CN118184852A - Peroxide vulcanized fluororubber and preparation method thereof - Google Patents

Peroxide vulcanized fluororubber and preparation method thereof Download PDF

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CN118184852A
CN118184852A CN202211600638.XA CN202211600638A CN118184852A CN 118184852 A CN118184852 A CN 118184852A CN 202211600638 A CN202211600638 A CN 202211600638A CN 118184852 A CN118184852 A CN 118184852A
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vinyl ether
peroxide
producing
comonomer
fluororubber
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刘波
余金龙
肖忠良
钟子强
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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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
    • C08F214/00—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
    • C08F214/18—Monomers containing fluorine
    • C08F214/22—Vinylidene fluoride
    • C08F214/222—Vinylidene fluoride with fluorinated vinyl ethers
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • 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
    • C08F214/00—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
    • C08F214/18—Monomers containing fluorine
    • C08F214/184—Monomers containing fluorine with fluorinated vinyl ethers
    • 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
    • C08F214/00—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
    • C08F214/18—Monomers containing fluorine
    • C08F214/26—Tetrafluoroethene
    • C08F214/262—Tetrafluoroethene with fluorinated vinyl ethers
    • 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
    • C08F214/00—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
    • C08F214/18—Monomers containing fluorine
    • C08F214/28—Hexyfluoropropene
    • C08F214/282—Hexyfluoropropene with fluorinated vinyl ethers
    • 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
    • C08F216/00—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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
    • C08F216/12—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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
    • C08F216/14—Monomers containing only one unsaturated aliphatic radical
    • C08F216/1408—Monomers containing halogen
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention relates to the technical field of fluorine chemical engineering, in particular to peroxide vulcanized fluororubber and a preparation method thereof, and specifically comprises the following steps: taking vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene and perfluoroalkyl vinyl ether as comonomers to carry out polymerization reaction; wherein the molar ratio of the vinylidene fluoride, the tetrafluoroethylene, the hexafluoropropylene and the perfluoroalkyl vinyl ether is (45-55): (8-15): (8-12): (25-35). The formula of the comonomer is optimized, so that the prepared peroxide vulcanized fluororubber has the performances of high and low temperature resistance and medium resistance, and has good processing fluidity.

Description

Peroxide vulcanized fluororubber and preparation method thereof
Technical Field
The invention relates to the technical field of fluorine chemical engineering, in particular to peroxide vulcanized fluororubber and a preparation method thereof.
Background
A peroxide (or free radical) vulcanized fluororubber is a fluoropolymer prepared by copolymerizing vinylidene fluoride (VDF), perfluoroalkyl vinyl ether (PAVE), tetrafluoroethylene (TFE) and a vulcanization point monomer (CSM) in a certain proportion. The rubber was originally developed and commercialized by DuPont in the United states in the early 70 th century, and then Japanese Dajin and Italian Suwei developed series brand products, currently in a production facility of kiloton scale. The rubber product has excellent performances of special high temperature resistance, corrosion resistance and the like of fluororubber, also has outstanding performances of hot tearing property, superheated steam resistance, organic medium resistance and the like, namely, the rubber product has excellent high temperature resistance, so the rubber product is widely applied to various fields of electronic and electric industry, chemical industry, mechanical industry, national defense industry and the like.
In the aspect of low temperature resistance, the low temperature resistant peroxide vulcanized fluororubber in the prior art is a fluoropolymer which is mainly prepared by copolymerizing vinylidene fluoride (VDF), perfluoroalkyl vinyl ether (PAVE), tetrafluoroethylene (TFE) and a vulcanization point monomer (CSM) according to a certain proportion, wherein the Tg of the fluoropolymer is about-27 ℃, the fluorine content is about 62%, and the fluoropolymer can resist high temperature of about 220 ℃ at most, but has relatively poor organic medium resistance and is easy to embrittle and age in application. While CN110713564a also prepared a wide Wen Yuquan fluoroether rubber, it cannot meet the medium resistance at the same time, so there is still room for further improvement in its performance.
At present, along with the development of technology, fluororubber is gradually required to be applied to more severe environments, and more fields are required to have not only independent low temperature resistance, medium resistance and high temperature resistance, but also high and low temperature resistance and medium resistance. At present, the low temperature resistant peroxide vulcanized fluororubber at the level of minus 25 ℃ cannot simultaneously meet the requirements of medium resistance and 250 ℃ high temperature resistance at the low temperature of minus 25 ℃.
Disclosure of Invention
The invention provides peroxide vulcanized fluororubber and a preparation method thereof, which are used for solving the defect that the prior art is difficult to simultaneously consider the performances of high temperature resistance, low temperature resistance and medium resistance.
