CN111073306A - Addition type solid conductive fluorosilicone rubber and preparation method thereof - Google Patents
Addition type solid conductive fluorosilicone rubber and preparation method thereof Download PDFInfo
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- CN111073306A CN111073306A CN201911421420.6A CN201911421420A CN111073306A CN 111073306 A CN111073306 A CN 111073306A CN 201911421420 A CN201911421420 A CN 201911421420A CN 111073306 A CN111073306 A CN 111073306A
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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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
- C08K2201/001—Conductive 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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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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Abstract
The invention discloses addition type solid conductive fluorosilicone rubber and a preparation method thereof, wherein the rubber comprises 100 parts of αα omega-divinyl polydimethyl fluorosilicone, 17-43 parts of carbon black, 0.1-0.3 part of vulcanizing agent and 2-3 parts of hydrogen-containing fluorosilicone oil.
Description
Technical Field
The invention relates to a preparation method of addition type solid conductive fluorosilicone rubber for an electric contact part and a liquid crystal display contact part of instruments such as a computer, a telephone and the like, in particular to addition type solid conductive fluorosilicone rubber and a preparation method thereof.
Background
At present, the research on the addition type solid conductive fluorosilicone rubber in China has related reports, but is only limited to theoretical research or experimental simulation, and no mature product appears in the domestic market. The related patents are roughly the following:
chinese patent (CN1255515A) reports a polysiloxane rubber composition for the preparation of cables or profiles. The method is a polysiloxane composition crosslinked or condensed with a peroxide, and a metal compound having at least one unsaturated group.
Chinese patent (CN1865353A) relates to a method for preparing a high voltage electrically insulating silicone rubber composition and a high voltage electrical insulator. The method is to improve the high-voltage-resistant electric insulation performance by treating the common aluminum hydroxide powder.
Chinese patent (CN1282354A) discloses an addition-crosslinked polysiloxane material having creep resistance and arc resistance, which is surface-treated with a metal oxide of aluminum hydroxide, zinc or titanium to improve the arc resistance.
The above-mentioned patents suffer from disadvantages and shortcomings in many aspects of the silicone rubber compositions used, the chemical reaction mechanisms, and the like. For example, the polysiloxane rubber composition is not acid-resistant and alkali-resistant, and the cable accessories buried underground are corroded by sewage for a long time, so that the requirement on the acid-resistant and alkali-resistant performance of the product is higher and higher, the acid-resistant and alkali-resistant performance of the polysiloxane rubber composition is poorer, and the environment is polluted by byproducts generated by peroxide type crosslinking.
Disclosure of Invention
The invention aims to make up for the defects of the prior art, provides the addition type solid conductive fluorosilicone rubber with acid and alkali resistance and excellent conductivity, is used for producing various high-tensile conductive fluorosilicone rubber products such as electrical connectors, electrical sealing shock absorbing parts, conductive connecting parts and the like, and solves the defects of the existing similar products.
In addition, the invention also provides a preparation method of the addition type solid conductive fluorosilicone rubber, and the method has the advantages of good flowability of raw materials, convenient operation, no pollutant emission in the vulcanization process, safety, environmental protection and good mechanical property of the prepared finished product.
In order to solve the technical problems, the invention adopts the following technical scheme:
an addition type solid conductive fluorosilicone rubber comprises the following components in parts by weight:
preferably, the sulfiding agent is a noble metal catalyst, preferably a platinum-based catalyst, a palladium-based catalyst or a rhodium-based catalyst, and the concentration of the sulfiding agent is 5000PPm to 6000 PPm.
Preferably, the vulcanizing agent is a platinum catalyst, and specifically, the vulcanizing agent is one of chloroplatinic acid, a reaction product of chloroplatinic acid and a hydroxyl alcohol, a complex of chloroplatinic acid and olefin, and platinum diacetylacetate.
The molecular weight of the α omega-divinyl dimethyl fluorosilicone is 65 ten thousand, the vinyl mass fraction is 0.08%, the omega-divinyl dimethyl fluorosilicone is purchased from Shanghai Sanai Rich new materials, Inc., the viscosity of hydrogen-containing fluorosilicone oil is 100mPa & s, the active hydrogen mass fraction is 1.0%, carbon black is Vxc-72, and Cabot (China) investment Inc.
Self-preparing hydrogen-containing fluorosilicone oil: adding trifluoropropylmethylcyclotrisiloxane and hydrogen-containing silicone oil KF-99 into a three-neck flask according to a proportion, adding acid clay accounting for 1% of the total weight of the trifluoropropylmethylcyclotrisiloxane and the KF-99, heating to 115-120 ℃, stirring for reacting for 2 hours, vacuumizing for 1 hour at the temperature of 120 ℃ to remove low-boiling-point substances, cooling, and filtering to obtain the organic hydrogen-containing polyfluorosiloxane which is colorless and transparent and has the active hydrogen mass fraction of 1.1%.
