CN114196108A - Modified polypropylene film material for capacitor and preparation method thereof - Google Patents
Modified polypropylene film material for capacitor and preparation method thereof Download PDFInfo
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- CN114196108A CN114196108A CN202111489743.6A CN202111489743A CN114196108A CN 114196108 A CN114196108 A CN 114196108A CN 202111489743 A CN202111489743 A CN 202111489743A CN 114196108 A CN114196108 A CN 114196108A
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- Prior art keywords
- modified polypropylene
- modified
- polypropylene film
- film material
- barium titanate
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 115
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 115
- -1 polypropylene Polymers 0.000 title claims abstract description 114
- 239000000463 material Substances 0.000 title claims abstract description 45
- 239000003990 capacitor Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical class [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000002033 PVDF binder Substances 0.000 claims abstract description 13
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 13
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012965 benzophenone Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 5
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 56
- 239000000243 solution Substances 0.000 claims description 41
- 238000001035 drying Methods 0.000 claims description 29
- 239000011259 mixed solution Substances 0.000 claims description 29
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 28
- 238000001125 extrusion Methods 0.000 claims description 24
- 229910002113 barium titanate Inorganic materials 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 16
- 238000005469 granulation Methods 0.000 claims description 16
- 230000003179 granulation Effects 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 9
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 9
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 9
- 239000007822 coupling agent Substances 0.000 claims description 9
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 claims description 7
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 5
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 4
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 4
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 3
- 229920001911 maleic anhydride grafted polypropylene Polymers 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 47
- 230000015556 catabolic process Effects 0.000 description 6
- 230000005855 radiation Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003989 dielectric material Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use 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; Derivatives of such polymers
- C08J2427/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/16—Homopolymers or copolymers of vinylidene fluoride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use 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; Derivatives of such polymers
- C08J2427/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/20—Homopolymers or copolymers of hexafluoropropene
-
- 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
- C08K3/24—Acids; Salts thereof
-
- 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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a modified polypropylene film material for a capacitor, which comprises the following raw materials in parts by weight: 60-90 parts of modified polypropylene, 5-10 parts of modified barium titanate, 30-50 parts of polyvinylidene fluoride, 0.5-2 parts of benzophenone, 3-5 parts of a cross-linking agent, 5-10 parts of a compatilizer and 0.5-1.5 parts of an antioxidant. The film prepared by the invention takes polypropylene as a base material, has low dielectric loss, is added with the modified inorganic ceramic material, has high dielectric property, good mechanical property and processing property, simple and easy preparation method, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of high polymer material processing, and particularly relates to a modified polypropylene film material for a capacitor and a preparation method thereof.
Background
With the rapid development of the microelectronics industry, the demand for miniaturized capacitors is more and more urgent. In order to obtain a capacitor having a small volume while satisfying light weight and high energy storage density, it is critical to develop a dielectric thin film having a small density, a high dielectric constant and a low dielectric loss as a dielectric material.
Polypropylene is the most used dielectric material in power capacitors, and has the advantages of high breakdown field strength, low dielectric loss, wide source and the like, but the low dielectric constant limits the energy storage of polypropylene and further more extensive application of polypropylene.
Chinese CN101955621A describes a ceramic powder of barium titanate (BaTiO) with a high dielectric constant3) And PVDF; chinese patent CN 102702652a describes a composite material of purified metal Al and PVDF, in which the Al powder is up to 10-50% by volume; chinese patent CN 101423645A discloses a BaTiO compound3Al powder and PVDF; chinese patent CN 102265361a discloses a film in which rubber particles and highly dielectric inorganic particles are dispersed in a thermoplastic resin. In the above prior art, high dielectric constant and withstand voltage can be obtained by adding a high content of ceramic particles, but at the same time, the mechanical strength, particularly elongation, of the film itself is lowered due to incompatibility between the added inorganic ceramic particles and the polymer. Based on the seepage effect, the dielectric constant of the film can be greatly improved by adding the metal particles, but the dielectric loss is large, and the requirements of obtaining high dielectricity, low dielectric loss, strong mechanical property and easiness in industrial production cannot be met simultaneously.
