CN114395240A - High-temperature-resistant ultra-pure perfluoroether rubber and preparation method thereof - Google Patents
High-temperature-resistant ultra-pure perfluoroether rubber and preparation method thereof Download PDFInfo
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- CN114395240A CN114395240A CN202111647514.2A CN202111647514A CN114395240A CN 114395240 A CN114395240 A CN 114395240A CN 202111647514 A CN202111647514 A CN 202111647514A CN 114395240 A CN114395240 A CN 114395240A
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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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
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Abstract
The invention belongs to the technical field of preparation of high polymer materials, and particularly relates to high-temperature-resistant ultra-pure perfluoroether rubber and a preparation method thereof. The high-temperature-resistant ultra-pure perfluoroether rubber comprises the following components in parts by mass: 80-120 parts by mass of peroxide perfluoroether rubber; dispersing agent, less than or equal to 10 parts by mass; 5-25 parts of fumed silica; accelerator less than or equal to 10 parts by mass; less than or equal to 10 parts by mass of a vulcanizing agent. The peroxide perfluoroether rubber has the temperature resistance of 300 ℃ and excellent medium resistance; according to the invention, the fumed silica is adopted to improve the high temperature resistance and mechanical property of the material, and the dispersant is adopted to ensure the processability of the material; the invention is ultra-pure perfluoroether rubber, and the precipitation of metal ions is extremely low.
Description
Technical Field
The invention belongs to the technical field of preparation of high polymer materials, and particularly relates to high-temperature-resistant ultra-pure perfluoroether rubber and a preparation method thereof.
Background
The perfluoro ether rubber is a synthetic elastomer, has the characteristics of low temperature resistance of the perfluoro ether oil, solvent resistance of the perfluoro rubber and the like, and is a colorless, tasteless and transparent solid at normal temperature. Perfluoropolyether is a high-molecular fluorinated polymer which appears in the beginning of the last 60 th century, is mainly used as a lubricant and is applied to severe environments such as high oxidation, high corrosion, high radiation and the like. Compared with the traditional fluororubber, the perfluoropolyether rubber has lower brittleness temperature, wider use temperature range, more processing mode choices, high production efficiency and high production efficiency, and is close to the resistance of various solvents and especially suitable for modern large-scale production. Due to the advantages of the perfluoropolyether rubber, the perfluoropolyether rubber has great significance for the domestic research.
Patent CN 105218985 a discloses a high temperature and pressure resistant hydrofluoric acid-resistant fluororubber, which is resistant to high temperature, but only solves the problem that the rubber on the market is not resistant to media, but the perfluoroether rubber cannot be used in the fields of semiconductors and aerospace, and has a small application range.
The feature of high temperature resistance and medium resistance of the perfluoro-ether rubber is commonly used in the market, and the further development of the perfluoro-ether rubber is rarely carried out in more top fields. The semiconductor industry needs high temperature resistant ultra pure perfluoroether rubbers.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-temperature-resistant ultra-pure perfluoroether rubber and a preparation method thereof.
The technical scheme adopted by the invention is as follows: the high-temperature-resistant ultra-pure perfluoroether rubber comprises the following components in parts by mass:
80-120 parts by mass of peroxide perfluoroether rubber;
the mass portion of the dispersant is less than or equal to 10;
5-25 parts of fumed silica;
not more than 10 parts by mass of an accelerator;
less than or equal to 10 parts by mass of vulcanizing agent.
Preferably, the composition comprises the following components in parts by mass:
100 parts by mass of peroxide perfluoroether rubber;
1 part by mass of a dispersant;
15 parts of fumed silica;
2 parts of an accelerator;
and 1 part by mass of a vulcanizing agent.
The accelerant is at least one of BPP, benzyltriphenylphosphonium chloride and TAIC triallyl isocyanurate.
The vulcanizing agent is at least one of bis-di-penta and bisphenol AF.
