CN119161681A - A corrosion-resistant and folding-resistant PTFE composite material and its preparation method and application - Google Patents
A corrosion-resistant and folding-resistant PTFE composite material and its preparation method and application Download PDFInfo
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- CN119161681A CN119161681A CN202411659418.3A CN202411659418A CN119161681A CN 119161681 A CN119161681 A CN 119161681A CN 202411659418 A CN202411659418 A CN 202411659418A CN 119161681 A CN119161681 A CN 119161681A
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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
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers 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
- C08F114/18—Monomers containing fluorine
- C08F114/26—Tetrafluoroethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
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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 an anti-corrosion folding-resistant PTFE composite material, and a preparation method and application thereof. The preparation method of the corrosion-resistant and folding-resistant PTFE composite material comprises the following steps of (1) preparing a PTFE component I by taking persulfate as an initiator through a dispersion polymerization process, (2) preparing a PTFE component II by taking dibenzoyl peroxide as an initiator through a dispersion polymerization process, and (3) blending and granulating the PTFE component I and the PTFE component II to obtain the corrosion-resistant and folding-resistant PTFE composite material. According to the invention, the scheme of modifying polytetrafluoroethylene by adopting heterogeneous additives in the prior art is abandoned, polytetrafluoroethylene prepared by adopting different processes is modified, and because each material in the composite material is polytetrafluoroethylene, the incompatibility condition is avoided, the fatigue resistance effect is far greater than that of polytetrafluoroethylene materials obtained by heterogeneous compatibility, and the composite material has excellent corrosion resistance and folding resistance.
Description
Technical Field
The invention belongs to the technical field, and particularly relates to an anti-corrosion and folding-resistant PTFE composite material, and a preparation method and application thereof.
Background
The polytetrafluoroethylene diaphragm (also called as a polytetrafluoroethylene sealing element, a sealing ring, an oil seal or a PTFE diaphragm fitting) has excellent characteristics of corrosion resistance, high temperature stability, wear resistance, aging resistance and the like, and can be used as a dielectric material in the fields of chemical industry, electronics, medicine and the like.
However, polytetrafluoroethylene (PTFE) is a chain-like polymer material with a basic molecular structure composed of fluorocarbon, and the fluorocarbon bond energy is as high as 485 kJ/mol, which results in very low surface energy and very high viscosity, and is more difficult to pass through other substances to effectively improve the physical properties. For polytetrafluoroethylene diaphragm, the additive modification technology commonly used at present belongs to heterogeneous modification technology, and has serious interfacial compatibility problem between the additive and polytetrafluoroethylene, and the additive inevitably leads to the reduction of elongation at break while improving the tensile strength, so that the polytetrafluoroethylene diaphragm is lack of flexibility and elasticity and is not resistant to folding.
Disclosure of Invention
The invention aims to provide an anti-corrosion folding-resistant PTFE composite material, a preparation method and application thereof, and solves the problems in the prior art.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
The preparation method of the corrosion-resistant folding-resistant PTFE composite material comprises the following steps:
(1) Preparing a first PTFE component by using persulfate as an initiator through a dispersion polymerization process;
(2) Preparing a PTFE component II by using dibenzoyl peroxide as an initiator through a dispersion polymerization process;
(3) And (3) blending and granulating the PTFE component I and the PTFE component II to obtain the corrosion-resistant and folding-resistant PTFE composite material.
According to the invention, the scheme of modifying polytetrafluoroethylene by adopting heterogeneous additives in the prior art is abandoned, polytetrafluoroethylene prepared by adopting different processes is modified, and because each material in the composite material is polytetrafluoroethylene, the incompatibility condition is avoided, the fatigue resistance effect is far greater than that of polytetrafluoroethylene materials obtained by heterogeneous compatibility, and the composite material has excellent corrosion resistance and folding resistance.
Preferably, in the step (1), the persulfate includes ammonium persulfate, potassium persulfate, or sodium persulfate.
