CN111138577A - PTFE concentrated dispersion liquid and preparation method and application thereof - Google Patents
PTFE concentrated dispersion liquid and preparation method and application thereof Download PDFInfo
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- CN111138577A CN111138577A CN201811307532.4A CN201811307532A CN111138577A CN 111138577 A CN111138577 A CN 111138577A CN 201811307532 A CN201811307532 A CN 201811307532A CN 111138577 A CN111138577 A CN 111138577A
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- concentrated dispersion
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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
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
Abstract
The invention relates to a PTFE concentrated dispersion liquid and a preparation method and application thereof. The PTFE concentrated dispersion liquid comprises: introducing a tetrafluoroethylene monomer into water containing a stabilizer, adding an initiator, and starting a polymerization reaction; continuously adding a dispersing agent in the whole polymerization process; and stopping the polymerization reaction when the solid content in the emulsion system reaches 35-45%, adding an emulsifier, and performing vacuum concentration to obtain the PTFE concentrated dispersion liquid with the solid content of 55-65%. By controlling the saturation degree of particles in the homopolymerization process of tetrafluoroethylene, adjusting the uniform particle shape and consistent sphericity, and adding a small amount of emulsifier in the concentration process, the residual problem in the coating is reduced, the pure tetrafluoroethylene coating for the glass fiber cloth circuit board is manufactured, the dielectric loss tangent Df of the obtained coating reaches below 0.001, and the processing requirement of a downstream circuit board can be better met.
Description
Technical Field
The invention relates to a PTFE concentrated dispersion liquid and a preparation method and application thereof, belonging to the technical field of fluorine chemical industry.
Background
The Polytetrafluoroethylene (PTFE) concentrated dispersion has solid content of about 60%, and can be used for glass fiber cloth fabric, porous metal impregnation, formed film, metal coating, coating of other base materials, and the like.
Suspending a non-ionic wetting agent (emulsifier) in water in a polytetrafluoroethylene concentrated dispersion to form stable micelles (spheres) with the average particle size of 0.18-0.28 mu m; the glass fiber cloth circuit board coating is prepared by adding various fillers to be dispersed in emulsion, forming a film by coating glass fiber cloth, pressing and sintering at high temperature. Wherein, the content of the dispersant, the content of the emulsifier and the particle shape of the resin in the dispersion liquid have great influence on the dielectric loss of the coating.
In order to reduce the dielectric loss of the coating, some studies have been made in the prior art, such as: CN1754894A discloses a modified polytetrafluoroethylene and a manufacturing method thereof, which is characterized in that tetrafluoroethylene and comonomer are polymerized to obtain the modified polytetrafluoroethylene, the use amount of the modified monomer is controlled to be 0.1-1.0 percent of the modified polytetrafluoroethylene, the average primary particle size of the modified polytetrafluoroethylene is 0.22-0.5 mu m, a large amount of non-ionic wetting agent is added, and a dispersion liquid with the emulsifier content of 13 percent is obtained through chemical concentration, the dispersion liquid has excellent film forming property and good light transmittance; however, when the dispersion is used for manufacturing circuit board coatings, the problems of excessive residual emulsifier, inconsistent sphericity of resin particle morphology and the like exist, and the dielectric loss of the coatings is large.
CN200580051041.2 discloses an aqueous PTFE dispersion containing 55 to 75 wt% of fine Polytetrafluoroethylene (PTFE) particles having an average particle diameter of 100 to 500nm, 0.0001 to 0.02% by mass of PTFE of a specific fluorocarboxylate (APFO) having 8 carbon atoms such as ammonium perfluorooctanoate, 1 to 20% by mass of PTFE of a specific nonionic surfactant, and 0.01 to 0.3% by mass of PTFE of a specific fluorocarboxylate having 5 to 7 carbon atoms such as ammonium perfluorohexanoate. The dispersion has good friction stability and good properties of preventing thickening, etc. However, when the dispersion is used for manufacturing a circuit board coating, the problems of high-temperature residue of a dispersing agent, uneven sphericity and size of resin particle shapes and the like exist, and the dielectric loss of the coating is large.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a PTFE concentrated dispersion liquid and a preparation method thereof. The dispersion liquid obtained by the scheme of the invention contains spherical particles with ultra-large particle size, the particle shapes are uniform, the sphericity is consistent, and the content of the emulsifier is less; the residual quantity of the emulsifier in the pure tetrafluoro coating for the glass fiber cloth circuit board prepared from the dispersion liquid is greatly reduced, the thickness and the density of an emulsion coating are favorably improved, the dielectric loss of the coating is greatly reduced, the dielectric loss tangent Df of the coating reaches below 0.001, and the processing requirement of a downstream circuit board can be better met.
The technical scheme of the invention is as follows.