The preparation method of the high-temperature-resistant ultra-pure perfluoroether rubber comprises the following steps:
(1) weighing the raw materials according to the formula dosage;
(2) adding the raw materials weighed in the step (1) into an open mill for mixing, wherein the open mill temperature is 40-70 ℃, and uniformly mixing to obtain mixed rubber;
(3) vulcanizing the rubber compound obtained in the step (2) in a vulcanizing machine for one time, wherein the vulcanization temperature is 150-200 ℃;
(4) and (4) placing the material vulcanized in the step (3) into an oven for secondary vulcanization at the vulcanization temperature of 200-270 ℃.
In the step (3), the one-time vulcanization time is 5-15 min.
In the step (4), the secondary vulcanization time is 4-24 h.
The invention has the following beneficial effects: the peroxide perfluoroether rubber has the temperature resistance of 300 ℃ and excellent medium resistance; according to the invention, the fumed silica is adopted to improve the high temperature resistance and mechanical property of the material, and the dispersant is adopted to ensure the processability of the material; the invention is ultra-pure perfluoroether rubber, and the precipitation of metal ions is extremely low.
Detailed Description
The present invention will be described in detail with reference to examples. Materials used in the following examples: perfluoroether peroxide rubber, 95HT, 66-70 percent of fluorine content, and Suwei. Dispersant, HT290, STRUKTOL. Fumed silica. Accelerator, TAIC, aksu. Vulcanizing agent, Shuangerwu, Acksu.
Example 1:
the preparation of the high-temperature resistant ultra-pure perfluoroether rubber is carried out according to the protection method claimed by the application, and comprises the following steps:
s1, weighing 100 parts of perfluoroether rubber, 1 part of dispersing agent, 10 parts of fumed silica, 1.5 parts of accelerator and 1 part of vulcanizing agent.
And S2, adding the rubber weighed in the S1, the dispersing agent, the fumed silica, the vulcanizing agent and the accelerator into an open mill for mixing at 40-70 ℃, preferably 60 ℃ uniformly.
S3, carrying out primary vulcanization on the mixed rubber prepared in the S2 in a vulcanizing machine, wherein the vulcanization temperature is 170 ℃.
S4, placing the sealing ring prepared in the S3 in an oven for secondary vulcanization, setting the vulcanization temperature to be 200 ℃, 230 ℃ and 250 ℃, and recording the obtained samples as M1, M2 and M3.
S5, the obtained sealing ring is subjected to a performance test, and the compression set is tested according to the method in ASTM D395 method B. The test results are shown in table 1, and it can be seen from the data results in table 1 that the pressure-dependent change property of the perfluoroether rubber can be improved by increasing the second-stage vulcanization temperature.
Example 2:
the preparation of the high-temperature resistant ultra-pure perfluoroether rubber is carried out according to the protection method claimed by the application, and comprises the following steps:
s1, weighing 100 parts of perfluoroether rubber, 1 part of dispersant, 10 parts of fumed silica, 2 parts of accelerator and 1 part of vulcanizing agent according to the formula dosage.
And S2, adding the rubber weighed in the S1, the dispersing agent, the fumed silica, the vulcanizing agent and the accelerator into an open mill for mixing at 40-70 ℃, preferably 60 ℃ uniformly.
S3, carrying out primary vulcanization on the mixed rubber prepared in the S2 in a vulcanizing machine, wherein the vulcanization temperature is set to be 170 ℃.
S4, placing the sealing ring prepared in the S3 in an oven for secondary vulcanization, setting the vulcanization temperature to be 250 ℃, and marking the obtained sample as M4.
S5, the obtained sealing ring is subjected to a performance test, and the compression set is tested according to the method in ASTM D395 method B. The test results are shown in Table 2, and it can be seen from the data results in Table 2 that the pressure-sensitive deformability of the perfluoroether rubber can be improved by increasing the content of the accelerator.
It will be understood by those skilled in the art that all or part of the steps in the method for implementing the above embodiments may be implemented by relevant hardware instructed by a program, and the program may be stored in a computer-readable storage medium, such as ROM/RAM, magnetic disk, optical disk, etc.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (7)
1. The high-temperature-resistant ultra-pure perfluoroether rubber is characterized by comprising the following components in parts by mass:
80-120 parts by mass of peroxide perfluoroether rubber;
the mass portion of the dispersant is less than or equal to 10;
5-25 parts of fumed silica;
not more than 10 parts by mass of an accelerator;
less than or equal to 10 parts by mass of vulcanizing agent.