Preferably, the dispersion polymerization process in step (1) or step (2) comprises:
(a) Adding an initiator, 20-30% of an emulsifying agent, a stabilizing agent and high-purity water into a polymerization kettle, uniformly stirring, adding 20-40% of tetrafluoroethylene under an inert atmosphere, and heating to the polymerization temperature;
(b) Continuously supplementing the rest 70-80% of emulsifying agent and 60-80% of tetrafluoroethylene in the polymerization process;
(c) And taking out the polytetrafluoroethylene emulsion after the reaction is finished, and obtaining the PTFE component I or the PTFE component II after coagulation, separation, washing and drying.
Preferably, the emulsifier is ammonium perfluorooctanoate, and the stabilizer comprises stearic acid or paraffin.
Preferably, in step (1), the polymerization temperature is 50-80 ℃, the polymerization pressure is 10-15 kgf/cm 2, and the polymerization time is 10-15 h.
Preferably, in step (2), the polymerization temperature is 70-100 ℃, the polymerization pressure is 20-30 kgf/cm 2, and the polymerization time is 10-20 h.
Preferably, in step (3), the mass ratio of the PTFE component I to the PTFE component II is 10 (4-6).
Preferably, in step (3), the blending granulation is performed at 330-350 ℃.
The invention also provides application of the corrosion-resistant folding-resistant PTFE composite material in preparation of the diaphragm. The PTFE composite material prepared by the method has small granularity, can be relatively uniformly dispersed in a die, reduces the concentration effect of internal stress, can effectively ensure the uniformity of crystallinity of all parts, ensures that the prepared diaphragm is not easy to damage, and greatly prolongs the service life.
Compared with the prior art, the invention has the technical effects that:
(1) According to the invention, the scheme of modifying polytetrafluoroethylene by adopting heterogeneous additives in the prior art is abandoned, polytetrafluoroethylene prepared by adopting different processes is modified, and because each material in the composite material is polytetrafluoroethylene, the incompatibility condition is avoided, the fatigue resistance effect is far greater than that of polytetrafluoroethylene materials obtained by heterogeneous compatibility, and the composite material has excellent corrosion resistance and folding resistance.
(2) The PTFE composite material prepared by the method has small granularity, can be relatively uniformly dispersed in a die, reduces the concentration effect of internal stress, can effectively ensure the uniformity of crystallinity of all parts, ensures that the prepared diaphragm is not easy to damage, and greatly prolongs the service life.
Detailed Description
The following examples illustrate the technical scheme of the invention in further detail.
Example 1
The preparation method of the corrosion-resistant folding-resistant PTFE composite material comprises the following steps:
(1) Preparing a first PTFE component by using persulfate as an initiator through a dispersion polymerization process;
Specifically, the method comprises the following steps:
(a) Adding an initiator, 20% of an emulsifying agent, a stabilizing agent and high-purity water into a polymerization kettle, uniformly stirring, introducing nitrogen into the polymerization kettle to discharge oxygen in the polymerization kettle, then adding 20% of tetrafluoroethylene in a nitrogen atmosphere, heating to 50 ℃ and setting the polymerization pressure to 15 kgf/cm 2 for polymerization;
The initiator adopted in the embodiment is potassium persulfate, the emulsifier is ammonium perfluorooctanoate, the stabilizer is paraffin wax, and the mass ratio of the initiator to the emulsifier to the stabilizer to the tetrafluoroethylene is 0.02:0.6:10:100;
In this example, the emulsifier and tetrafluoroethylene were both added in two stages, with only 20% of the total emulsifier and 20% of the total tetrafluoroethylene before the reaction was started;
(b) Continuously supplementing the rest 80% of emulsifying agent and 80% of tetrafluoroethylene in the polymerization process;
the duration of continuous addition of emulsifier and tetrafluoroethylene is equivalent to the duration of polymerization reaction and is 15 h;
(c) Taking out polytetrafluoroethylene emulsion after the reaction is finished, and obtaining a PTFE component I after coagulation, separation, washing and drying;
specifically, after the reaction is finished, continuously introducing nitrogen into a polymerization kettle for 10min, taking out polytetrafluoroethylene emulsion in the polymerization kettle after the polymerization kettle is cooled to room temperature, and obtaining a PTFE component I through conventional condensation, separation, washing and drying processes;
(2) Preparing a PTFE component II by using dibenzoyl peroxide as an initiator through a dispersion polymerization process;
The dispersion polymerization process of the PTFE component II is basically the same as that of the step (1), and is different in that the adopted initiator is dibenzoyl peroxide, the stabilizer is fatty acid, the mass ratio of the initiator to the emulsifier to the stabilizer to the tetrafluoroethylene is 0.03:0.8:15:100, the polymerization temperature is 70 ℃, the polymerization pressure is 30 kgf/cm 2, and the polymerization time is 20 h;
(3) Blending and granulating the PTFE component I and the PTFE component II to obtain the corrosion-resistant and folding-resistant PTFE composite material of the embodiment;
Specifically, the mass ratio of the first PTFE component to the second PTFE component is 10:4, and the blending granulation is performed at 330 ℃.
