CN111961283A - High-dielectric-constant polypropylene composite material and preparation method thereof - Google Patents
High-dielectric-constant polypropylene composite material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- 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
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a high dielectric constant polypropylene composite material and a preparation method thereof, belonging to the technical field of high polymer materials. The high dielectric constant polypropylene composite material comprises the following raw materials in parts by weight: 53-93.9 parts of polypropylene, 1-15 parts of long-chain alkyl modified silsesquioxane, 5-30 parts of inorganic particles and 0.1-2 parts of antioxidant. Compared with the prior art, the composite method has the advantages of low cost, easiness in preparation, uniform filler dispersion and the like, and the polypropylene composite material has the dielectric property which is remarkably improved compared with the dielectric property of common polypropylene on the premise of not influencing the inherent excellent mechanical property, processability, thermal stability and crystallization property of the polypropylene.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a high dielectric constant polypropylene composite material and a preparation method thereof.
Background
The polypropylene has the advantages of stable electrical property, good temperature resistance, good mechanical property, low dielectric loss and the like, and is widely applied in the field of capacitor films. An ideal capacitor film material should have the following characteristics: high dielectric constant (high energy density), high breakdown strength, high temperature resistance (>150 ℃), low energy loss (low heat generation), excellent ideal performance and the like. However, due to the special hydrocarbon structure of polypropylene, polypropylene has a low dielectric constant and the energy density of the corresponding capacitor film is low. The polypropylene and the inorganic particles with high dielectric constant are compounded to realize the advantage complementation of the two, and the polypropylene composite material with high dielectric constant and low dielectric loss is hopeful to be prepared. The inorganic particles have small particle size and large surface energy, and are easy to agglomerate in the process of blending with propylene, so that the inorganic particles cannot be uniformly dispersed in a polypropylene matrix. The non-uniform dispersion of inorganic particles will result in too large a difference in internal properties of the material and increased defects. On one hand, the electric field distribution is not uniform at the defect or interface part, the ion leakage conductance is larger, and the breakdown strength is sharply reduced; on the other hand, the inhomogeneous distribution of the filler can also cause the poor mechanical property of the composite material, which is difficult to form a film on a large scale or be easily damaged in the using process, and is difficult to be utilized in the technical field of industrial production. In order to prepare polypropylene composites with excellent properties, it is necessary to surface-modify the inorganic filler or to improve the dispersibility of the inorganic filler using a compatibilizer.
In view of the problems in the prior art, the invention provides a high-dielectric-constant polypropylene composite material and a preparation method thereof, which can improve the dielectric property of the polypropylene composite material under the condition of lower cost and simultaneously maintain the excellent mechanical property, processability, thermal property and crystallization property of polypropylene.
Disclosure of Invention
The invention provides a high dielectric constant polypropylene composite material and a preparation method thereof, which adopts low-cost C30-45 alkyl modified propyl silsesquioxane and inorganic filler and a simple and easy compounding method to modify polypropylene, so that compared with common polypropylene, the dielectric property of polypropylene is improved at lower cost on the premise of not influencing the inherent excellent mechanical property, processing property, thermal property and crystallization property of polypropylene.
The invention is realized by the following technical scheme: the high-dielectric-constant polypropylene composite material comprises the following raw materials in parts by weight:
in the above technical solution, preferably, the polypropylene is a composition composed of one or two of isotactic polypropylene and syndiotactic polypropylene.
In the above technical solution, preferably, the polypropylene is a composition comprising one or more of isotactic polypropylene prepared by metallocene catalyst catalysis, syndiotactic polypropylene prepared by metallocene catalyst catalysis (respectively abbreviated as metallocene isotactic polypropylene and metallocene syndiotactic polypropylene), and isotactic polypropylene prepared by ziegler natta catalyst catalysis (abbreviated as ZN isotactic polypropylene).
In the above technical solution, preferably, the inorganic particles are a composition composed of any one or more of montmorillonite, mica, boron nitride, alumina, silica, titanium oxide, silicon carbide, silicon nitride, barium titanate, and barium strontium titanate.
In the above aspect, the inorganic particles are preferably fine inorganic particles having a particle diameter of 1 nm to 100 μm.
In the above technical solution, preferably, the refining treatment of the inorganic particles includes high power ultrasonic stripping, ball milling, pulverizing and physical grinding. The inorganic particles are spherical, fiber, lamellar or block, wherein the particle size of the refined spherical and block particles is 1-1000 nanometers, the fiber length of the fiber-shaped particles is 1-100 micrometers, and the thickness of the lamellar-shaped particles is 1-10 nanometers.