At present, one main research direction for improving the dielectric constant of the dielectric material is to add inorganic nanoparticles, but the easy agglomeration property of the inorganic nanoparticles and the poor compatibility with a polymer matrix cause the processing performance of an inorganic nanoparticle/polypropylene system to be extremely poor, and engineering application is difficult to obtain in practice. And the dielectric constant of the polypropylene film is about 2.2, although the breakdown strength is relatively high, about 600kV/mm or more, under the condition of such low dielectric coefficient, the application range of the polypropylene film as a capacitor under a low working electric field is influenced to a certain extent, so that the preparation of a thin film dielectric material with high dielectric constant and high breakdown strength is a great challenge in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a modified polypropylene film material for a capacitor and a preparation method thereof. The preparation method is simple and feasible and is suitable for industrial production.
In order to achieve the purpose, the invention provides the following technical scheme:
a modified polypropylene film material for a capacitor comprises the following raw materials in parts by weight:
preferably, the preparation method of the modified polypropylene comprises the following steps:
s21, adding the perovskite powder into a mixture with the volume ratio of 1: soaking the mixed solution of the sodium carbonate and the potassium permanganate of the 1 for 3-4h, taking out and washing, calcining for 1-3h at the temperature of 500-600 ℃, cooling, ball-milling and sieving to obtain modified perovskite powder;
s22, adding polypropylene, triphenyl phosphite and the modified perovskite powder obtained in the step (1) into dimethylbenzene, heating to 135 ℃ under the condition of stirring, preserving heat after the reaction is finished, then cooling to room temperature at a certain speed, filtering and drying to obtain the modified polypropylene.
Preferably, the reaction time in the step S22 is 1-2h, the heat preservation time is 2-4h, and the heat preservation temperature is 120-; the cooling rate is 1-2 ℃/min.
Preferably, in step S22, the mass ratio of the polypropylene to the triphenyl phosphite to the modified perovskite is 100: 2-4: 5-10.
Preferably, the preparation method of the modified barium titanate comprises the following steps:
s51, preparing tetrabutyl titanate into a butanol solution with the mass percentage of 30%, adding the butanol solution into a high-pressure reaction kettle, then adding a barium hydroxide aqueous solution, uniformly stirring and mixing, then reacting the mixed solution at 160 ℃ for 12-24 hours, pouring an upper layer solution obtained by hydrothermal reaction after the reaction is finished, pouring acetic acid and deionized water, and then centrifuging, washing and drying to obtain barium titanate powder;
s52, adding the barium titanate powder obtained in the step S51 into 1mol/L hydrochloric acid solution for soaking, then filtering, calcining at 500 ℃ for 1-2h, cooling to room temperature, adding into ethanol solution, adding titanate coupling agent, fully mixing, and drying to obtain the modified barium titanate powder.
Preferably, the molar ratio of tetrabutyl titanate to barium hydroxide in step S51 is 1: 3, in the step S52, the mass ratio of the barium titanate powder to the titanate coupling agent is 100: 0.5-1.
Preferably, the crosslinking agent is one or more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate and pentaerythritol triacrylate; the compatilizer is one or more of polyvinylidene fluoride hexafluoropropylene and maleic anhydride grafted polypropylene; the antioxidant is one or more of antioxidant 1010, antioxidant 168 and antioxidant 1098.
The invention also discloses a preparation method of the modified polypropylene film material for the capacitor, which comprises the following steps:
s81, respectively weighing modified polypropylene, modified barium titanate, polyvinylidene fluoride, benzophenone, a cross-linking agent, a compatilizer and an antioxidant according to a formula, adding the weighed materials into a mixer, stirring for 0.5-1h, adding the materials into a double-screw extruder for granulation, wherein the extrusion temperature is 190-250 ℃, and drying after the granulation is finished to obtain modified polypropylene master batches;
s82, adding the modified polypropylene master batch obtained in the step S81 into a single-screw extruder for sheet extrusion, and obtaining the modified polypropylene film after biaxial stretching and ultraviolet irradiation.
Preferably, the extrusion temperature in the step S82 is 220-2。
The invention also discloses application of the modified polypropylene film material in a capacitor.