2. The high temperature resistant ultra pure perfluoroether rubber according to claim 1, wherein:
100 parts by mass of peroxide perfluoroether rubber;
1 part by mass of a dispersant;
15 parts of fumed silica;
2 parts of an accelerator;
and 1 part by mass of a vulcanizing agent.
3. The perfluoroether rubber according to claim 1, wherein: the accelerant is at least one of BPP, benzyltriphenylphosphonium chloride and TAIC triallyl isocyanurate.
4. The high temperature resistant ultra pure perfluoroether rubber according to claim 1, wherein: the vulcanizing agent is at least one of bis-di-penta and bisphenol AF.
5. A method for preparing the high temperature resistant ultra pure perfluoroether rubber according to any one of claims 1 to 4, comprising the steps of:
(1) weighing the raw materials according to the formula dosage;
(2) adding the raw materials weighed in the step (1) into an open mill for mixing, wherein the open mill temperature is 40-70 ℃, and uniformly mixing to obtain mixed rubber;
(3) vulcanizing the rubber compound obtained in the step (2) in a vulcanizing machine for one time, wherein the vulcanization temperature is 150-200 ℃;
(4) and (4) placing the material vulcanized in the step (3) into an oven for secondary vulcanization at the vulcanization temperature of 200-270 ℃.
6. The method for preparing a high-temperature resistant ultra-pure perfluoroether rubber according to claim 5, wherein: in the step (3), the one-time vulcanization time is 5-15 min.
7. The method for preparing a high-temperature resistant ultra-pure perfluoroether rubber according to claim 5, wherein: in the step (4), the secondary vulcanization time is 4-24 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111647514.2A CN114395240A (en) | 2021-12-30 | 2021-12-30 | High-temperature-resistant ultra-pure perfluoroether rubber and preparation method thereof |
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| CN202111647514.2A CN114395240A (en) | 2021-12-30 | 2021-12-30 | High-temperature-resistant ultra-pure perfluoroether rubber and preparation method thereof |
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| CN114395240A true CN114395240A (en) | 2022-04-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558313A (en) * | 2022-09-08 | 2023-01-03 | 中绿新材料（江苏）有限公司 | Fluororubber composite material for transparent UV-resistant wearable equipment and preparation method thereof |
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| CN104530610A (en) * | 2014-12-29 | 2015-04-22 | 中国兵器工业集团第五三研究所 | Fluorine rubber-fluorosilicone rubber blend and preparation method thereof |
| CN104974451A (en) * | 2014-04-11 | 2015-10-14 | 辽宁省铁岭橡胶工业研究设计院 | Anti-explosion rubber seal ring composition used for all-welded ball valve |
| CN107690451A (en) * | 2015-05-29 | 2018-02-13 | 索尔维特殊聚合物意大利有限公司 | Fluoroelastomer composition |
| CN112457612A (en) * | 2020-11-16 | 2021-03-09 | 上海如实密封科技有限公司 | Low-temperature-resistant perfluoroether rubber composition and preparation method and application thereof |
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- 2021-12-30 CN CN202111647514.2A patent/CN114395240A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974451A (en) * | 2014-04-11 | 2015-10-14 | 辽宁省铁岭橡胶工业研究设计院 | Anti-explosion rubber seal ring composition used for all-welded ball valve |
| CN104530610A (en) * | 2014-12-29 | 2015-04-22 | 中国兵器工业集团第五三研究所 | Fluorine rubber-fluorosilicone rubber blend and preparation method thereof |
| CN107690451A (en) * | 2015-05-29 | 2018-02-13 | 索尔维特殊聚合物意大利有限公司 | Fluoroelastomer composition |
| CN112457612A (en) * | 2020-11-16 | 2021-03-09 | 上海如实密封科技有限公司 | Low-temperature-resistant perfluoroether rubber composition and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| 王珍: "三种含氟橡胶的性能对比" * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558313A (en) * | 2022-09-08 | 2023-01-03 | 中绿新材料（江苏）有限公司 | Fluororubber composite material for transparent UV-resistant wearable equipment and preparation method thereof |
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