In the above technical solution, preferably, the long-chain alkyl modified silsesquioxane is C30-45 alkyl modified propyl silsesquioxane, and preferably, the long-chain alkyl modified silsesquioxane is C30-45 alkyl modified propyl silsesquioxane (Dow Corning Corp.) produced by Dow Corp
SW-8005 C30 Resin Wax)。
In the above-mentioned embodiment, preferably, the antioxidant is 2, 6-di-tert-butyl-p-cresol, pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 1,3, 5-trimethyl-2, 4,6- (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, 2' -methylenebis (4-ethyl-6-tert-butylphenol), 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, 4-hydroxydodecanoic acid anilide, 4-hydroxyoctadecanoic acid anilide, or the like, The composition is composed of one or more of tris (nonylphenyl) phosphite, tris (2, 4-di-tert-butylphenyl) phosphite, dioctadecyl pentaerythrityl diphosphite, tetrakis (2, 4-di-tert-butylphenyl) 4, 4' -biphenylene diphosphite, dilauryl thiodipropionate, calcium stearate, barium stearate, lead stearate, tribasic lead sulfate, magnesium oxide, hydrotalcite, zinc oxide and calcium lactate.
The preparation method of the high dielectric constant polypropylene composite material comprises the following steps:
(1) the raw materials for preparing the material comprise the following components in parts by weight:
(2) after polypropylene, long-chain alkyl modified silsesquioxane and an antioxidant are uniformly mixed, inorganic particles are added and continuously mixed until all components are uniformly mixed, and the obtained mixture is added into a double-screw extruder for extrusion and granulation to obtain the high-dielectric-constant polypropylene composite material particles.
In the above technical solution, preferably, in the step (2), the temperature of the extrusion granulation is 160-240 ℃, that is, the obtained mixture is added into a twin-screw extruder and extruded and granulated at 160-240 ℃ to obtain the particles of the high dielectric constant polypropylene composite material.
The long-chain alkyl modified silsesquioxane is a special organosilicon hybrid material with a silicon-oxygen-silicon structural unit, reactive silicon hydroxyl and long-chain alkyl. The long-chain alkyl modified silsesquioxane contains long-chain alkyl and has good compatibility with polypropylene, and the long-chain alkyl modified silsesquioxane can be used as a compatibilizer of polypropylene and inorganic filler to improve the dispersibility of the inorganic filler in a polypropylene matrix, thereby being beneficial to the preparation of a polypropylene composite material with high dielectric constant and low dielectric loss.
The invention has the beneficial effects that: compared with the prior art, the composite method has the advantages of low cost, easiness in preparation, uniform filler dispersion and the like, and the polypropylene composite material has the dielectric property which is remarkably improved compared with the dielectric property of common polypropylene on the premise of not influencing the inherent excellent mechanical property, processability, thermal stability and crystallization property of the polypropylene.
Drawings
FIG. 1 is a solid silicon spectrum of a compatibilizer long-chain alkyl modified silsesquioxane, which shows that the structure of the silsesquioxane contains a silicon-oxygen-silicon structural unit and a reactive silicon hydroxyl group.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way. Any person skilled in the art can substitute or change the technical solution of the present invention and its inventive concept within the technical scope of the present invention.
The following examples are only exemplary and are only used to explain and illustrate the technical solution of the present invention, but not to be construed as limiting the technical solution of the present invention.
The long chain alkyl modified silsesquioxanes described in the examples below are C30-45 alkyl modified propyl silsesquioxanes (Dow) manufactured by Dow Corning
SW-8005 C30 Resin Wax)。
The raw materials in the following examples are all in parts by weight.
Example 1
Weighing 70 parts of metallocene isotactic polypropylene, 8 parts of long-chain alkyl modified silsesquioxane, 21 parts of ball-milled and refined barium strontium titanate powder (spherical particles with the average particle size of 20 nm-100 mu m), 0.5 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4 hydroxyphenyl) propionic acid ] pentaerythritol ester and 0.5 part of antioxidant dilauryl thiodipropionate. Mixing polypropylene, an antioxidant and long-chain alkyl modified silsesquioxane, adding barium strontium titanate powder after uniformly mixing until the components are uniformly mixed, adding the obtained mixture into a double-screw extruder, and extruding and granulating to obtain the high-dielectric-constant polypropylene composite material particles. The temperature of the first temperature zone of the double-screw extruder is 210 ℃, the temperature of the second temperature zone is 220 ℃, the temperature of the third temperature zone is 220 ℃, the temperature of the fourth temperature zone is 220 ℃, the temperature of the fifth temperature zone is 220 ℃, the head temperature of the double-screw extruder is 210 ℃, the melt temperature is 190 ℃ and the feeding speed is 30 r/min. The composite film base material (the particles of the polypropylene composite material) is placed in a flat vulcanizing machine, and film pressing is carried out for 300s at 2Mpa and 220 ℃, so as to prepare the polypropylene composite material film with the thickness of 25 microns. And comparing the dielectric property with that of common polypropylene (the common polypropylene film with the thickness of 25 microns is prepared by placing metallocene isotactic polypropylene in a flat vulcanizing machine and pressing the film for 300s at the temperature of 220 ℃ and under the pressure of 2 Mpa).