Example 2
The preparation method of the corrosion-resistant folding-resistant PTFE composite material comprises the following steps:
(1) Preparing a first PTFE component by using persulfate as an initiator through a dispersion polymerization process;
Specifically, the method comprises the following steps:
(a) Adding initiator, 25% of emulsifier, stabilizer and high-purity water into a polymerization kettle, stirring uniformly, introducing nitrogen into the polymerization kettle to discharge oxygen in the polymerization kettle, then adding 30% of tetrafluoroethylene under nitrogen atmosphere, heating to 60 ℃ and setting the polymerization pressure to 15 kgf/cm 2 for polymerization;
The initiator adopted in the embodiment is potassium persulfate, the emulsifier is ammonium perfluorooctanoate, the stabilizer is paraffin wax, and the mass ratio of the initiator to the emulsifier to the stabilizer to the tetrafluoroethylene is 0.02:0.6:10:100;
in this example, the emulsifier and tetrafluoroethylene were both added in two stages, with only 25% of the total emulsifier and 30% of the total tetrafluoroethylene before the reaction was started;
(b) Continuously supplementing the rest 75% of emulsifying agent and 70% of tetrafluoroethylene in the polymerization process;
the duration of continuous addition of emulsifier and tetrafluoroethylene is equivalent to the duration of polymerization reaction and is 15 h;
(c) Taking out polytetrafluoroethylene emulsion after the reaction is finished, and obtaining a PTFE component I after coagulation, separation, washing and drying;
specifically, after the reaction is finished, continuously introducing nitrogen into a polymerization kettle for 10min, taking out polytetrafluoroethylene emulsion in the polymerization kettle after the polymerization kettle is cooled to room temperature, and obtaining a PTFE component I through conventional condensation, separation, washing and drying processes;
(2) Preparing a PTFE component II by using dibenzoyl peroxide as an initiator through a dispersion polymerization process;
The dispersion polymerization process of the PTFE component II is basically the same as that of the step (1), and is different in that the adopted initiator is dibenzoyl peroxide, the stabilizer is fatty acid, the mass ratio of the initiator to the emulsifier to the stabilizer to the tetrafluoroethylene is 0.03:0.8:15:100, the polymerization temperature is 85 ℃, the polymerization pressure is 25 kgf/cm 2, and the polymerization time is 18 h;
(3) Blending and granulating the PTFE component I and the PTFE component II to obtain the corrosion-resistant and folding-resistant PTFE composite material of the embodiment;
specifically, the mass ratio of the first PTFE component to the second PTFE component is 10:5, and the blending granulation is performed at 340 ℃.
