CN112480577A - Modified fluorine-containing polymer resin for mould pressing and preparation method thereof - Google Patents
Modified fluorine-containing polymer resin for mould pressing and preparation method thereof Download PDFInfo
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- CN112480577A CN112480577A CN202011210835.1A CN202011210835A CN112480577A CN 112480577 A CN112480577 A CN 112480577A CN 202011210835 A CN202011210835 A CN 202011210835A CN 112480577 A CN112480577 A CN 112480577A
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
- C08K2003/3072—Iron sulfates
Abstract
The invention discloses a modified fluorine-containing polymer resin for mould pressing and a preparation method thereof, which can solve the problems of poor fluidity and cracking resistance. Preparing modified fluoropolymer resin for mould pressing by adding a metal simple substance or a metal compound into fluoropolymer emulsion, solution, powder or particles, and adjusting particle melt index by adjusting granulation temperature and residence time; or adjusting the processing temperature and the molding time when manufacturing the product to adjust the melting index and the performance of the product. The invention can realize the finger-melting control of the fluoropolymer resin by post-processing, reduce the corrosivity of the fluoropolymer for mould pressing to metal, improve the mechanical property of the fluoropolymer resin, enlarge the application field and facilitate industrial production.
Description
Technical Field
The invention belongs to the technical field of fluorine chemical industry, and particularly relates to the field of fluoropolymer production.
Background
The fluoropolymer is also called fluororesin, and is a general name of synthetic resins containing fluorine atoms in the molecule. Mainly prepared by polymerizing fluorinated ethylene monomers. Important varieties comprise polytetrafluoroethylene, polyfluorinated ethylene propylene, soluble polytetrafluoroethylene and the like, and the polytetrafluoroethylene has better heat resistance, cold resistance, electrical insulation, chemical corrosion resistance and mechanical property, and is an excellent high-temperature resistant material and an excellent insulating material.
The compression molding process is one of the main processing processes of the fluorine-containing polymer, and the product is mainly applied to the fields of petroleum and chemical anticorrosion sealing, but the compression molding fluorine-containing polymer has lower melt index and poorer fluidity, and the insufficient mold filling is easy to occur in the processing process to influence the quality of the product; the inflation pressure is high, and the requirement on equipment is too high.
Patent CN107880202 provides a sintering method for preparing FEP for mould pressing, which can reduce FEP melt index by sintering method and can meet the performance requirement of FEP for mould pressing, but said method takes too long time and limits industrial production. Patent CN107216584 provides a method for preparing a novel fluororesin alloy, which is characterized in that one of mica powder, talcum powder, kaolin, wollastonite, calcium carbonate and barium sulfate is introduced as a nucleating agent component to obtain the fluororesin alloy with a melt index and a processing temperature, but the method is complicated, increases the melt index and is not suitable for mould pressing.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of modified fluorine-containing polymer resin for mould pressing, which can solve the problems of poor fluidity and cracking resistance.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing modified fluorine-containing polymer resin for mould pressing is characterized in that a metal simple substance or a metal compound is added into fluorine-containing polymer emulsion, solution, powder or particles to prepare the modified fluorine-containing polymer resin for mould pressing.
Preferably, the amount of the metal element or the metal compound added is 50 to 5000ppm based on the mass of the metal element, wherein the mass of the metal element is 50 to 5000ppm based on the mass of the fluorine-containing polymer.
Preferably, after the metal simple substance or the metal compound is added to the fluoropolymer emulsion or the fluoropolymer solution, the modified fluoropolymer powder is obtained through coagulation and washing, and the modified fluoropolymer pellets for die pressing are obtained through extrusion and granulation by a screw machine.
Preferably, the modified fluoropolymer pellets for molding are obtained by adding a metal simple substance or a metal compound to fluoropolymer powder or pellets and then extruding and pelletizing the mixture by a screw extruder.
Preferably, the modified fluoropolymer article is obtained by compression molding after adding the metal element or metal compound to the fluoropolymer pellets.
Preferably, the particle melting finger is adjusted by adjusting the granulation temperature and the retention time; or adjusting the processing temperature and the molding time when manufacturing the product to adjust the melting index and the performance of the product.
Preferably, the metal elements include Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Zr, Nb, Mo, Al, Pd, Ag, Cd, W, Sn, Pt, Au, Hg, Pb.