Compared with the prior art, the invention has the following beneficial effects:
(1) the modified polypropylene film material provided by the invention is prepared by firstly modifying perovskite powder to remove residual micromolecules and organic impurities on the surface of the perovskite powder, and then carrying out a solvent precipitation method on polypropylene, triphenyl phosphite and the perovskite powder in a high-pressure reaction kettle to obtain the modified polypropylene powder. By controlling the heat preservation time and the cooling rate, the perovskite powder is uniformly dispersed in the polypropylene, and simultaneously the crystallinity of the polypropylene can be controlled, so that the roughness of the subsequently prepared film can be controlled, and the added perovskite can also improve the dielectric constant of the polypropylene.
(2) The modified polypropylene film material provided by the invention is prepared into barium titanate powder through hydrothermal reaction, and then surface modification is carried out on the barium titanate powder, so that the compatibility of the barium titanate powder with polypropylene and the dispersibility of the barium titanate powder in the polypropylene material are improved, and the mechanical property of the film is improved while the low dielectric loss of the polypropylene material is maintained.
(3) According to the preparation method of the modified polypropylene film material, the photoinitiator benzophenone and the cross-linking agent are added, and the modified polypropylene film material is cross-linked through ultraviolet irradiation in the preparation process, so that the mechanical property of the film can be improved, and the polypropylene can be cross-linked with the compatilizer through the cross-linking reaction under the action of the cross-linking agent and the compatilizer through the cross-linking reaction, so that the compatibility of the polypropylene and polyvinylidene fluoride is improved, and the dielectric constant of the film is improved.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
A modified polypropylene film material for a capacitor comprises the following raw materials in parts by weight:
the preparation method of the modified polypropylene comprises the following steps:
adding the perovskite powder into a mixture with a volume ratio of 1: 1, soaking the mixed solution of sodium carbonate and potassium permanganate in the mixed solution for 3 hours, taking out and washing the mixed solution, calcining the mixed solution for 1 hour at the temperature of 500 ℃, cooling the calcined solution, and then carrying out ball milling and sieving to obtain modified perovskite powder; adding 100 parts of polypropylene, 2 parts of triphenyl phosphite and 5 parts of modified perovskite powder into 800mL of dimethylbenzene, heating to 135 ℃ under the condition of stirring, reacting for 1h, then preserving the heat for 2h at 120 ℃, then reducing the temperature to room temperature at the speed of 1 ℃/min, filtering and drying to obtain the modified polypropylene.
The preparation method of the modified barium titanate comprises the following steps:
preparing 34g of tetrabutyl titanate into a butanol solution with the mass percentage of 30%, adding the butanol solution into a high-pressure reaction kettle, then adding an aqueous solution containing 51g of barium hydroxide, uniformly stirring and mixing, then reacting the mixed solution at 120 ℃ for 12 hours, pouring an upper layer solution obtained by hydrothermal reaction after the reaction is finished, pouring acetic acid and deionized water, and then centrifuging, washing and drying to obtain barium titanate powder; and then 100g of barium titanate powder is added into 1mol/L hydrochloric acid solution for soaking, then filtration is carried out, calcination is carried out for 1h at 500 ℃, the mixture is cooled to room temperature and then added into ethanol solution, 0.5g of titanate coupling agent is added, and the modified barium titanate powder is obtained after full mixing and drying.
A preparation method of a modified polypropylene film material for a capacitor comprises the following steps:
(1) respectively weighing modified polypropylene, modified barium titanate, polyvinylidene fluoride, benzophenone, trimethylolpropane triacrylate, polyvinylidene fluoride hexafluoropropylene and an antioxidant 1010 according to a formula, adding into a mixer, stirring for 0.5h, adding into a double-screw extruder for granulation, wherein the extrusion temperature is 200 ℃, and drying after granulation is finished to obtain modified polypropylene master batches;
(2) and (2) adding the modified polypropylene master batch obtained in the step (1) into a single-screw extruder for sheet extrusion, and performing biaxial tension and ultraviolet irradiation to obtain the modified polypropylene film.
