CN111117064A - Polypropylene composite material and preparation method thereof - Google Patents
Polypropylene composite material and preparation method thereof Download PDFInfo
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- CN111117064A CN111117064A CN201911337340.2A CN201911337340A CN111117064A CN 111117064 A CN111117064 A CN 111117064A CN 201911337340 A CN201911337340 A CN 201911337340A CN 111117064 A CN111117064 A CN 111117064A
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention provides a low dielectric polypropylene composite material, which is prepared by adding a certain amount of nitrogen with the specific adsorption surface area of more than or equal to 300m2The carbon black per gram can reduce the addition amount of the carbon black, thereby improving the increase of the dielectric constant and the dielectric loss caused by the excessive addition amount of the carbon black. Can be used for the interior and exterior trimming parts of the automobile with the requirement on dielectric.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a low-dielectric polypropylene composite material and a preparation method thereof.
Background
The polypropylene is used as a general plastic with high cost performance, has the characteristics of high strength, high toughness, excellent mechanical property, chemical resistance, high heat resistance and the like after being modified, is widely applied to household appliances and automobile products, and the polypropylene product used as a decorating part needs color matching treatment, wherein the color matching of the automobile product is mostly black, and the black tone of the polypropylene is mainly realized by adding carbon black, so that the influence of carbon black dispersion on the blackness and glossiness of the product is also considered.
However, since carbon black is poor in dispersibility, tends to agglomerate during melt-kneading of polypropylene, and it is considered by those skilled in the art that carbon black having a smaller fineness (having a large specific surface area) tends to agglomerate more easily, carbon black having a nitrogen adsorption specific surface area in the range of less than 250m is often used2The result is that excessive carbon black is required to be added in the color matching of high-blackness products, the problem of dispersibility is also introduced, the gloss of the material is influenced, and the dielectric constant and the dielectric loss of the material are increased more.
Patent CN 101704974A discloses a preparation method of high-gloss polypropylene containing carbon black colorant, which adopts a pre-dispersion method of carbon black and a dispersant to improve the dispersibility of the carbon black, and the particle size of the selected carbon black is 13-70 microns, so that high-black color matching cannot be achieved, and the preparation method is only limited to common products with low requirement on blackness; in addition, CN 106854308A discloses aThe preparation method of the high-gloss black impact polypropylene also does not limit the carbon black, and the nitrogen adsorption specific surface area range of the carbon black contained in the color master batch selected by the preparation method can be presumed to fall within the range of 200-250m2In the range of/g, and it can be seen from the examples that if the L value is less than 25, the addition amount of the black master is as high as 3-4%, and the dispersion defect of the carbon black is caused at such a high addition ratio, and the addition of the high-content master leads to the deterioration of the dielectric property of the polypropylene.
Disclosure of Invention
The invention aims to provide a polypropylene composite material which has low dielectric constant and high glossiness under the premise of high black color matching.
Another object of the present invention is to provide a method for preparing the low dielectric polypropylene composite material.
The invention is realized by the following technical scheme:
a low dielectric polypropylene composite material comprises the following components in parts by weight:
100 parts of homopolymerized polypropylene resin;
1-3 parts of carbon black;
0-30 parts of a filler;
the nitrogen adsorption specific surface area of the carbon black is more than or equal to 300m2/g。
Preferably, the nitrogen adsorption specific surface area of the carbon black is more than or equal to 350m2/g。
The polypropylene composite material of the present invention has a dielectric constant of less than 2.40.
The melt mass flow rate of the homopolymerized polypropylene is 1-100 g/10min at 230 ℃ under the load of 2.16 Kg.
The nitrogen adsorption specific surface area mainly reflects the particle size information of carbon black.
In order to stiffen polypropylene composites, it is often necessary to add a certain amount of filler. However, the conventional fillers (such as talc powder and mica powder) not only easily cover the carbon black, but also reduce the surface gloss of the polypropylene resin and reduce the dielectric properties of the composite material to different degrees. Experiments show that the covering rate of calcium carbonate and barium sulfate to carbon black is low, so that the blackness of the filled polypropylene composite material can be ensured, the surface gloss is not greatly reduced, and the reduction of dielectric property caused by the addition of the filler can be improved.
Preferably, the filler is at least one selected from calcium carbonate and barium sulfate.
More preferably, it is selected from calcium carbonate.