A method of making a concentrated dispersion of PTFE comprising: introducing a tetrafluoroethylene monomer into water containing a stabilizer, adding an initiator, and starting a polymerization reaction; continuously adding a dispersing agent in the whole polymerization process; and stopping the polymerization reaction when the solid content in the emulsion system reaches 35-45%, adding an emulsifier, and performing vacuum concentration to obtain the PTFE concentrated dispersion liquid with the solid content of 55-65%.
The polymerization is an emulsion polymerization.
The pressure of the polymerization reaction is 2.0-3.0 MPa.
During the polymerization, the reaction temperature is controlled to be low (e.g., 70 ℃) and high (90 ℃), and the polymerization temperature is preferably 70 to 90 ℃.
Further, the water is used in an amount of 50 to 70% by volume of the reaction vessel.
Further, the stabilizer is solid paraffin, and the melting point of the stabilizer is 56-58 ℃; the addition amount of the stabilizer is 1-3% of the mass of water.
Further, the initiator is selected from one or more of persulfate (such as ammonium persulfate), organic peroxide, persulfate-ferrous ion and organic peroxide-ferrous ion, and the addition amount of the initiator is 3-5ppm of the mass of water.
Further, the emulsifier is nonionic surfactant, preferably one or more of phenol polyoxyethylene ether, alkyl polyoxyethylene ether, etc., such as NP-12, TX-10, OP-10, 15-S-12, and the addition amount is 3-5% of the weight of polytetrafluoroethylene. The emulsifier provides support for PTFE particles in an emulsion system, improves the storage stability of the PTFE particles, and solves the problem of residue of the concentrated dispersion after sintering.
Further, the dispersing agent is a fluorine-containing anionic surfactant, preferably perfluorooctanoate and perfluorosulfonate; further preferably one or more of ammonium perfluorooctanoate, sodium perfluorooctanoate, potassium perfluorobutyl sulfonate, potassium perfluorohexyl sulfonate, and potassium perfluorooctyl sulfonate; the addition amount is 0.05-0.1% of the water mass.
As one embodiment of the present invention, a method for producing a concentrated PTFE dispersion includes:
(1) adding a stabilizer into water, stirring, vacuumizing, and replacing with nitrogen until the oxygen content is less than 30 ppm;
(2) controlling the temperature in the kettle to 70 ℃, introducing a tetrafluoroethylene monomer, adding an initiator, controlling the reaction pressure to be 2-3MPa, and starting to react; stopping the reaction when the solid content of the obtained emulsion is 35-45%;
(3) adding an emulsifier into the emulsion, and concentrating in vacuum to obtain a PTFE concentrated dispersion liquid with the solid content of 60%;
the dispersant is added continuously throughout the reaction.
The invention also provides the PTFE concentrated dispersion liquid prepared by the method, the solid content of the PTFE concentrated dispersion liquid reaches 35-45%, the particle sphericity is full, and the primary particle size reaches more than 0.28 mu m.
The invention also provides application of the PTFE concentrated dispersion liquid in a coating of a glass fiber cloth circuit board.
The invention has the following beneficial effects:
according to the invention, the pure tetrafluoroethylene coating for the glass fiber cloth circuit board is prepared by controlling the saturation of particles in the homopolymerization process of tetrafluoroethylene, adjusting the particle shape to be uniform and the sphericity to be consistent, adding a small amount of emulsifier in the concentration process and reducing the residue problem in the coating, the dielectric loss tangent Df of the obtained coating reaches below 0.001, and the processing requirement of a downstream circuit board can be better met.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
EXAMPLE 1 preparation of a concentrated dispersion of PTFE
2.8L of deionized water and 84g of paraffin wax are added into a 5L stainless steel high-pressure reaction kettle which is provided with a jacket and is stirred, a kettle cover is covered, the stirring is started, the vacuum pumping is carried out, and the nitrogen gas replacement is carried out. Until the oxygen content is less than 30ppm, controlling the temperature in the kettle to 70 ℃, introducing tetrafluoroethylene monomer, adding 0.01g of ammonium persulfate initiator, controlling the reaction pressure to be 2.5MPa, starting the reaction, continuously adding the ammonium perfluorooctanoate dispersing agent, adding 2.8g in total, controlling the highest temperature in the kettle to be 90 ℃ in the reaction process, and stopping the reaction after reacting for 2.5 hours to obtain the emulsion with the solid content of 38%.
And adding 60g of NP-12 into the obtained emulsion, carrying out vacuum concentration to obtain a PTFE concentrated dispersion liquid with the solid content of 60%, and detecting the performance of the emulsion and Df.
Example 2 preparation of a concentrated dispersion of PTFE
The process described in example 1 is the same except that:
(1) continuously adding 1.4g of ammonium perfluorooctanoate dispersant into the polymerization reaction process, and reacting for 2 hours to obtain emulsion with the solid content of 35 percent;
(2) 88.5g of TX-10 were added to give a concentrated dispersion of PTFE having a solids content of 60%.