Preferably, the fluorine-containing polymer is obtained by homopolymerization or copolymerization of more than one fluorine-containing olefin monomer, or copolymerization of more than one fluorine-containing olefin monomer and more than one non-fluorine-containing olefin monomer.
Preferably, the fluoroolefin monomer comprises tetrafluoroethylene, vinyl fluoride, vinylidene fluoride, trifluoroethylene, chlorotrifluoroethylene, hexafluoropropylene, trifluoropropene, perfluoromethyl vinyl ether, perfluoroethyl vinyl ether, perfluoro-n-propyl vinyl ether, perfluoro 3, 6-dioxa-4-methyl-7-octenesulfonyl fluoride, 2-trifluoromethylpropene, 2-methyl-1, 1,1,3,3, 3-hexafluoropropene; the non-fluorine-containing olefin monomer comprises ethylene, propylene, butylene, isobutylene, butadiene, pentene, isoprene, hexene, vinyl chloride, vinylidene chloride and styrene.
The invention also provides the modified fluorine-containing polymer resin for mould pressing, which is prepared by the preparation method of the modified fluorine-containing polymer resin for mould pressing.
The technical scheme adopted by the invention is that one or more common metal simple substances or metal compounds are introduced into the conventional fluorine-containing polymer resin to obtain the modified fluorine-containing polymer resin, the modified fluorine-containing polymer resin is simple and easy to implement, the production period is short, unstable end groups such as carboxyl (-COOH), unsaturated double bond (-CF (CF) 2), acyl fluoride (-COF) and the like can be effectively reduced, the finger-melting control of the fluorine-containing polymer resin by post-processing is realized, the corrosivity of the fluorine-containing polymer for mould pressing on metal is reduced, the mechanical property of the fluorine-containing polymer resin is improved, the application field is expanded, and the industrial production is facilitated.
The following detailed description will explain the present invention and its advantages.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of modified fluorine-containing polymer resin for mould pressing, which comprises the following steps:
a. conventional fluoropolymer resins are obtained by known polymerization methods;
b. and (c) introducing one or more metal elements into the conventional fluoropolymer resin obtained in step a to obtain a modified fluoropolymer resin for molding.
Among them, the conventional fluoropolymer resin may be emulsion, solution, powder or particles, and it is preferable to add a metal simple substance or a metal compound to the emulsion or powder. The metal element may be introduced as a simple metal or a metal compound.
The fluorine-containing polymer is a conventional technique, for example, homopolymerization or copolymerization of more than one fluorine-containing olefin monomer, or copolymerization of more than one fluorine-containing olefin monomer and more than one non-fluorine-containing olefin monomer. The fluorine-containing olefin monomer comprises tetrafluoroethylene, vinyl fluoride, vinylidene fluoride, trifluoroethylene, chlorotrifluoroethylene, hexafluoropropylene, trifluoropropene, perfluoromethyl vinyl ether, perfluoroethyl vinyl ether, perfluoro-n-propyl vinyl ether, perfluoro 3, 6-dioxa-4-methyl-7-octenesulfonyl fluoride, 2-trifluoromethylpropene, 2-methyl-1, 1,1,3,3, 3-hexafluoropropylene; the non-fluorine-containing olefin monomer comprises ethylene, propylene, butylene, isobutylene, butadiene, pentene, isoprene, hexene, vinyl chloride, vinylidene chloride and styrene.
The introduced metal element is a key step of the invention. Common introduced metal elements comprise Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Zr, Nb, Mo, Al, Pd, Ag, Cd, W, Sn, Pt, Au, Hg and Pb.
Further, the present invention obtains through a large amount of practice that the added metal mass is 50-5000ppm, preferably 200-2000ppm, more preferably 500-1500ppm of the mass of the fluorine-containing polymer. The addition amount of one or more of the metal simple substance or the compound is not excessive, and the excessive addition amount can cause serious reduction of the whiteness of the fluorine-containing polymer product and influence the appearance of the product.
The manner of introducing the metal element is another key step of the present invention. As an embodiment, after adding a metal simple substance or a metal compound to a conventional fluoropolymer emulsion or a conventional fluoropolymer solution, the modified fluoropolymer powder is obtained by coagulation and washing, and the modified fluoropolymer pellets for molding are obtained by extrusion and granulation by a screw machine.
