of small-particle carbon black and 7kg of large-particle carbon black;
adding the rubber compound into an open mill, adding 2kg of vulcanizing agent and 4kg of accelerator into the rubber compound, vulcanizing, carrying out thin-pass 6 times, and cooling to obtain low-temperature-resistant fluorine rubber; wherein the vulcanizing agent is dicumyl peroxide; the accelerator is a mixture of triallyl isocyanurate and tetramethylthiuram disulfide, and the weight ratio of the triallyl isocyanurate to the tetramethylthiuram disulfide is 1:30.
example 2
Example 2 provides a preparation method of a low temperature resistant fluorine rubber, comprising the following steps:
putting 60kg of fluororubber and 40kg of ethylene propylene diene monomer into an internal mixer, plasticating and mixing for 45s to obtain a mixture A;
7.5kg of modified filler in preparation example 1, 3.5kg of active agent, 1.5kg of flow aid, 1kg of release agent, part of reinforcing agent and 12kg of lubricant are added into mixture A and mixed to 100 ℃ to obtain mixture B; wherein the lubricant is advanced graphite AO; the partial reinforcing agent is 18kg of small-particle carbon black, 8kg of large-particle carbon black and 6kg of cellulose; the active agent comprises a mixture of zinc oxide and SA, and the weight ratio of the zinc oxide to the SA is 6:1, a step of;
7.5kg of the modified filler in preparation example 1, the rest of the reinforcing agent and 12kg of the plasticizer are added into the mixture B and mixed to 125 ℃ to obtain a rubber compound; the rest reinforcing agent is 18kg of small-particle carbon black and 8kg of large-particle carbon black;
adding the rubber compound into an open mill, adding 3.5kg of vulcanizing agent and 4.65kg of accelerator into the rubber compound, vulcanizing, carrying out thin-pass 6 times, and cooling to obtain low-temperature-resistant fluorine rubber; wherein the vulcanizing agent is dicumyl peroxide; the accelerator is a mixture of triallyl isocyanurate and tetramethylthiuram disulfide, and the weight ratio of the triallyl isocyanurate to the tetramethylthiuram disulfide is 1:30.
example 3
Example 3 provides a preparation method of a low temperature resistant fluorine rubber, comprising the following steps:
70kg of fluororubber and 50kg of ethylene propylene diene monomer are put into an internal mixer to be plasticated and mixed for 45s, so as to obtain a mixture A;
10kg of modified filler, 5kg of active agent, 2kg of flow aid, 1.5kg of release agent, part of reinforcing agent and 15kg of lubricant in preparation example 1 are added into the mixture A and mixed to 100 ℃ to obtain a mixture B; wherein the lubricant is advanced graphite AO; the partial reinforcing agent is 20.5kg of small-particle carbon black, 9kg of large-particle carbon black and 6kg of cellulose; the active agent comprises a mixture of zinc oxide and SA, and the weight ratio of the zinc oxide to the SA is 6:1, a step of;
10kg of modified filler, the rest of reinforcing agent and 15kg of plasticizer in preparation example 1 are added into the mixture B and mixed to 125 ℃ to obtain a rubber compound; the rest reinforcing agent is 20.5kg of small-particle carbon black and 9kg of large-particle carbon black;
adding the rubber compound into an open mill, adding 5kg of vulcanizing agent and 5kg of accelerator into the rubber compound, vulcanizing, carrying out thin-pass 6 times, and cooling to obtain low-temperature-resistant fluorine rubber; wherein the vulcanizing agent is dicumyl peroxide; the accelerator is a mixture of triallyl isocyanurate and tetramethylthiuram disulfide, and the weight ratio of the triallyl isocyanurate to the tetramethylthiuram disulfide is 1:30.
examples 4 to 7
As shown in Table 1, examples 4-7 differ from example 2 mainly in the amounts of fluororubber and ethylene propylene diene monomer.
TABLE 1 amounts of raw materials used in examples 4-7
| Sample of | Fluororubber (kg) | Ethylene propylene diene monomer (kg) |
| Example 2 | 60 | 40 |
| Example 4 | 50 | 40 |
| Example 5 | 56 | 40 |
| Example 6 | 64 | 40 |
| Example 7 | 70 | 40 |
Examples 8 to 11
As shown in Table 2, examples 8-11 differ from example 2 mainly in the choice of modified filler.
TABLE 2 selection of modified fillers for examples 8-11
| Sample of | Modified filler is selected |
| Example 2 | Preparation example 1 |
| Example 8 | Preparation example 2 |
| Example 9 | Preparation example 3 |
| Example 10 | Preparation example 4 |
| Example 11 | Preparation example 5 |
Example 12
Example 12 differs from example 9 in that the active agent is zinc oxide; the remaining steps are in accordance with example 9.