EXAMPLE 3 preparation of a concentrated dispersion of PTFE
The process described in example 1 is the same except that:
(1) continuously adding 2.8g of potassium perfluorohexyl sulfonate dispersant and 0.0084g of ammonium persulfate in the polymerization reaction process, wherein the reaction pressure is 3.0MPa, and the solid content of the obtained emulsion is 45%;
(2) 100g of NP-12 was added to obtain a concentrated dispersion of PTFE having a solid content of 60%.
Example 4 preparation of a concentrated dispersion of PTFE
The process described in example 1 is the same except that:
(1) continuously adding 2.4g of perfluoro ammonium caprylate dispersant and 0.014g of succinic peroxide initiator in the polymerization reaction process, wherein the reaction pressure is 2.0MPa, and the solid content of the obtained emulsion is 37%;
(2) 104g of TX-10 was added to give a concentrated dispersion of PTFE having a solids content of 60%.
Example 5 preparation of a concentrated dispersion of PTFE
The process described in example 1 is the same except that:
(1) continuously adding 2.4g of ammonium perfluorooctanoate dispersing agent and 0.01g of ammonium persulfate in the polymerization reaction process to obtain 42% of emulsion solid content;
(2) 74g of TX-10 were added to give a concentrated dispersion of PTFE having a solids content of 60%.
Comparative example 1
The process described in example 1 is the same except that:
(1) 2.8g of ammonium perfluorooctanoate dispersant is added at one time before the polymerization reaction;
(2) carrying out polymerization reaction for 1.5 hours to obtain an emulsion with the solid content of 32 percent;
(3) 61.9g NP12 was added.
The method comprises the following specific steps:
in a 5L stainless steel high-pressure reaction kettle equipped with a jacket and stirring, 2.8L deionized water and 84g solid paraffin are cleaned and added, 2.8g perfluoro ammonium caprylate dispersing agent is added at one time, the kettle cover is covered, the stirring is started, the vacuum pumping is carried out, and the nitrogen gas replacement is carried out. Controlling the temperature in the kettle to 70 ℃ until the oxygen content is less than 30ppm, introducing tetrafluoroethylene monomer, adding 0.01g of ammonium persulfate initiator, controlling the reaction pressure to be 2.5MPa, starting the reaction, controlling the highest temperature in the kettle to be 90 ℃ in the reaction process, and stopping the reaction after the reaction is carried out for 1.5 hours to obtain the emulsion with the solid content of 32%.
Adding 61.9g of NP12 into the obtained emulsion, uniformly stirring, carrying out vacuum concentration to obtain a PTFE concentrated dispersion liquid with the solid content of 60%, and detecting the performance of the emulsion and Df.
Comparative example 2
The process described in example 1 is the same except that:
(1) 1.4g of ammonium perfluorooctanoate dispersant is added at one time before the polymerization reaction;
(2) after reacting for 2 hours, the solid content of the obtained emulsion is 28 percent;
(3) 104gTX-10 was added and the emulsion was chemically concentrated to give a concentrated dispersion of PTFE having a solids content of 60%.
The method comprises the following specific steps:
in a 5L stainless steel high-pressure reaction kettle equipped with a jacket and stirring, 2.8L deionized water and 84g solid paraffin are cleaned and added, 1.4g perfluoro ammonium caprylate dispersing agent is added at one time, the kettle cover is covered, the stirring is started, the vacuum pumping is carried out, and the nitrogen gas replacement is carried out. Controlling the temperature in the kettle to 70 ℃ until the oxygen content is less than 30ppm, introducing tetrafluoroethylene monomer, adding 0.01g of ammonium persulfate initiator, controlling the reaction pressure to be 2.5MPa, starting the reaction, controlling the highest temperature in the kettle to be 90 ℃ in the reaction process, and stopping the reaction after the reaction is carried out for 2 hours to obtain the emulsion with the solid content of 28%.
Adding 104gTX-10 into the obtained emulsion, stirring uniformly, carrying out chemical concentration on the emulsion to obtain PTFE concentrated dispersion liquid with solid content of 60%, and detecting the performance of the emulsion and Df.
Comparative example 3
The same preparation as in the examples is carried out, with the only difference that: 0.46g of ammonium perfluorooctanoate was added before the start of the reaction, and 2.34g of ammonium perfluorooctanoate was added in one portion during the reaction.
Comparative example 4
The same preparation as in the examples is carried out, with the only difference that: 2.8g of ammonium perfluorooctanoate was added in one portion during the reaction.
Effect verification
The emulsions obtained in examples 1 to 5 and comparative examples 1 to 4 were subjected to a performance test, and the dielectric loss tangent Df of the coatings obtained therefrom was also tested.