As another embodiment, after adding the metal simple substance or the metal compound to the conventional fluoropolymer powder or pellets, the pellets are extruded and pelletized by a screw machine to obtain modified fluoropolymer pellets for molding.
As another embodiment, the modified fluoropolymer article is obtained by compression molding after adding the metal element or metal compound to conventional fluoropolymer pellets.
Further, the fluorine-containing polymer for mold pressing prepared by the method of the invention can further adjust the particle melting index by adjusting the granulation temperature and the residence time; the processing temperature and the molding time can be adjusted during the manufacture of the product to adjust the melt finger and the performance of the product, so that the control of the fluoropolymer melt finger by post-processing can be realized. Thereby having better melt fluidity and being easy to process.
The melt index of the conventional fluorine-containing polymer is more than or equal to 2g/10min, and the melt index of the modified fluorine-containing polymer for mould pressing is less than 2g/10 min. When the conventional fluorine-containing polymer is subjected to high-temperature production processing after metal elements are introduced, the conventional polymer-containing molecular chain is subjected to crosslinking reaction, so that the tensile strength of the modified fluorine-containing polymer for mould pressing is improved by 2MPa-15MPa compared with the conventional fluorine-containing polymer, the elongation at break is increased by 20% -100%, and the bending resistance is improved by 10-1000 times. Thereby ensuring that the fluoropolymer for molding has excellent comprehensive properties.
The modified fluorine-containing polymer for mould pressing prepared by the method introduces metal simple substances or metal ions, and the metal simple substances or the metal ions can catalyze and degrade unstable end groups caused by an inorganic initiator, such as carboxyl (-COOH), unsaturated double bond (-CF (CF) 2), acyl fluoride (-COF) and other end groups, so that the corrosivity of the fluorine-containing polymer for mould pressing to metal is reduced, and the application field of materials is improved.
The preparation method is simple and easy to implement, has short process period and is beneficial to industrial production.
Example 1
The method comprises the following steps: adding water, emulsifier and initiator (ammonium persulfate and potassium persulfate) into a 20L reaction kettle, and polymerizing under the pressure of 3.0-4.2MPa and the temperature of 85-110 ℃ to obtain the fluorinated ethylene propylene resin emulsion.
Step two: and (3) adding the fluorinated ethylene propylene resin emulsion obtained in the step one into an emulsification tank, adding deionized water to adjust the specific gravity to 1.12, adding concentrated nitric acid to adjust the pH value to 6, and stirring for 45min under strong shearing force to obtain the fluorinated ethylene propylene resin.
Step three: and (3) washing the perfluorinated ethylene propylene copolymer resin obtained in the step two by using deionized water until the water conductivity after washing is less than 3 mu S/cm, so as to obtain perfluorinated ethylene propylene copolymer resin powder.
Step four: and (3) putting the perfluorinated ethylene propylene copolymer resin powder obtained in the third step into a drying oven, and drying for 2 hours at the temperature of 120 ℃ until the water content is lower than 0.3% to obtain the perfluorinated ethylene propylene copolymer resin dry powder. The melt index of the dry powder was 27.4g/10 min.
Step five: putting the perfluorinated ethylene propylene copolymer resin dry powder obtained in the fourth step into a dry powder mixer without adding Fe2(SO4)3And mixing for 30min to obtain the mixed fluorinated ethylene propylene resin dry powder.
Step six: and D, granulating the mixed fluorinated ethylene propylene resin dry powder obtained in the step five by using a double-screw machine to obtain the FEP for die pressing.
The FEP for die pressing prepared by the method is semitransparent and granular, the whiteness is 62, the melting point is 263.7 ℃, the melt index is 25.3g/10min, the tensile strength is 26.8MPa, the elongation at break is 341%, the number of unstable terminals is 483, and the bending resistance is 1103 times.
This example is a comparative example, in which no metal element or metal compound is added, compared with the following examples in which a metal element or metal compound is added.
Example 2
Compared with example 1, the difference is that 200ppm Fe is added in step five2(SO4)3。
The FEP for die pressing prepared by the method is semitransparent and granular, the whiteness is 61, the melting point is 264.2 ℃, the melt index is 1.8g/10min, the tensile strength is 32.6MPa, the elongation at break is 365%, the number of unstable terminals is 92, and the bending resistance times are 22543.