Example 13
Example 13 differs from example 9 in that the active agent is SA; the remaining steps are in accordance with example 9.
Example 14
Example 14 differs from example 9 in that 7.5kg of the modified filler of preparation 4, 3.5kg of the active agent, 1.5kg of the flow aid, 1kg of the mold release agent, part of the reinforcing agent, 12kg of the lubricant, 0.5kg of the anti-aging agent, 6kg of the anti-wear agent were added to mixture A and mixed to 100℃to obtain mixture B; wherein the anti-aging agent is 2-mercaptobenzimidazole; the remaining steps are in accordance with example 9.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that 50kg of fluororubber and 30kg of ethylene propylene diene monomer were put into an internal mixer and plasticated and mixed for 45s to obtain a mixture A;
adding 2kg of active agent, 1kg of flow aid, 0.5kg of release agent, part of reinforcing agent and 10kg of lubricant into the mixture A, and mixing to 100 ℃ to obtain a mixture B; wherein the lubricant is advanced graphite AO; the partial reinforcing agent is 17.5kg of small-particle carbon black, 7kg of large-particle carbon black and 6kg of cellulose; the active agent comprises a mixture of zinc oxide and SA, and the weight ratio of the zinc oxide to the SA is 6:1, a step of;
adding 5 rest reinforcing agent and 10kg plasticizer into the mixture B, and mixing to 125 ℃ to obtain a rubber compound; the rest reinforcing agent is 17.5kg of small-particle carbon black and 7kg of large-particle carbon black; the remaining steps are in accordance with example 1.
Comparative example 2
Comparative example 2 differs from example 1 in that 50kg of fluororubber and 30kg of ethylene propylene diene monomer were put into an internal mixer and plasticated and mixed for 45s to obtain a mixture A;
adding 5kg of white carbon black, 2kg of an active agent, 1kg of a flow aid, 0.5kg of a release agent, part of a reinforcing agent and 10kg of a lubricant into the mixture A, and mixing to 100 ℃ to obtain a mixture B; wherein the lubricant is advanced graphite AO; the partial reinforcing agent is 17.5kg of small-particle carbon black, 7kg of large-particle carbon black and 6kg of cellulose; the active agent comprises a mixture of zinc oxide and SA, and the weight ratio of the zinc oxide to the SA is 6:1, a step of;
adding 5kg of white carbon black, the rest of reinforcing agent and 10kg of plasticizer into the mixture B, and mixing to 125 ℃ to obtain a rubber compound; the rest reinforcing agent is 17.5kg of small-particle carbon black and 7kg of large-particle carbon black; the remaining steps are in accordance with example 1.
Performance test
High and low temperature resistance: and testing the temperature resistant range of the fluorine rubber in each embodiment by a third-party detection mechanism.
TABLE 3 results of performance measurements of fluorine gums
By combining the embodiment 1 with the comparative examples 1-2, the fluororubber in the embodiment 1 has the best low temperature resistance, and the white carbon black modified by the dimethylvinylethoxysilane is added into the raw materials in the preparation of the fluororubber, and uniformly dispersed in the system, and the fluororubber and the ethylene propylene diene monomer are blended, so that the low temperature resistance of the fluororubber is improved under the cooperation of the white carbon black and the ethylene propylene diene monomer.
In combination with examples 1 to 3, the low temperature resistance of the fluororubber in example 2 is optimal, and it can be seen that the low temperature resistance of the prepared fluororubber tends to be improved and then reduced when the amount of raw materials used is increased during the preparation of the fluororubber.
In combination with examples 2 and 4-7, the fluororubber in examples 2, 5 and 6 has better high and low temperature resistance, and it can be seen that when the fluororubber is prepared, the ratio of ethylene propylene diene monomer rubber to fluororubber in the raw materials is preferably 1: (1.4-1.6), the prepared fluorine rubber not only has better low temperature resistance, but also has higher high temperature resistance.
In combination with examples 2 and examples 8 to 11, the low temperature resistance of the fluorocarbons in examples 8 to 10 is good, and it can be seen that when the white carbon black is modified with dimethylvinylethoxysilane, the ratio of dimethylvinylethoxysilane to white carbon black is preferably 1: (60-70) so that the dimethyl vinyl ethoxy silane can better coat the white carbon black, thereby improving the low temperature resistance of the prepared fluorine rubber.
In combination with examples 9, 12 and 13, the low temperature resistance of the fluororubber in example 9 is optimal, and it can be seen that when the fluororubber is prepared, the active agent is preferably a mixture of zinc oxide and SA, the zinc oxide and SA react to generate zinc salt, and the zinc salt promotes vulcanization of rubber, so that the performance of the fluororubber is improved.