The mesh number of the calcium carbonate and the barium sulfate is less than 5000 meshes.
A certain amount of toughening agent can be added, and the toughening agent also comprises 0 to 25 parts by weight; the toughening agent is selected from at least one of POE, SEBS and EPDM.
POE (polyolefin elastomer) is a polyolefin elastomer;
SEBS (styrene ethylene styrene block copolymer) is a linear triblock copolymer which takes polystyrene as a terminal block and takes an ethylene-butylene copolymer obtained by hydrogenation of polybutadiene as a middle elastic block;
EPDM (ethylene Propylene Diene monomer) is also known as ethylene Propylene Diene monomer;
in order to improve the processing performance or the light stability, 0-2 parts of an auxiliary agent is also included according to the parts by weight; the auxiliary agent is at least one selected from an antioxidant, a lubricant and a light stabilizer.
The antioxidant can be hindered phenol and phosphite antioxidant, specifically one or a mixture of two or more of 1010, 1076, 3114, 168 and PEP-36;
the light stabilizer can be hindered amine light stabilizer, specifically can be one or a mixture of two or more of UV-3808PP5, LA-402XP and LA-402 AF;
the lubricant can be one or a mixture of two or more of silicones, esters, amides, polyethylenes, stearic acids, fatty acids and esters;
the method comprises the following steps: firstly, mixing carbon black and polypropylene with the weight 1-5 times of that of the carbon black to obtain carbon black/polypropylene particles, uniformly mixing the carbon black/polypropylene particles with the rest polypropylene and other components, adding the mixture into a double-screw extruder, carrying out melt mixing at the temperature of 170-220 ℃ and the screw rotation speed of 350-450 rpm, and carrying out extrusion granulation to obtain the low-dielectric polypropylene composite material; the screw rod original paper adopts high shear setting.
The high shear setting can better disperse the carbon black in the polypropylene resin matrix to ensure high black chroma and low dielectric property under the condition of small carbon black adding amount.
Compared with the prior art, the invention has the following beneficial effects:
the prior art mainly adopts that the nitrogen adsorption specific surface area is less than 250m2However, such carbon black is inferior in blackening effect and requires a large amount of addition to obtain a high black color, which results in a significant increase in dielectric constant and dielectric loss of the resin matrix. The nitrogen adsorption specific surface area is more than or equal to 300m2The carbon black per gram can obtain high black color matching under a small adding amount, has low agglomeration and low dielectric constant, and is prepared by high shear and sufficient for shearing and dispersing carbon powder.
Furthermore, experiments show that the addition of calcium carbonate and barium sulfate does not cover the carbon black in the resin matrix and does not greatly reduce the surface gloss of the resin matrix.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw materials used in the invention are derived from commercial products:
polypropylene resin a: lanzhou petrochemical PP H9018, homo-polypropylene;
polypropylene resin B: zhonghai shell brand EP548R, copolypropylene;
carbon black A: nitrogen adsorption specific surface area about 375m2/g；
Carbon black B: nitrogen adsorption specific surface area about 300m2/g；
Carbon black C: the nitrogen adsorption specific surface area is about 270m2/g；
Carbon black D: nitrogen adsorption specific surface area about equal to 195m2/g；
Barium sulfate: 1250 mesh;
calcium carbonate: 1250 mesh;
talc powder: 1250 mesh;
mica powder: 1250 mesh;
POE: dow ENGAGE 8137;
lubricant: a stearic acid-based lubricant;
antioxidant: an antioxidant 168;
examples and comparative examples preparation methods of polypropylene composites: firstly, mixing carbon black and polypropylene with the weight 1-5 times of that of the carbon black to obtain carbon black/polypropylene particles, uniformly mixing the carbon black/polypropylene particles with the rest of the polypropylene, POE, barium sulfate, lubricant and antioxidant, adding the mixture into a double-screw extruder, carrying out melt mixing at the temperature of 170-220 ℃ and the screw rotation speed of 350-450 rpm, and carrying out extrusion granulation to obtain the low-dielectric polypropylene composite material; the screw rod original paper adopts high shear setting.
The performance test method comprises the following steps:
the preparation method of the test sample plate comprises the following steps: the modified particles were injection molded by double-sided mirror polishing to prepare a 10mm by 5mm by 1.5mm sample plate.