Wherein the extrusion temperature is 240 ℃, the longitudinal stretching ratio is 3.0, the transverse stretching ratio is 5.5, and the ultraviolet radiation dose is 1500mJ/cm2。
Example 2
A modified polypropylene film material for a capacitor comprises the following raw materials in parts by weight:
the preparation method of the modified polypropylene comprises the following steps:
adding the perovskite powder into a mixture with a volume ratio of 1: 1, soaking the mixed solution of sodium carbonate and potassium permanganate in the mixed solution for 3 hours, taking out and washing the mixed solution, calcining the mixed solution for 1 hour at the temperature of 550 ℃, cooling the calcined solution, and then carrying out ball milling and sieving to obtain modified perovskite powder; adding 100 parts of polypropylene, 3 parts of triphenyl phosphite and 7 parts of modified perovskite powder into 800mL of dimethylbenzene, heating to 135 ℃ under the condition of stirring, reacting for 1.5h, then preserving heat for 3h at 120 ℃, then reducing to room temperature at the speed of 1 ℃/min, filtering and drying to obtain the modified polypropylene.
The preparation method of the modified barium titanate comprises the following steps:
preparing 34g of tetrabutyl titanate into a butanol solution with the mass percentage of 30%, adding the butanol solution into a high-pressure reaction kettle, then adding an aqueous solution containing 51g of barium hydroxide, uniformly stirring and mixing, then reacting the mixed solution at 130 ℃ for 16 hours, pouring an upper layer solution obtained by hydrothermal reaction after the reaction is finished, pouring acetic acid and deionized water, and then centrifuging, washing and drying to obtain barium titanate powder; and then 100g of barium titanate powder is added into 1mol/L hydrochloric acid solution for soaking, then filtration is carried out, calcination is carried out for 1.5h at 500 ℃, the mixture is cooled to room temperature and then added into ethanol solution, 0.5g of titanate coupling agent is added, and the modified barium titanate powder is obtained after full mixing and drying.
A preparation method of a modified polypropylene film material for a capacitor comprises the following steps:
(1) respectively weighing modified polypropylene, modified barium titanate, polyvinylidene fluoride, benzophenone, trimethylolpropane trimethacrylate, polyvinylidene fluoride hexafluoropropylene and an antioxidant 1098 according to a formula, adding into a mixer, stirring for 0.5h, adding into a double-screw extruder for granulation, wherein the extrusion temperature is 220 ℃, and drying after granulation is finished to obtain modified polypropylene master batches;
(2) and (2) adding the modified polypropylene master batch obtained in the step (1) into a single-screw extruder for sheet extrusion, and performing biaxial tension and ultraviolet irradiation to obtain the modified polypropylene film.
Wherein the extrusion temperature is 240 ℃, the longitudinal stretching ratio is 3.5, the transverse stretching ratio is 6.0, and the ultraviolet radiation dose is 1700mJ/cm2。
Example 3
A modified polypropylene film material for a capacitor comprises the following raw materials in parts by weight:
the preparation method of the modified polypropylene comprises the following steps:
adding the perovskite powder into a mixture with a volume ratio of 1: 1, soaking the mixed solution of sodium carbonate and potassium permanganate in the mixed solution for 3 hours, taking out and washing the mixed solution, calcining the mixed solution for 3 hours at the temperature of 550 ℃, cooling the calcined solution, and then carrying out ball milling and sieving to obtain modified perovskite powder; adding 100 parts of polypropylene, 3 parts of triphenyl phosphite and 8 parts of modified perovskite powder into 800mL of dimethylbenzene, heating to 135 ℃ under the condition of stirring, reacting for 2 hours, then preserving the heat for 3 hours at 125 ℃, then cooling to room temperature at the speed of 1.5 ℃/min, filtering and drying to obtain the modified polypropylene.
The preparation method of the modified barium titanate comprises the following steps:
preparing 34g of tetrabutyl titanate into a butanol solution with the mass percentage of 30%, adding the butanol solution into a high-pressure reaction kettle, then adding an aqueous solution containing 51g of barium hydroxide, uniformly stirring and mixing, then reacting the mixed solution at 140 ℃ for 20 hours, pouring an upper layer solution obtained by hydrothermal reaction after the reaction is finished, pouring acetic acid and deionized water, and then centrifuging, washing and drying to obtain barium titanate powder; and then 100g of barium titanate powder is added into 1mol/L hydrochloric acid solution for soaking, then filtration is carried out, calcination is carried out for 2h at 500 ℃, the mixture is cooled to room temperature and then added into ethanol solution, 0.8g of titanate coupling agent is added, and the modified barium titanate powder is obtained after full mixing and drying.