Wherein, the testing method of the average grain diameter adopts a laser particle sizer for testing;
the method for testing the solid content adopts the method of ASTM D4441;
the stability test method adopts a high-rotating-speed emulsifying machine to test the gel time (second) of the emulsion, and the test conditions are as follows: the rotating speed of the emulsifying machine is 20000rpm at 25 ℃;
the Df test method adopts a high-frequency q table of 1MHz for testing.
The experimental test data are shown in table 1.
Table 1:
as can be seen from Table 1, dispersions with different properties can be obtained by controlling the addition mode and the amount of the dispersing agent in the process of homopolymerization of tetrafluoroethylene. By adopting the dispersant adding mode (namely the mode of continuously adding in the polymerization reaction process), the dispersion liquid containing spherical particles with ultra-large particle size can be obtained, the content of the emulsifier is low, the residue of the emulsifier in the coating is effectively reduced, the thickness and the density of the emulsion coating are favorably improved, and the dielectric loss of the coating is greatly reduced.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for preparing a concentrated dispersion of PTFE, comprising: introducing a tetrafluoroethylene monomer into water containing a stabilizer, adding an initiator, and starting a polymerization reaction; continuously adding a dispersing agent in the whole polymerization process;
and stopping the polymerization reaction when the solid content in the emulsion system reaches 35-45%, adding an emulsifier, and performing vacuum concentration to obtain the PTFE concentrated dispersion liquid with the solid content of 55-65%.
2. The production method according to claim 1, wherein the pressure of the polymerization reaction is 2.0 to 3.0 MPa;
and/or the temperature of the polymerization reaction is 70-90 ℃, and the temperature needs to be controlled to be low before and high after the reaction temperature is controlled in the polymerization reaction process.
3. The production method according to claim 1 or 2, characterized in that the stabilizer is paraffin wax;
and/or the addition amount of the stabilizer is 1-3% of the mass of water.
4. The production method according to any one of claims 1 to 3, wherein the initiator is selected from one or more of persulfate, organic peroxide, persulfate-ferrous ion, and organic peroxide-ferrous ion;
and/or the addition amount of the initiator is 3-5ppm of the mass of water.
5. The process according to any one of claims 1 to 4, wherein the emulsifier is a nonionic surfactant, preferably a phenol polyoxyethylene ether or an alkyl polyoxyethylene ether;
and/or the addition amount of the emulsifier is 3-5% of the weight of the polytetrafluoroethylene.
6. The method according to any one of claims 1 to 5, wherein the dispersing agent is a fluorine-containing anionic surfactant, preferably a perfluorooctanoate, a perfluorosulfonate; further preferably one or more of ammonium perfluorooctanoate, sodium perfluorooctanoate, potassium perfluorobutyl sulfonate, potassium perfluorohexyl sulfonate, and potassium perfluorooctyl sulfonate;
and/or the addition amount of the dispersant is 0.05-0.1% of the mass of water.
7. The method of any one of claims 1 to 6, comprising:
(1) adding a stabilizer into water, stirring, vacuumizing, and replacing with nitrogen until the oxygen content is less than 30 ppm;
(2) controlling the temperature in the kettle to 70 ℃, introducing a tetrafluoroethylene monomer, adding an initiator, controlling the reaction pressure to be 2-3MPa, and starting to react; stopping the reaction when the solid content of the obtained emulsion is 35-45%;
(3) adding an emulsifier into the emulsion, and concentrating in vacuum to obtain a PTFE concentrated dispersion liquid with the solid content of 60%;
the dispersant is added continuously throughout the reaction.
8. A concentrated dispersion of PTFE obtained by the production method according to any one of claims 1 to 7.
9. The concentrated PTFE dispersion of claim 8, wherein the concentrated PTFE dispersion has a solids content of 35% to 45%, a full particle size, and a primary particle size of 0.28 μm or greater.
10. Use of the PTFE concentrated dispersion obtained by the production method according to any one of claims 1 to 7 or the PTFE concentrated dispersion according to claim 8 or 9 for coating glass cloth circuit boards.
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Cited By (3)
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| CN114381013A (en) * | 2022-01-30 | 2022-04-22 | 广州熵能创新材料股份有限公司 | Concentrated aqueous dispersion of fluorine-containing polymer, preparation method and application thereof |
| CN116199905A (en) * | 2022-11-11 | 2023-06-02 | 中昊晨光化工研究院有限公司 | Polytetrafluoroethylene concentrated dispersion |
| CN116199905B (en) * | 2022-11-11 | 2024-05-14 | 中昊晨光化工研究院有限公司 | Polytetrafluoroethylene concentrated dispersion |
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Cited By (4)
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| CN114381013A (en) * | 2022-01-30 | 2022-04-22 | 广州熵能创新材料股份有限公司 | Concentrated aqueous dispersion of fluorine-containing polymer, preparation method and application thereof |
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