Example 2
Weighing 50 parts of metallocene isotactic polypropylene, 20 parts of ZN isotactic polypropylene, 5 parts of long-chain alkyl modified silsesquioxane, 24.5 parts of barium titanate (irregular sheet shape, length and width of 50 nm-100 mu m and average thickness of 2-100 nm) ground and refined by a mortar, and 0.5 part of antioxidant 1,3,5 trimethyl-2, 4,6- (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene. Mixing polypropylene, an antioxidant and long-chain alkyl modified silsesquioxane, adding barium titanate after uniformly mixing until the components are uniformly mixed, adding the obtained mixture into a double-screw extruder, and extruding and granulating to obtain the high-dielectric-constant polypropylene composite material particles. The temperature of the first temperature zone of the double-screw extruder is 200 ℃, the temperature of the second temperature zone is 210 ℃, the temperature of the third temperature zone is 215 ℃, the temperature of the fourth temperature zone is 215 ℃, the temperature of the fifth temperature zone is 220 ℃, the head temperature of the double-screw extruder is 200 ℃, the melt temperature is 195 ℃, and the feeding speed is 15 r/min. The composite film base material (the particles of the polypropylene composite material) is placed in a flat vulcanizing machine, and film pressing is carried out for 300s at 5Mpa and 210 ℃, so as to prepare the polypropylene composite material film with the thickness of 25 microns.
Example 3
89 parts of ZN isotactic polypropylene, 2.5 parts of long-chain alkyl modified silsesquioxane, 8 parts of boron nitride (irregular sheet shape, length and width of 50 nm-100 mu m and average thickness of 2-80 nm) ground and refined by a mortar and 0.5 part of antioxidant 1,3,5 trimethyl-2, 4,6- (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene are weighed. Mixing polypropylene, an antioxidant and long-chain alkyl modified silsesquioxane, adding a physically ground and refined boron nitride sheet after uniformly mixing, adding the obtained mixture into a double-screw extruder, and carrying out extrusion granulation to obtain the high-dielectric-constant polypropylene composite material particles. The temperature of the first temperature zone of the double-screw extruder is 220 ℃, the temperature of the second temperature zone is 230 ℃, the temperature of the third temperature zone is 225 ℃, the temperature of the fourth temperature zone is 225 ℃, the temperature of the fifth temperature zone is 230 ℃, the head temperature of the double-screw extruder is 220 ℃, the melt temperature is 200 ℃ and the feeding speed is 40 r/min. The composite film base material is placed in a flat vulcanizing machine, and film pressing is carried out for 300s at the temperature of 215 ℃ under the pressure of 5Mpa, so as to prepare the polypropylene composite film with the thickness of 25 microns.
Example 4
60 parts of ZN isotactic polypropylene, 15 parts of metallocene syndiotactic polypropylene, 7 parts of long-chain alkyl modified silsesquioxane, 17 parts of boron nitride powder (spherical particles with the average particle size of 50 nm-100 mu m) ground and refined by a mortar and 1 part of antioxidant 1, 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane are weighed. Mixing polypropylene, an antioxidant and long-chain alkyl modified silsesquioxane, adding boron nitride powder after uniformly mixing until all components are uniformly mixed, adding the obtained mixture into a double-screw extruder, and extruding and granulating to obtain the high-dielectric-constant polypropylene composite material particles. The temperature of a first temperature zone of the double-screw extruder is 200 ℃, the temperature of a second temperature zone is 210 ℃, the temperature of a third temperature zone is 205 ℃, the temperature of a fourth temperature zone is 205 ℃, the temperature of a fifth temperature zone is 200 ℃, the head temperature of the double-screw extruder is 200 ℃, the melt temperature is 180 ℃, and the feeding speed is 30 r/min. The composite film base material (the particles of the polypropylene composite material) is placed in a flat vulcanizing machine, and film pressing is carried out for 300s at 2Mpa and 220 ℃, so as to prepare the polypropylene composite material film with the thickness of 25 microns.
Table 1 shows the dielectric properties of the polypropylene composite materials and the common polypropylene in examples 1-3 according to GB/T1409-2006 test standard. As can be seen from table 1, the polypropylene composite material has a higher dielectric constant than ordinary polypropylene, while maintaining a higher breakdown strength and a lower dielectric loss value.