A preparation method of a modified polypropylene film material for a capacitor comprises the following steps:
(1) respectively weighing modified polypropylene, modified barium titanate, polyvinylidene fluoride, benzophenone, pentaerythritol triacrylate, maleic anhydride grafted polypropylene and antioxidant 168 according to a formula, adding into a mixer, stirring for 1h, adding into a double-screw extruder for granulation, wherein the extrusion temperature is 240 ℃, and drying after granulation is finished to obtain modified polypropylene master batches;
(2) and (2) adding the modified polypropylene master batch obtained in the step (1) into a single-screw extruder for sheet extrusion, and performing biaxial tension and ultraviolet irradiation to obtain the modified polypropylene film.
Wherein the extrusion temperature is 260 ℃, the longitudinal stretching ratio is 4.0, the transverse stretching ratio is 6.5, and the ultraviolet radiation dose is 1800mJ/cm2。
Example 4
A modified polypropylene film material for a capacitor comprises the following raw materials in parts by weight:
the preparation method of the modified polypropylene comprises the following steps:
adding the perovskite powder into a mixture with a volume ratio of 1: 1, soaking the mixed solution of sodium carbonate and potassium permanganate in the mixed solution for 4 hours, taking out and washing the mixed solution, calcining the mixed solution for 3 hours at the temperature of 600 ℃, cooling the calcined solution, and then carrying out ball milling and sieving to obtain modified perovskite powder; adding 100 parts of polypropylene, 4 parts of triphenyl phosphite and 10 parts of modified perovskite powder into 800mL of dimethylbenzene, heating to 135 ℃ under the condition of stirring, reacting for 2 hours, then preserving the heat for 4 hours at 130 ℃, then reducing to room temperature at the speed of 2 ℃/min, filtering and drying to obtain the modified polypropylene.
The preparation method of the modified barium titanate comprises the following steps:
preparing 34g of tetrabutyl titanate into a butanol solution with the mass percentage of 30%, adding the butanol solution into a high-pressure reaction kettle, then adding an aqueous solution containing 51g of barium hydroxide, uniformly stirring and mixing, then reacting the mixed solution at 160 ℃ for 24 hours, pouring an upper layer solution obtained by hydrothermal reaction after the reaction is finished, pouring acetic acid and deionized water, and then centrifuging, washing and drying to obtain barium titanate powder; and then adding 100g of barium titanate powder into 1mol/L hydrochloric acid solution for soaking, then filtering, calcining at 500 ℃ for 2h, cooling to room temperature, adding into ethanol solution, then adding 1g of titanate coupling agent, fully mixing, and drying to obtain modified barium titanate powder.
A preparation method of a modified polypropylene film material for a capacitor comprises the following steps:
(1) respectively weighing modified polypropylene, modified barium titanate, polyvinylidene fluoride, benzophenone, pentaerythritol triacrylate, polyvinylidene fluoride hexafluoropropylene and an antioxidant 1098 according to a formula, adding into a mixer, stirring for 1h, adding into a double-screw extruder for granulation, wherein the extrusion temperature is 250 ℃, and drying after granulation is finished to obtain modified polypropylene master batches;
(2) and (2) adding the modified polypropylene master batch obtained in the step (1) into a single-screw extruder for sheet extrusion, and performing biaxial tension and ultraviolet irradiation to obtain the modified polypropylene film.
Wherein the extrusion temperature is 270 ℃, the longitudinal stretching ratio is 4.0, the transverse stretching ratio is 7.0, and the ultraviolet radiation dose is 2000mJ/cm2。
Comparative example 1
A modified polypropylene film material for a capacitor comprises the following raw materials in parts by weight:
the preparation method of the modified barium titanate comprises the following steps:
preparing 34g of tetrabutyl titanate into a butanol solution with the mass percentage of 30%, adding the butanol solution into a high-pressure reaction kettle, then adding an aqueous solution containing 51g of barium hydroxide, uniformly stirring and mixing, then reacting the mixed solution at 120 ℃ for 12 hours, pouring an upper layer solution obtained by hydrothermal reaction after the reaction is finished, pouring acetic acid and deionized water, and then centrifuging, washing and drying to obtain barium titanate powder; and then 100g of barium titanate powder is added into 1mol/L hydrochloric acid solution for soaking, then filtration is carried out, calcination is carried out for 1h at 500 ℃, the mixture is cooled to room temperature and then added into ethanol solution, 0.5g of titanate coupling agent is added, and the modified barium titanate powder is obtained after full mixing and drying.