In order to achieve the above object, the present invention provides a method for producing a peroxide-vulcanized fluororubber, comprising: taking vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene and perfluoroalkyl vinyl ether as comonomers to carry out polymerization reaction; wherein the molar ratio of the vinylidene fluoride, the tetrafluoroethylene, the hexafluoropropylene and the perfluoroalkyl vinyl ether is (45-55): (8-15): (8-12): (25-35).
According to the invention, the modified monomer hexafluoropropylene is selected, and under the dosage proportion of the comonomer, the fluorine content of the low-temperature-resistant peroxide vulcanized fluororubber can be effectively improved, meanwhile, the low-temperature-resistant peroxide vulcanized fluororubber has good processing fluidity, the Tg value is not obviously improved, and the low-temperature resistance and the high-temperature resistance of the peroxide vulcanized fluororubber are ensured.
Preferably, the mole percentage content of hexafluoropropylene is 8-12% based on the total amount of the comonomer; and/or the molar percentage content of the tetrafluoroethylene is 8-15% based on the total amount of the comonomer.
In the present invention, the amounts of hexafluoropropylene and tetrafluoroethylene in the comonomer have an important effect on the peroxide cured fluororubber properties. According to the invention, when the dosage of hexafluoropropylene in the comonomer is within the limit range, the polymer can be kept at a higher fluorine content, so that the peroxide vulcanized fluororubber is better ensured to have excellent processing fluidity; the amount of the tetrafluoroethylene is within the limit range, so that the fluorine content of the polymer can be improved, the Tg value of the polymer is kept within a lower range, the loss of low-temperature performance is effectively avoided, the polymerization system is kept to have higher polymerization activity, and the efficient polymerization rate is ensured.
Preferably, the perfluoroalkyl vinyl ether is one or more of perfluoromethyl vinyl ether, perfluoroethyl vinyl ether and perfluoropropyl vinyl ether.
Preferably, the preparation method of the peroxide vulcanized fluororubber further comprises the following steps: and mixing the comonomer with the dispersing agent, and then mixing the mixture with the initiator, the vulcanization point monomer and the chain transfer agent, and carrying out polymerization reaction.
The invention also discovers that the dispersing agent is added before the initiator, the vulcanization point monomer and the chain transfer agent, namely before the polymerization reaction, so that the emulsification of the monomer can be effectively optimized, micelles can be formed before the chain initiation, and the arrangement and the distribution of molecular chains are more facilitated.
Preferably, the vulcanization point monomer is one or more of perfluoro-4-bromo-1-butene, perfluoro-4-iodo-1-butene, perfluoro bromoethyl vinyl ether and perfluoro iodoethyl vinyl ether; more preferably, the cure site monomer is used in an amount of from 0.4 to 4 weight percent of the total amount of comonomers.
The invention discovers that the vulcanization point monomer is added into the system, so that crosslinking points can be provided for peroxide vulcanization crosslinking of the copolymer, and good vulcanization performance is ensured; alkane with a diiodo structure plays a role in controlling the Mooney viscosity in the synthesis process of the low-temperature-resistant peroxide vulcanized fluororubber, and meanwhile, forms an I atom at the chain end of a molecule, so that a chain end crosslinking point is provided for the polymer in the vulcanization process, and the compression deformation value of various rubber products of the obtained polymer is lower.
Preferably, the initiator is ammonium persulfate or potassium persulfate; more preferably, 0.01 to 10 parts by weight is added per 100 parts by weight of the aqueous medium.
Preferably, the chain transfer agent is I (CF 2)n I where n is 2, 3, 4 or 5; more preferably, the chain transfer agent is used in an amount of 0.01 to 5wt% of the comonomer.
Preferably, the dispersant is perfluorooctanoic acid salt, more preferably, one or more of perfluorooctanoic acid ammonium salt, perfluorooctanoic acid sodium salt and perfluorooctanoic acid potassium salt.
Preferably, 0.01 to 5 parts by weight of dispersant is added per 100 parts by weight of aqueous medium.
Preferably, the preparation method of the peroxide-cured fluororubber comprises the following steps: mixing part of the comonomer and the dispersing agent with an aqueous medium under the conditions that the oxygen content is less than or equal to 30ppm and the temperature is 80-105 ℃, then mixing an initiator, a chain transfer agent and a vulcanization point monomer under the conditions that the pressure is 2.5-3.8 MPa, and supplementing the comonomer to maintain the initial pressure so as to carry out polymerization reaction.
In the specific embodiment, the dispersion may be subjected to coagulation, washing, drying, and the like after the completion of the copolymerization reaction, as necessary, by those skilled in the art.