Table 2 shows examples 1-3 table 1 the mechanical properties, thermal stability and crystallization properties of the polypropylene composites of examples 1-3 are compared with those of conventional polypropylene. It can be seen that the mechanical properties, processability (melt index), thermal properties (thermal stability) and crystallization properties of the polypropylene composite are superior or comparable to those of ordinary polypropylene.
TABLE 1 dielectric Properties of Polypropylene composites in examples 1-3 compared to ordinary Polypropylene
| Dielectric constant | Breakdown Strength (MV/m) | Dielectric loss | |
| Example 1 | 3.2 | 380 | 0.8％ |
| Example 2 | 3.5 | 400 | 0.7％ |
| Example 3 | 2.9 | 430 | 0.5％ |
| Metallocene isotactic polypropylene | 2.2 | 300 | 1.1％ |
TABLE 2 comparison of mechanical, processing, thermal and crystallization Properties of the Polypropylene composites of examples 1-3 with ordinary Polypropylene
Note: the melt index test is carried out according to the national standard, the temperature is 230 ℃, and the weight is 2.16 kg;
a second heating curve, heating from 30 ℃ to 200 ℃ at 10 ℃/min;
# Nitrogen atmosphere, 10 ℃/min temperature increase from 30 ℃ to 700 ℃.
Claims (10)
1. A high dielectric constant polypropylene composite material is characterized in that: the composite material comprises the following raw materials in parts by weight:
2. the high dielectric constant polypropylene composite of claim 1, wherein: the polypropylene is a composition consisting of one or two of isotactic polypropylene and syndiotactic polypropylene.
3. The high dielectric constant polypropylene composite of claim 1, wherein: the polypropylene is a composition consisting of any one or more of isotactic polypropylene prepared by metallocene catalyst catalysis, syndiotactic polypropylene prepared by metallocene catalyst catalysis and isotactic polypropylene prepared by Ziegler Natta catalyst catalysis.
4. The high dielectric constant polypropylene composite of claim 1, wherein: the inorganic particles are a composition consisting of any one or more of montmorillonite, mica, boron nitride, alumina, silicon oxide, titanium oxide, silicon carbide, silicon nitride, barium titanate or barium strontium titanate.
5. The high dielectric constant polypropylene composite of claim 1, wherein: the particle size of the inorganic particles is 1 nanometer to 100 micrometers.
6. The high dielectric constant polypropylene composite of claim 5, wherein: the inorganic particles are spherical, fiber, lamella or block, wherein the particle diameter of the spherical and block particles is 1-1000 nm, the fiber length of the fiber-shaped particles is 1-100 microns, and the thickness of the lamella-shaped particles is 1-10 nm.
7. The high dielectric constant polypropylene composite of claim 1, wherein: the long-chain alkyl modified silsesquioxane is C30-45 alkyl modified propyl silsesquioxane.
8. The high dielectric constant polypropylene composite of claim 1, wherein: the antioxidant is 2, 6-di-tert-butyl-p-cresol, tetra [ beta- (3, 5-di-tert-butyl-4 hydroxyphenyl) propionic acid ] pentaerythritol ester, 1,3, 5-trimethyl-2, 4,6- (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, 2' -methylenebis (4-ethyl-6-tert-butylphenol), 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, 4-hydroxydodecanoic acid anilide, 4-hydroxyoctadecanoic acid anilide, tris (nonylphenyl) phosphite, Tri (2, 4-di-tert-butylphenyl) phosphite, dioctadecyl pentaerythritol diphosphite, tetra (2, 4-di-tert-butylphenyl) 4, 4' -biphenylene diphosphate, dilauryl thiodipropionate, calcium stearate, barium stearate, lead stearate, tribasic lead sulfate, magnesium oxide, hydrotalcite, zinc oxide, calcium lactate.
9. The method for preparing a high dielectric constant polypropylene composite material according to any one of claims 1 to 8, wherein: the method comprises the following steps:
after polypropylene, long-chain alkyl modified silsesquioxane and an antioxidant are uniformly mixed, inorganic particles are added and continuously mixed until all components are uniformly mixed, and the obtained mixture is added into a double-screw extruder for extrusion and granulation to obtain the granules of the polypropylene composite material.
10. The method as claimed in claim 9, wherein the temperature of the extrusion granulation is 160-240 ℃.
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| CN114957841A (en) * | 2022-08-02 | 2022-08-30 | 沧州洁通塑料有限公司 | High-strength HDPE double-wall corrugated pipe and preparation method thereof |
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| CN114957841A (en) * | 2022-08-02 | 2022-08-30 | 沧州洁通塑料有限公司 | High-strength HDPE double-wall corrugated pipe and preparation method thereof |
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Application publication date: 20201120 |