A preparation method of a modified polypropylene film material for a capacitor comprises the following steps:
(1) respectively weighing polypropylene, modified barium titanate, polyvinylidene fluoride, benzophenone, trimethylolpropane triacrylate, polyvinylidene fluoride hexafluoropropylene and an antioxidant 1010 according to a formula, adding the weighed materials into a mixer, stirring for 0.5h, adding the mixture into a double-screw extruder for granulation, wherein the extrusion temperature is 200 ℃, and drying after granulation is finished to obtain modified polypropylene master batches;
(2) and (2) adding the modified polypropylene master batch obtained in the step (1) into a single-screw extruder for sheet extrusion, and performing biaxial tension and ultraviolet irradiation to obtain the modified polypropylene film.
Wherein the extrusion temperature is 240 ℃, the longitudinal stretching ratio is 3.0, the transverse stretching ratio is 5.5, and the ultraviolet radiation dose is 1500mJ/cm2。
Comparative example 2
A modified polypropylene film material for a capacitor comprises the following raw materials in parts by weight:
the preparation method of the modified polypropylene comprises the following steps:
adding the perovskite powder into a mixture with a volume ratio of 1: 1, soaking the mixed solution of sodium carbonate and potassium permanganate in the mixed solution for 3 hours, taking out and washing the mixed solution, calcining the mixed solution for 1 hour at the temperature of 500 ℃, cooling the calcined solution, and then carrying out ball milling and sieving to obtain modified perovskite powder; adding 100 parts of polypropylene, 2 parts of triphenyl phosphite and 5 parts of modified perovskite powder into 800mL of dimethylbenzene, heating to 135 ℃ under the condition of stirring, reacting for 1h, then preserving the heat for 2h at 120 ℃, then reducing the temperature to room temperature at the speed of 1 ℃/min, filtering and drying to obtain the modified polypropylene.
A preparation method of a modified polypropylene film material for a capacitor comprises the following steps:
(1) respectively weighing modified polypropylene, barium titanate, polyvinylidene fluoride, benzophenone, trimethylolpropane triacrylate, polyvinylidene fluoride hexafluoropropylene and an antioxidant 1010 according to a formula, adding into a mixer, stirring for 0.5h, adding into a double-screw extruder for granulation, wherein the extrusion temperature is 200 ℃, and drying after granulation is finished to obtain modified polypropylene master batches;
(2) and (2) adding the modified polypropylene master batch obtained in the step (1) into a single-screw extruder for sheet extrusion, and performing biaxial tension and ultraviolet irradiation to obtain the modified polypropylene film.
Wherein the extrusion temperature is 24The longitudinal stretching ratio is 3.0 at 0 ℃, the transverse stretching ratio is 5.5, and the ultraviolet radiation dose is 1500mJ/cm2。
The films prepared in examples 1 to 4 of the present invention and comparative examples 1 to 2 were subjected to a performance test.