Example 3
In step five, 500ppm Fe was added as compared to example 12(SO4)3。
The FEP for die pressing prepared by the method is semitransparent and granular, the whiteness is 63, the melting point is 263.9 ℃, the melt index is 1.5g/10min, the tensile strength is 34.4MPa, the elongation at break is 373 percent, the number of unstable terminals is 81, and the bending resistance time is 38469 times.
Example 4
In step five, 100 was added as compared to example 10ppm Fe2(SO4)3。
The FEP for die pressing prepared by the method is semitransparent and granular, the whiteness is 60, the melting point is 263.5 ℃, the melt index is 1.0g/10min, the tensile strength is 37.2MPa, the elongation at break is 395%, the number of unstable terminals is 59, and the bending resistance times are 62543 times.
Example 5
Compared with example 1, 1000ppm of CuSO was added in step five4。
The FEP for die pressing prepared by the method is semitransparent and granular, the whiteness is 52, the melting point is 263.1 ℃, the melt index is 0.8g/10min, the tensile strength is 37.1MPa, the elongation at break is 392%, the number of unstable terminals is 61, and the bending resistance time is 69251.
Example 6
Compared with example 1, 3000ppm Fe was added in step five2(SO4)3。
The FEP for die pressing prepared by the method is semitransparent and granular, the whiteness is 19, the melting point is 264.5 ℃, the melt index is 0.3g/10min, the tensile strength is 38.3MPa, the breaking elongation is 399%, the number of unstable terminals is 37, and the bending resistance times are 93816.
Example 7
The method comprises the following steps: PFA emulsion is prepared by polymerization, and PFA dry powder is obtained by coagulation, washing and drying.
Step two: the PFA powder was put into a dry mixer without adding Fe2(SO4)3And mixing to obtain the mixed PFA dry powder.
Step three: and D, granulating the mixed PFA dry powder obtained in the step five by using a double-screw machine to obtain PFA granules.
The prepared PFA granules have the whiteness of 66, the melting point of 303.4 ℃, the melt index of 14g/10min, the tensile strength of 30.2MPa, the elongation at break of 342 percent, the bending resistance times of 42381 times and 246 unstable end groups.
This example is a comparative example, in which no metal element or metal compound is added, compared with the following examples in which a metal element or metal compound is added.
Example 8
In comparison with example 7, 1000ppm Fe were added in step two2(SO4)3。
The modified PFA for mould pressing prepared by the method is semitransparent and granular, the whiteness is 60, the melting point is 303.9 ℃, the melt index is 1.8g/10min, the tensile strength is 36.5MPa, the elongation at break is 388%, the bending times are 493541 times, and 53 unstable end groups exist.
Example 9
In comparison with example 7, 1500ppm Fe were added in step two2(SO4)3。
The modified PFA for mould pressing prepared by the method is semitransparent and granular, the whiteness is 64, the melting point is 304.1 ℃, the melt index is 1.1g/10min, the tensile strength is 37.6MPa, the breaking elongation is 424%, the bending resistant times are 627915 times, and the number of unstable terminal groups is 18.
Example 10
Compared with example 7, 1500ppm of CuSO was added in step two4。
The modified PFA for mould pressing prepared by the method is semitransparent and granular, and has the whiteness of 63, the melting point of 303.7 ℃, the melt index of 1.4g/10min, the tensile strength of 36.2MPa, the elongation at break of 438 percent, the bending resistance times of 593671 times and 13 unstable terminal groups.
Specific parameters of the above examples are shown in the following table
It will be understood by those skilled in the art that the addition of the elemental metal or metal compound is not limited to the list of examples described above.
Other embodiments of the present invention than the preferred embodiments described above, and those skilled in the art can make various changes and modifications according to the present invention without departing from the spirit of the present invention, should fall within the scope of the present invention defined in the claims.
Claims (10)
1. A method for preparing modified fluorine-containing polymer resin for mould pressing is characterized in that: the modified fluoropolymer resin for die pressing is prepared by adding a metal simple substance or a metal compound into fluoropolymer emulsion, solution, powder or particles.
2. The process according to claim 1, wherein the modified fluoropolymer resin for molding comprises: the addition amount of the metal simple substance or the metal compound is based on the mass of the metal element, wherein the mass of the metal element is 50-5000ppm of the mass of the fluorine-containing polymer.