By combining the embodiment 9 and the embodiment 14, the high and low temperature resistance of the fluorine rubber in the embodiment 9 and the embodiment 14 are not greatly different, and the fact that the aging resistance and the wear resistance of the prepared fluorine rubber can be improved by adding the anti-aging agent and the wear-resistant agent into the raw materials when the fluorine rubber is prepared, but the high and low temperature resistance of the fluorine rubber is not greatly influenced.
The foregoing are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.
Claims (8)
1. The utility model provides a low temperature resistant fluorine gum which characterized in that: the raw materials of the fluorine rubber comprise the following components in parts by weight: 50-70 parts of fluororubber, 30-50 parts of ethylene propylene diene monomer rubber, 10-20 parts of modified filler, 2-5 parts of active agent, 1-2 parts of flow aid, 0.5-1.5 parts of release agent, 55-65 parts of reinforcing agent, 10-15 parts of lubricant, 10-15 parts of plasticizer, 2-5 parts of vulcanizing agent and 4-5 parts of accelerator; the raw materials of the modified filler comprise dimethylvinylethoxysilane, ethanol and white carbon black.
2. The low temperature resistant fluorine gel as set forth in claim 1, wherein: the preparation method of the modified filler comprises the following steps:
uniformly stirring and mixing dimethylvinylethoxysilane, ethanol and water to obtain a modified liquid; and stirring the white carbon black, spraying the modified liquid on the white carbon black in the stirring process, and drying to obtain the modified filler.
3. The low temperature resistant fluorine gel as set forth in claim 2, wherein: the weight ratio of the dimethylvinylethoxysilane to the white carbon black is 1: (60-70).
4. The low temperature resistant fluorine gel as set forth in claim 1, wherein: the weight ratio of the ethylene propylene diene monomer rubber to the fluororubber is 1: (1.4-1.6).
5. The low temperature resistant fluorine gel as set forth in claim 1, wherein: the active agent comprises a mixture of zinc oxide and SA.
6. The low temperature resistant fluorine gel as set forth in claim 1, wherein: the reinforcing agent comprises a mixture of large-particle carbon black, small-particle carbon black and cellulose.
7. The low temperature resistant fluorine gel as set forth in claim 1, wherein: the raw materials of the fluorine rubber further comprise 0.1-1 part by weight of an anti-aging agent and 5-7 parts by weight of an anti-wear agent.
8. A method for preparing the low temperature resistant fluorine rubber according to any one of claims 1 to 7, which is characterized in that: the method comprises the following steps:
plasticating and mixing fluororubber and ethylene propylene diene monomer rubber to obtain a mixture A;
adding part of modified filler, an active agent, a flow aid, a release agent, part of reinforcing agent, a lubricant, an anti-aging agent and an anti-wear agent into the mixture A, and mixing to 90-110 ℃ to obtain a mixture B;
adding the rest modified filler, the rest reinforcing agent and the plasticizer into the mixture B, and mixing to 120-130 ℃ to obtain a rubber compound;
and adding a vulcanizing agent and an accelerator into the rubber compound, vulcanizing, and cooling to obtain the low-temperature-resistant fluorine rubber.
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| CN103102531A (en) * | 2012-12-11 | 2013-05-15 | 芜湖恒坤汽车部件有限公司 | Leather cup rubber for laundry machine and preparation method thereof |
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| CN106674831A (en) * | 2016-12-29 | 2017-05-17 | 关正顺 | Ethylene propylene rubber-fluororubber blending and mixing rubber capable of resisting high-temperature steam |
| CN110183784A (en) * | 2019-05-14 | 2019-08-30 | 株洲时代新材料科技股份有限公司 | A kind of cold-resistant EPDM composite material and preparation method |
| CN113637267A (en) * | 2021-09-08 | 2021-11-12 | 广州美村橡胶科技股份有限公司 | Acid and alkali resistant ethylene propylene diene monomer rubber and preparation method thereof |
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| CN103102531A (en) * | 2012-12-11 | 2013-05-15 | 芜湖恒坤汽车部件有限公司 | Leather cup rubber for laundry machine and preparation method thereof |
| CN106279822A (en) * | 2016-08-09 | 2017-01-04 | 安徽微威胶件集团有限公司 | The rubber cup of master cylinder and manufacturing process thereof |
| CN106674831A (en) * | 2016-12-29 | 2017-05-17 | 关正顺 | Ethylene propylene rubber-fluororubber blending and mixing rubber capable of resisting high-temperature steam |
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