As a preferred technical scheme of the invention, the preparation method of the peroxide vulcanized fluororubber comprises the following steps:
(1) Adding deionized water into a reactor, vacuumizing until the oxygen content is less than or equal to 30ppm, adding a dispersing agent, and heating the inside of the reactor to 80-105 ℃;
(2) Adding comonomer into the reactor, raising the pressure of the reactor to 2.5-3.8 MPa, and stirring for 5-15min;
(3) Continuously adding an initiator, a chain transfer agent and a vulcanization point monomer, supplementing a comonomer, and maintaining the initial pressure for 2-4.5 h;
(4) After the reaction, the reaction monomer is recovered, and the dispersion is subjected to treatments such as coagulation, washing, drying, and the like.
The invention also provides the peroxide vulcanized fluororubber, which is prepared by the method.
Based on the technical scheme, the invention has the following beneficial effects:
the formula of the comonomer is optimized, so that the prepared peroxide vulcanized fluororubber has the performances of high and low temperature resistance and medium resistance, and has good processing fluidity. Meanwhile, the preparation method is further optimized, so that the Tg of the peroxide vulcanized fluororubber is about-27 ℃, the fluorine content is about 65%, and the peroxide vulcanized fluororubber has the low temperature resistance of-25 ℃ and the high temperature resistance of 250 ℃ and the medium resistance.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides peroxide vulcanized fluororubber, which is prepared by the following preparation method, and comprises the following specific steps:
(1) 30L of deionized water is added into the reactor, the reactor is evacuated, 35g of ammonium perfluorooctanoate is added when the oxygen content is less than or equal to 30ppm, and the temperature in the reactor is raised to 90 ℃.
(2) The reactor was charged with a molar ratio of 52:9:8:32 vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene and perfluoroalkyl vinyl ether as comonomers, the reactor pressure was raised to 3.0MPa and stirred for 8min.
(3) Continuously adding 20g of potassium persulfate, 25g of perfluoro-1, 3-diiodopropane and 68g of perfluoro-4-iodo-1-butene, and maintaining the absolute pressure in the reactor between 3.5+/-0.02 MPa by supplementing the mixed monomers, wherein the reaction time in the polymerization process is 3.2h, and finishing the polymerization when the solid content of the emulsion reaches 28 wt%.
(4) The reaction monomer was recovered, and the dispersion was coagulated by adding magnesium chloride and vacuum-dried at 100℃to obtain 10.5Kg of a polymer.
Example 2
The embodiment provides peroxide vulcanized fluororubber, which is prepared by the following preparation method, and comprises the following specific steps:
(1) 30L of deionized water was added to the reactor, the reactor was evacuated, and when the oxygen content was not more than 30ppm, 35g of ammonium perfluorooctanoate was added, and the temperature in the reactor was raised to 102 ℃.
(2) The reactor was charged with a molar ratio of 47:12:8:33 vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene and perfluoroalkyl vinyl ether as comonomers, the reactor pressure was raised to 3.5MPa and stirred for 10min.
(3) Continuously adding 20g of potassium persulfate, 35g of perfluoro-1, 2-diiodoethane and 70g of perfluoro-4-bromo-1-butene, and maintaining the absolute pressure in the reactor between 3.0+/-0.02 MPa by supplementing the mixed monomers, wherein the reaction time in the polymerization process is 4 hours, and finishing the polymerization when the solid content of the emulsion reaches 28 wt%.
(4) The reaction monomer was recovered, and the dispersion was coagulated by adding magnesium chloride and vacuum-dried at 100℃to obtain 10.2Kg of a polymer.
Example 3
The embodiment provides peroxide vulcanized fluororubber, which is prepared by the following preparation method, and comprises the following specific steps:
(1) 30L of deionized water is added into the reactor, the reactor is evacuated, 35g of ammonium perfluorooctanoate is added when the oxygen content is less than or equal to 30ppm, and the temperature in the reactor is raised to 85 ℃.
(2) The reactor was charged with a molar ratio of 54:8:12:26 vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene and perfluoroalkyl vinyl ether as comonomers, the reactor pressure was raised to 2.6MPa and stirred for 15min.
(3) Continuously adding 20g of potassium persulfate, 35g of perfluoro-1, 4-diiodobutane and 62g of perfluoro-1-bromoethyl vinyl ether, and maintaining the absolute pressure in the reactor between 2.6+/-0.02 MPa by supplementing the mixed monomers, wherein the reaction time in the polymerization process is 2.5h, and finishing the polymerization when the solid content of the emulsion reaches 28 wt%.