The preparation method of the addition type solid conductive fluorosilicone rubber comprises the following steps:
adding α omega-divinyl polydimethyl fluorosilicone into a kneading machine, heating to 120-140 ℃, adding carbon black, kneading for 2.5 hours at normal temperature and normal pressure, treating for 1 hour at 165 ℃, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive fluorosilicone rubber, adding a vulcanizing agent and hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber;
vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product. The test piece has the following comprehensive properties:
shore hardness: 32.5-43; tensile strength: 3.3-6.1 MPa; tear strength: 21-30 KN/mm; elongation at break: 461-600 percent; volume resistivity: 1X 102-2.5×104Ω·cm。
Compared with the prior art, the invention has the following advantages:
in the invention, the raw materials have better fluidity, the operation is convenient during the preparation, the mechanical property is good, the transparency observed by naked eyes is excellent, and no by-product is generated in the vulcanization process, so that no pollutant is emitted, and the invention is safe and environment-friendly.
The product prepared by the addition type solid conductive fluorosilicone rubber is mainly used for producing a series of high-stretch conductive fluorosilicone rubber products such as various electrical plug connectors, electrical sealing shock absorbing parts, conductive connecting parts and the like.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The α, omega-divinylpolydimethylfluorosilicones used in the present invention were purchased from Shanghai Sanai Rich materials, Inc.
The preparation method of the addition type fluorosilicone rubber comprises the following steps:
adding α omega-divinyl polydimethyl fluorosilicone into a kneading machine, heating to 120-140 ℃, adding carbon black, kneading for 2.5 hours at normal temperature and normal pressure, treating for 1 hour at 165 ℃, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive fluorosilicone rubber, adding a vulcanizing agent and hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber;
vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product.
α, wherein the molecular weight of omega-divinyl polydimethyl fluorosilicone is 65 ten thousand, the mass fraction of vinyl is 0.08%, the vulcanizing agent is a noble metal catalyst, preferably a platinum catalyst, a palladium catalyst or a rhodium catalyst, the concentration of the vulcanizing agent is 5000-6000 PPm, furthermore, the vulcanizing agent is selected from one of chloroplatinic acid, a reaction product of chloroplatinic acid and hydroxyl alcohol, a complex of chloroplatinic acid and olefin and platinum diacetylacetate, and the vulcanizing agent of the embodiments 1-6 is selected from chloroplatinic acid for detailed description.
Example 1:
adding 100 parts of α omega-divinyl polydimethyl fluorosilicone serving as a base rubber into a kneading machine, heating to 120-140 ℃, adding 43 parts of carbon black, kneading at normal temperature and normal pressure for 2.5 hours, treating at 165 ℃ for 1 hour, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive base rubber, adding 0.1 part of chloroplatinic acid and 2 parts of hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber.
Vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product.
The prepared addition type solid conductive fluorosilicone rubber is tested to obtain the following comprehensive properties:
hardness, shore a: 43; tensile strength, MPa: 6.1; tear strength, KN/m: 30, of a nitrogen-containing gas; elongation at break,%: 500, a step of; volume resistivity, Ω · cm: 100.
example 2:
adding 100 parts of α omega-divinyl polydimethyl fluorosilicone serving as a base rubber into a kneading machine, heating to 120-140 ℃, adding 36 parts of carbon black, kneading at low temperature and normal pressure for 2.5 hours, treating at 165 ℃ for 1 hour, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive base rubber, adding 0.2 part of chloroplatinic acid and 2.5 parts of hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber.
The comprehensive performance of the prepared addition type solid conductive fluorosilicone rubber in testing is as follows:
hardness, shore a: 41; tensile strength, MPa: 5.6; tear strength, KN/m: 29.5; elongation at break,%: 530; volume resistivity, Ω · cm: 260.
example 3:
adding 100 parts of α omega-divinyl polydimethyl fluorosilicone serving as a base rubber into a kneading machine, heating to 120-140 ℃, adding 33 parts of carbon black, kneading at low temperature and normal pressure for 2.5 hours, then treating at 165 ℃ for 1 hour, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive base rubber, adding 0.3 part of chloroplatinic acid and 3 parts of hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber.
Vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product.
The comprehensive performance of the prepared addition type solid conductive fluorosilicone rubber in testing is as follows:
hardness, shore a: 39; tensile strength, MPa: 5.0; tear strength, KN/m: 28.5; elongation at break,%: 560; volume resistivity, Ω · cm: 1000.
example 4:
adding 100 parts of α omega-divinyl polydimethyl fluorosilicone serving as a base rubber into a kneading machine, heating to 120-140 ℃, adding 27 parts of carbon black, kneading at low temperature and normal pressure for 2.5 hours, treating at 165 ℃ for 1 hour, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive base rubber, adding 0.28 part of chloroplatinic acid and 2.8 parts of hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber.
Vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product.
The comprehensive performance of the prepared addition type solid conductive fluorosilicone rubber in testing is as follows:
hardness, shore a: 37; tensile strength, MPa: 4.5; tear strength, KN/m: 27; elongation at break,%: 520, respectively; volume resistivity, Ω · cm: 4600.
example 5:
adding 100 parts of α omega-divinyl polydimethyl fluorosilicone serving as a base rubber into a kneading machine, heating to 120-140 ℃, adding 23 parts of carbon black, kneading at low temperature and normal pressure for 2.5 hours, treating at 165 ℃ for 1 hour, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive base rubber, adding 0.15 part of chloroplatinic acid and 2.3 parts of hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber.
Vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product.
The comprehensive performance of the prepared addition type solid conductive fluorosilicone rubber in testing is as follows:
hardness, shore a: 36; tensile strength, MPa: 3.9; tear strength, KN/m: 24; elongation at break,%: 441; volume resistivity, Ω · cm: 10018.
example 6:
adding 100 parts of α omega-divinyl polydimethyl fluorosilicone serving as a base rubber into a kneading machine, heating to 120-140 ℃, adding 17 parts of carbon black, kneading at low temperature and normal pressure for 2.5 hours, treating at 165 ℃ for 1 hour, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive base rubber, adding 0.18 part of chloroplatinic acid and 2.6 parts of hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber.
Vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product.
The comprehensive performance of the prepared addition type solid conductive fluorosilicone rubber in testing is as follows:
hardness, shore a: 32.5; tensile strength, MPa: 3.3; tear strength, KN/m: 21; elongation at break,%: 461; volume resistivity, Ω · cm: 25000.
while the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The addition type solid conductive fluorosilicone rubber is characterized by comprising the following components in parts by weight:
2. the addition type solid conductive fluorosilicone rubber as set forth in claim 1, wherein said vulcanizing agent is a noble metal catalyst.
3. The addition type solid conductive fluorosilicone rubber as set forth in claim 2, wherein the vulcanizing agent is a platinum-based catalyst, a palladium-based catalyst or a rhodium-based catalyst, and a concentration of the vulcanizing agent is 5000PPm to 6000 PPm.
4. The addition type solid conductive fluorosilicone rubber as set forth in claim 2, wherein said vulcanizing agent is a platinum-based catalyst.
5. The addition type solid conductive fluorosilicone rubber as claimed in claim 3, wherein the vulcanizing agent is one of chloroplatinic acid, a reaction product of chloroplatinic acid and a hydroxyl alcohol, a complex of chloroplatinic acid and an olefin, and platinum diacetoacetate.
6. The addition type solid conductive fluorosilicone rubber as claimed in claim 1, wherein the α, omega-divinyl polydimethyl fluorosilicone has a molecular weight of 65 ten thousand and a vinyl mass fraction of 0.08%.
7. The method for preparing the addition type solid conductive fluorosilicone rubber according to any one of claims 1 to 5, comprising the steps of:
adding α omega-divinyl polydimethyl fluorosilicone into a kneading machine, heating to 120-140 ℃, adding carbon black, kneading for 2.5 hours at normal temperature and normal pressure, treating for 1 hour at 165 ℃, vacuumizing for 1.5 hours, milling by a double-roller mill to obtain solid conductive fluorosilicone rubber, adding a vulcanizing agent and hydrogen-containing fluorosilicone oil into the double-roller mill, and uniformly stirring and dispersing to obtain the conductive fluorosilicone rubber;
vulcanizing the conductive fluorosilicone rubber for 10-15 min at 130-170 ℃ by using a flat vulcanizing machine to obtain addition type conductive fluorosilicone rubber, and preparing a rubber sheet; then putting the mixture into a 160 ℃ oven, and carrying out secondary vulcanization for 0.6h to obtain the product.
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| US20170198100A1 (en) * | 2014-08-27 | 2017-07-13 | 3M Innovative Properties Company | Novel polyfluoroalkylated alkenes and silicone compounds prepared therefrom |
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2019
- 2019-12-31 CN CN201911421420.6A patent/CN111073306A/en active Pending
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| US20170198100A1 (en) * | 2014-08-27 | 2017-07-13 | 3M Innovative Properties Company | Novel polyfluoroalkylated alkenes and silicone compounds prepared therefrom |
| CN105153710A (en) * | 2015-07-28 | 2015-12-16 | 广东中蓝硅氟管材有限公司 | Cold-contraction type electric fluorosilicone sleeve and application thereof |
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| CN106349717A (en) * | 2016-08-29 | 2017-01-25 | 太仓中化环保化工有限公司 | Curable composition of high-strength perfluoropolyether fluorosilicone oil and preparing method thereof |
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Application publication date: 20200428 |