Wherein, the mechanical property test is carried out according to GB/T1040.3-2006 (part 3 for measuring the tensile property of plastics: the test condition of films and sheets); the breakdown strength is tested by a program-controlled withstand voltage tester according to GB/T1408.1-2016 (insulating material electrical strength test method), the dielectric constant is tested by a radio frequency impedance material analyzer, the dielectric loss factor is tested by a radio frequency impedance material analyzer, and the results are shown in the following table 1:
TABLE 1 Performance test results for modified Polypropylene films
As can be seen from the data analysis of Table 1, the modified polypropylene film material prepared by the invention is beneficial to improving the dielectric constant and the breakdown strength of the polypropylene film by modifying polypropylene and barium titanate, and simultaneously can keep a lower dielectric loss factor; the dielectric constant of comparative example 1 in which no modified polypropylene was added and comparative example 2 in which no modified barium titanate was added were not significantly improved, and the dielectric loss was also high. Meanwhile, the added photoinitiator benzophenone and the crosslinking agent are used as functional additives, so that the function of the whole modified polypropylene film is achieved, the crosslinking function of the modified polypropylene film can be exerted, and the integral performance of the modified polypropylene film is also influenced to a certain extent. From the above, it can be seen that: the modified polypropylene film material prepared by the invention has the advantages of pressure resistance, high dielectric constant, low dielectric loss factor and high breakdown strength.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The modified polypropylene film material for the capacitor is characterized by comprising the following raw materials in parts by weight:
2. the modified polypropylene film material for capacitors as claimed in claim 1, wherein the preparation process of the modified polypropylene comprises the following steps:
s21, adding the perovskite powder into a mixture with the volume ratio of 1: soaking the mixed solution of the sodium carbonate and the potassium permanganate of the 1 for 3-4h, taking out and washing, calcining for 1-3h at the temperature of 500-600 ℃, cooling, ball-milling and sieving to obtain modified perovskite powder;
s22, adding polypropylene, triphenyl phosphite and the modified perovskite powder obtained in the step (1) into dimethylbenzene, heating to 135 ℃ under the condition of stirring, preserving heat after the reaction is finished, then cooling to room temperature at a certain speed, filtering and drying to obtain the modified polypropylene.
3. The modified polypropylene film material for capacitor as claimed in claim 2, wherein the reaction time in step S22 is 1-2h, the temperature preservation time is 2-4h, and the temperature preservation temperature is 120-130 ℃; the cooling rate is 1-2 ℃/min.
4. The modified polypropylene film material for capacitors claimed in claim 2, wherein the mass ratio of the polypropylene, triphenyl phosphite and modified perovskite in step S22 is 100: 2-4: 5-10.
5. The modified polypropylene film material for capacitors as claimed in claim 1, wherein the preparation process of the modified barium titanate comprises the following steps:
s51, preparing tetrabutyl titanate into a butanol solution with the mass percentage of 30%, adding the butanol solution into a high-pressure reaction kettle, then adding a barium hydroxide aqueous solution, uniformly stirring and mixing, then reacting the mixed solution at the temperature of 120-160 ℃ for 12-24 hours, pouring an upper layer solution obtained by hydrothermal reaction after the reaction is finished, pouring acetic acid and deionized water, and then centrifuging, washing and drying to obtain barium titanate powder;
s52, adding the barium titanate powder obtained in the step S51 into 1mol/L hydrochloric acid solution for soaking, then filtering, calcining at 500 ℃ for 1-2h, cooling to room temperature, adding into ethanol solution, adding titanate coupling agent, fully mixing, and drying to obtain the modified barium titanate powder.
6. The modified polypropylene film material for capacitors as claimed in claim 5, wherein the molar ratio of tetrabutyl titanate to barium hydroxide in step S51 is 1: 3, in the step S52, the mass ratio of the barium titanate powder to the titanate coupling agent is 100: 0.5-1.
7. The modified polypropylene film material for capacitor as claimed in claim 1, wherein the cross-linking agent is one or more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, pentaerythritol triacrylate; the compatilizer is one or more of polyvinylidene fluoride hexafluoropropylene and maleic anhydride grafted polypropylene; the antioxidant is one or more of antioxidant 1010, antioxidant 168 and antioxidant 1098.
8. A method for preparing a modified polypropylene film material for capacitors as claimed in any one of claims 1 to 7, comprising the steps of:
s81, respectively weighing modified polypropylene, modified barium titanate, polyvinylidene fluoride, benzophenone, a cross-linking agent, a compatilizer and an antioxidant according to a formula, adding the weighed materials into a mixer, stirring for 0.5-1h, adding the materials into a double-screw extruder for granulation, wherein the extrusion temperature is 190-250 ℃, and drying after the granulation is finished to obtain modified polypropylene master batches;
s82, adding the modified polypropylene master batch obtained in the step S81 into a single-screw extruder for sheet extrusion, and obtaining the modified polypropylene film after biaxial stretching and ultraviolet irradiation.
9. The method as claimed in claim 8, wherein the extrusion temperature in step S82 is 220-270 ℃, the longitudinal stretching ratio is 3.0-4.0, the transverse stretching ratio is 5.5-7.0, and the UV irradiation dose is 1500-2000mJ/cm2。
10. Use of the modified polypropylene film material of any one of claims 1 to 7 in a capacitor.
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