Example 3
The preparation method of the corrosion-resistant folding-resistant PTFE composite material comprises the following steps:
(1) Preparing a first PTFE component by using persulfate as an initiator through a dispersion polymerization process;
Specifically, the method comprises the following steps:
(a) Adding initiator, 30% of emulsifier, stabilizer and high-purity water into a polymerization kettle, stirring uniformly, introducing nitrogen into the polymerization kettle to discharge oxygen in the polymerization kettle, then adding 40% of tetrafluoroethylene under nitrogen atmosphere, heating to 80 ℃ and setting the polymerization pressure to 10 kgf/cm 2 for polymerization;
The initiator adopted in the embodiment is potassium persulfate, the emulsifier is ammonium perfluorooctanoate, the stabilizer is paraffin wax, and the mass ratio of the initiator to the emulsifier to the stabilizer to the tetrafluoroethylene is 0.02:0.6:10:100;
in this example, the emulsifier and tetrafluoroethylene were both added in two stages, with only 30% of the total emulsifier and 40% of the total tetrafluoroethylene before the reaction was started;
(b) Continuously supplementing the rest 70% of emulsifying agent and 60% of tetrafluoroethylene in the polymerization process;
The duration of continuous addition of emulsifier and tetrafluoroethylene is equivalent to the duration of polymerization reaction and is 10 h;
(c) Taking out polytetrafluoroethylene emulsion after the reaction is finished, and obtaining a PTFE component I after coagulation, separation, washing and drying;
specifically, after the reaction is finished, continuously introducing nitrogen into a polymerization kettle for 10min, taking out polytetrafluoroethylene emulsion in the polymerization kettle after the polymerization kettle is cooled to room temperature, and obtaining a PTFE component I through conventional condensation, separation, washing and drying processes;
(2) Preparing a PTFE component II by using dibenzoyl peroxide as an initiator through a dispersion polymerization process;
The dispersion polymerization process of the PTFE component II is basically the same as that of the step (1), and is different in that the adopted initiator is dibenzoyl peroxide, the stabilizer is fatty acid, the mass ratio of the initiator to the emulsifier to the stabilizer to the tetrafluoroethylene is 0.03:0.8:15:100, the polymerization temperature is 100 ℃, the polymerization pressure is 20 kgf/cm 2, and the polymerization time is 15 h;
(3) Blending and granulating the PTFE component I and the PTFE component II to obtain the corrosion-resistant and folding-resistant PTFE composite material of the embodiment;
Specifically, the mass ratio of the first PTFE component to the second PTFE component is 10:6, and the blending granulation is performed at 350 ℃.
Example 4
The preparation method of the corrosion-resistant folding-resistant PTFE composite material is basically the same as that of the embodiment 2, except that the dispersion polymerization process (polymerization temperature, polymerization pressure and polymerization time) of the PTFE component II is the same as that of the PTFE component I.
Example 5
The preparation method of the corrosion-resistant folding-resistant PTFE composite material is basically the same as that of the embodiment 2, and the difference is that the mass ratio of the PTFE component I to the PTFE component II is 1:1.
Example 6
The preparation method of the corrosion-resistant folding-resistant PTFE composite material is basically the same as that of the embodiment 2, and the difference is that the mass ratio of the PTFE component I to the PTFE component II is 1:2.
The PTFE composites prepared in examples 1-6 were tested for properties and the results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the PTFE composite material prepared by the invention has excellent physical properties, wherein the PTFE composite material prepared by examples 1-3 has better properties, and is characterized in that the number of folding resistance is more than 20 ten thousand times, the tensile strength reaches more than 75 MPa, the elongation at break reaches more than 550 percent, and the PTFE composite material is basically unchanged when being treated in 240 ℃ and 50% concentrated hydrochloric acid or sodium hydroxide for 24 hours. The PTFE composite material is corrosion-resistant, folding-resistant and has excellent mechanical properties.
Claims (10)
1. The preparation method of the corrosion-resistant and folding-resistant PTFE composite material is characterized by comprising the following steps of:
(1) Preparing a first PTFE component by using persulfate as an initiator through a dispersion polymerization process;
(2) Preparing a PTFE component II by using dibenzoyl peroxide as an initiator through a dispersion polymerization process;
(3) And (3) blending and granulating the PTFE component I and the PTFE component II to obtain the corrosion-resistant and folding-resistant PTFE composite material.