3. The process according to claim 2, wherein the modified fluoropolymer resin for molding comprises: adding a metal simple substance or a metal compound into the fluorine-containing polymer emulsion or the fluorine-containing polymer solution, coagulating and washing to obtain modified fluorine-containing polymer powder, and extruding and granulating by a screw machine to obtain modified fluorine-containing polymer granules for die pressing.
4. The process according to claim 2, wherein the modified fluoropolymer resin for molding comprises: adding a metal simple substance or a metal compound into fluoropolymer powder or pellets, and extruding and granulating by a screw machine to obtain the modified fluoropolymer pellets for die pressing.
5. The process according to claim 2, wherein the modified fluoropolymer resin for molding comprises: adding a metal simple substance or a metal compound into the fluorine-containing polymer pellets, and performing compression molding to obtain a modified fluorine-containing polymer product.
6. The process for producing a modified fluoropolymer resin for molding according to any one of claims 1 to 5, wherein: adjusting the particle melting finger by adjusting the granulation temperature and the retention time; or adjusting the processing temperature and the molding time when manufacturing the product to adjust the melting index and the performance of the product.
7. The process according to claim 6, wherein the modified fluoropolymer resin for molding comprises: the metal elements comprise Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Zr, Nb, Mo, Al, Pd, Ag, Cd, W, Sn, Pt, Au, Hg and Pb.
8. The process according to claim 7, wherein the modified fluoropolymer resin for molding comprises: the fluorine-containing polymer is prepared by homopolymerization or copolymerization of more than one fluorine-containing olefin monomer and more than one non-fluorine-containing olefin monomer.
9. The process according to claim 8, wherein the modified fluoropolymer resin for molding comprises: the fluorine-containing olefin monomer comprises tetrafluoroethylene, vinyl fluoride, vinylidene fluoride, trifluoroethylene, chlorotrifluoroethylene, hexafluoropropylene, trifluoropropene, perfluoromethyl vinyl ether, perfluoroethyl vinyl ether, perfluoro-n-propyl vinyl ether, perfluoro 3, 6-dioxa-4-methyl-7-octenesulfonyl fluoride, 2-trifluoromethylpropene, 2-methyl-1, 1,1,3,3, 3-hexafluoropropylene; the non-fluorine-containing olefin monomer comprises ethylene, propylene, butylene, isobutylene, butadiene, pentene, isoprene, hexene, vinyl chloride, vinylidene chloride and styrene.
10. A modified fluoropolymer resin for molding, characterized by: the modified fluoropolymer resin for molding use according to any one of claims 1 to 9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0199991A2 (en) * | 1985-04-01 | 1986-11-05 | Shanghai Institute Of Organic Chemistry Academia Sinica | Fluoropolymer alloys, their preparation and application |
| CN1199062A (en) * | 1997-04-09 | 1998-11-18 | 纳幕尔杜邦公司 | Fluoropolymer stabilization |
| CN1382163A (en) * | 1999-09-08 | 2002-11-27 | 大金工业株式会社 | Fluoropolymer and electric wire and cable both coated with same |
| CN102471552A (en) * | 2009-06-30 | 2012-05-23 | 大金工业株式会社 | Composition and process for producing same, powder coating material, pellets, molded resin, and electric wire |
| CN110922608A (en) * | 2018-09-19 | 2020-03-27 | 中昊晨光化工研究院有限公司 | Method for treating PFA (fluorinated ethylene fluoro-compound) end group for mold pressing |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0199991A2 (en) * | 1985-04-01 | 1986-11-05 | Shanghai Institute Of Organic Chemistry Academia Sinica | Fluoropolymer alloys, their preparation and application |
| CN1199062A (en) * | 1997-04-09 | 1998-11-18 | 纳幕尔杜邦公司 | Fluoropolymer stabilization |
| CN1382163A (en) * | 1999-09-08 | 2002-11-27 | 大金工业株式会社 | Fluoropolymer and electric wire and cable both coated with same |
| CN102471552A (en) * | 2009-06-30 | 2012-05-23 | 大金工业株式会社 | Composition and process for producing same, powder coating material, pellets, molded resin, and electric wire |
| CN110922608A (en) * | 2018-09-19 | 2020-03-27 | 中昊晨光化工研究院有限公司 | Method for treating PFA (fluorinated ethylene fluoro-compound) end group for mold pressing |
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