(4) The reaction monomer was recovered, and the dispersion was coagulated by adding magnesium chloride and vacuum-dried at 100℃to obtain 10.0Kg of a polymer.
Comparative example 1
The preparation method of the peroxide-cured fluororubber described in this comparative example was the same as in example 1 except that the molar percentage of hexafluoropropylene based on the total amount of the comonomers was 2%.
Comparative example 2
The preparation method of the peroxide-cured fluororubber described in this comparative example was the same as in example 2, except that the molar percentage of tetrafluoroethylene was 3% based on the total amount of the comonomer.
Test examples
The peroxide-cured fluororubbers obtained in examples 1 to 3 and comparative examples 1 to 2 were prepared according to the following procedure
Vulcanization was carried out with the vulcanization formulation shown in table 1:
TABLE 1 vulcanization formulation of peroxide-vulcanized fluororubbers
Fluororubber 100 (Parts by mass)
MT carbon black 30 (Parts by mass)
ZnO 3 (Mass portion)
2, 5-Dimethyl-2, 5-bis (t-butylperoxy) hexane 2.5 (Parts by mass)
TAIC 1.5 (Parts by mass)
One-stage vulcanization 168℃×10min
Two-stage vulcanization 232℃×4h
The detection method of the items of each index is a common detection method in industry; the test results are shown in Table 2;
TABLE 2 Performance test of peroxide-cured fluororubbers obtained in examples 1 to 2 and comparative example 1
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for preparing peroxide-cured fluororubber, which is characterized by comprising the following steps: taking vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene and perfluoroalkyl vinyl ether as comonomers to carry out polymerization reaction;
Wherein the molar ratio of the vinylidene fluoride, the tetrafluoroethylene, the hexafluoropropylene and the perfluoroalkyl vinyl ether is (45-55): (8-15): (8-12): (25-35).
2. The method for producing a peroxide curable fluororubber according to claim 1, wherein the molar percentage of tetrafluoroethylene is 8 to 15% based on the total amount of the comonomers; and/or the mole percentage content of hexafluoropropylene is 8-12% based on the total amount of the comonomer.
3. The method for producing a peroxide curable fluororubber according to claim 1 or 2, wherein the perfluoroalkyl vinyl ether is one or more of perfluoromethyl vinyl ether, perfluoroethyl vinyl ether and perfluoropropyl vinyl ether.
4. A method for producing a peroxide curable fluororubber according to any one of claims 1 to 3, further comprising:
And mixing the comonomer with the dispersing agent, and then mixing the mixture with the initiator, the vulcanization point monomer and the chain transfer agent, and carrying out polymerization reaction.
5. The method for producing a peroxide curable fluororubber according to any one of claims 1 to 4, wherein the cure site monomer is one or more of perfluoro-4-bromo-1-butene, perfluoro-4-iodo-1-butene, perfluoro-bromoethyl vinyl ether, perfluoro-iodoethyl vinyl ether; preferably, the cure site monomer is used in an amount of from 0.4 to 4 weight percent of the total amount of comonomers.
6. The method for producing a peroxide curable fluororubber according to any one of claims 1 to 5, wherein the initiator is ammonium persulfate or potassium persulfate, preferably 0.01 to 10 parts by weight per 100 parts by weight of the aqueous medium.
7. The method for producing a peroxide cured fluororubber according to any one of claims 1 to 6, wherein the chain transfer agent is I (CF 2)n I wherein n is 2, 3, 4 or 5), and preferably the chain transfer agent is used in an amount of 0.01 to 5% by weight based on the total amount of the comonomer.
8. The method for producing a peroxide curable fluororubber according to any one of claims 1 to 7, wherein the dispersant is a perfluorooctanoic acid salt, preferably one or more of ammonium perfluorooctanoate, sodium perfluorooctanoate, potassium perfluorooctanoate; more preferably, the dispersant is added in an amount of 0.01 to 5 parts by weight per 100 parts by weight of the aqueous medium.
9. The method for producing a peroxide curable fluororubber according to any one of claims 1 to 8, comprising the steps of:
Mixing part of the comonomer and the dispersing agent with an aqueous medium under the conditions that the oxygen content is less than or equal to 30ppm and the temperature is 80-105 ℃, then mixing an initiator, a chain transfer agent and a vulcanization point monomer under the conditions that the pressure is 2.5-3.8 MPa, and supplementing the comonomer to maintain the initial pressure so as to carry out polymerization reaction.
10. Peroxide-cured fluororubber, characterized in that it is obtained by the preparation process according to any one of claims 1 to 9.
CN202211600638.XA 2022-12-12 2022-12-12 Peroxide vulcanized fluororubber and preparation method thereof Pending CN118184852A (en)

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