2. The method of claim 1, wherein in step (1), the persulfate comprises ammonium persulfate, potassium persulfate, or sodium persulfate.
3. The method of claim 1, wherein the dispersion polymerization process of step (1) or step (2) comprises:
(a) Adding an initiator, 20-30% of an emulsifying agent, a stabilizing agent and high-purity water into a polymerization kettle, uniformly stirring, adding 20-40% of tetrafluoroethylene under an inert atmosphere, and heating to the polymerization temperature;
(b) Continuously supplementing the rest 70-80% of emulsifying agent and 60-80% of tetrafluoroethylene in the polymerization process;
(c) And taking out the polytetrafluoroethylene emulsion after the reaction is finished, and obtaining the PTFE component I or the PTFE component II after coagulation, separation, washing and drying.
4. A method of preparing as claimed in claim 3 wherein the emulsifier is ammonium perfluorooctanoate and the stabilizer comprises stearic acid or paraffin wax.
5. The process according to claim 3, wherein in the step (1), the polymerization temperature is 50 to 80℃and the polymerization pressure is 10 to 15 kgf/cm 2 and the polymerization time is 10 to 15 h.
6. The process according to claim 3, wherein in the step (2), the polymerization temperature is 70 to 100 ℃, the polymerization pressure is 20 to 30 kgf/cm 2, and the polymerization time is 10 to 20 h.
7. The process according to claim 1, wherein in the step (3), the mass ratio of the PTFE component I to the PTFE component II is 10 (4-6).
8. The process of claim 1, wherein in step (3), the blending granulation is performed at 330 to 350 ℃.
9. A corrosion-resistant and folding-resistant PTFE composite material, characterized in that it is produced by the production method according to any one of claims 1 to 8.
10. Use of the corrosion-resistant and folding-resistant PTFE composite according to claim 9 for the production of membrane sheets.
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Citations (5)
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|---|---|---|---|---|
| JP2002201217A (en) * | 2000-10-30 | 2002-07-19 | Asahi Glass Co Ltd | Tetrafluoroethylene polymer with excellent strength |
| CN103910818A (en) * | 2014-03-21 | 2014-07-09 | 中昊晨光化工研究院有限公司 | Multipurpose polytetrafluoroethylene dispersion resin and preparation method thereof |
| CN110655664A (en) * | 2019-09-23 | 2020-01-07 | 铨盛聚碳科技股份有限公司 | A method and product for preparing polytetrafluoroethylene blend with high efficiency, environmental protection and low cost |
| CN112062891A (en) * | 2020-08-27 | 2020-12-11 | 浙江巨圣氟化学有限公司 | Preparation process of PTFE resin with high compression ratio |
| CN112625261A (en) * | 2019-09-24 | 2021-04-09 | 中昊晨光化工研究院有限公司 | Polytetrafluoroethylene dispersion concentrate and preparation method thereof |
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- 2024-11-20 CN CN202411659418.3A patent/CN119161681A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002201217A (en) * | 2000-10-30 | 2002-07-19 | Asahi Glass Co Ltd | Tetrafluoroethylene polymer with excellent strength |
| CN103910818A (en) * | 2014-03-21 | 2014-07-09 | 中昊晨光化工研究院有限公司 | Multipurpose polytetrafluoroethylene dispersion resin and preparation method thereof |
| CN110655664A (en) * | 2019-09-23 | 2020-01-07 | 铨盛聚碳科技股份有限公司 | A method and product for preparing polytetrafluoroethylene blend with high efficiency, environmental protection and low cost |
| CN112625261A (en) * | 2019-09-24 | 2021-04-09 | 中昊晨光化工研究院有限公司 | Polytetrafluoroethylene dispersion concentrate and preparation method thereof |
| CN112062891A (en) * | 2020-08-27 | 2020-12-11 | 浙江巨圣氟化学有限公司 | Preparation process of PTFE resin with high compression ratio |
Non-Patent Citations (2)
| Title |
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| 谢圣英 等: "《塑料材料》", vol. 1, 31 January 2010, 中国轻工业出版社, pages: 77 * |
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