L value: the sample is placed in an Alice Color-Eye 7000A colorimeter, an SCI mode is set, and an L value test is carried out to evaluate the blackness of the material (the lower the L value is, the higher the blackness is).
60 ° gloss: the 60 ° angle gloss was measured by a BYK Pvlt0925 gloss meter.
Dielectric constant: the N5225A vector network analyzer was used to test the dielectric constant and loss tangent of the coupons by transmission line reflectometry and setting the frequency at 76-77 GHz.
Table 1: the components of the polypropylene composite material of the example are proportioned and the results of the performance tests
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Polypropylene resin A | 100 | 100 | 100 | 100 | 100 |
| Carbon Black A | 1 | 1.5 | 2.5 | 1.5 | |
| Carbon Black B | 1.5 | ||||
| Barium sulfate | 20 | 20 | 20 | 20 | |
| Calcium carbonate | 20 | ||||
| POE | 4 | 4 | 4 | 4 | 4 |
| Lubricant agent | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
| Antioxidant agent | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
| Value of L | 23.71 | 23.43 | 23.06 | 23.97 | 23.38 |
| 60 degree gloss | 85.3 | 85.4 | 85.7 | 85.3 | 85.6 |
| Dielectric constant | 2.34 | 2.35 | 2.38 | 2.36 | 2.34 |
| Loss tangent value | 0.0084 | 0.0088 | 0.0094 | 0.0089 | 0.0087 |
From examples 1 to 3, it can be seen that nitrogen adsorption was usedThe specific surface area is about 375m2The amount of carbon black used per g is increased to increase the degree of blackness, but the range of increase in dielectric constant and loss tangent is not so large.
From example 2/4, it is preferable that the nitrogen adsorption specific surface area is larger than 350m2Carbon black per gram.
Table 2:
| example 6 | Example 7 | Example 8 | |
| Polypropylene resin A | 100 | 100 | 100 |
| Carbon Black A | 1.5 | 1.5 | 1.5 |
| Barium sulfate | |||
| Calcium carbonate | |||
| Mica powder | 20 | ||
| Talcum powder | 20 | ||
| POE | 4 | 4 | 4 |
| Lubricant agent | 0.4 | 0.4 | 0.4 |
| Antioxidant agent | 0.4 | 0.4 | 0.4 |
| Value of L | 23.06 | 24. 53 | 24.37 |
| 60 degree gloss | 88.9 | 78.3 | 79.3 |
| Dielectric constant | 2.28 | 2.40 | 2.38 |
| Loss tangent value | 0.0024 | 0.0096 | 0.0095 |
From example 2/5/6/7/8, it is understood that the addition of the inorganic filler can hide the carbon black, resulting in a decrease in blackness and gloss. However, the barium sulfate and the calcium carbonate which are preferred in the invention can reduce the covering of the carbon black and improve the reduction of the glossiness; calcium carbonate is more preferred.
Table 2: the polypropylene composite material of the comparative example comprises the components in proportion and the performance test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparison ofExample 4 | Comparative example 5 | |
| Polypropylene resin A | 100 | 100 | 100 | 100 | |
| Polypropylene resin B | 100 | ||||
| Carbon Black A | 1.5 | ||||
| Carbon Black C | 1.5 | 3 | |||
| Carbon Black D | 1.5 | 3 | |||
| Barium sulfate | 20 | 20 | 20 | 20 | 20 |
| Mica powder | |||||
| Talcum powder | |||||
| POE | 4 | 4 | 4 | 4 | 4 |
| Lubricant agent | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
| Antioxidant agent | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
| Value of L | 24.84 | 24.25 | 25.16 | 24.86 | 23.82 |
| 60 degree gloss | 85.4 | 85.1 | 85.2 | 84.9 | 52.6 |
| Dielectric constant | 2.37 | 2.45 | 2.37 | 2.46 | 2.36 |
| Loss tangent value | 0.0090 | 0.0124 | 0.0089 | 0.0121 | 0.0086 |
As can be seen from comparative examples 1 to 4, the nitrogen adsorption specific surface area was less than 300m2The carbon black/g has a low blackening effect, and the degree of blackness can be increased only by increasing the amount of carbon black. However, this causes a decrease in dielectric properties (an increase in dielectric constant and loss tangent).
Claims (10)
1. The polypropylene composite material is characterized by comprising the following components in parts by weight:
100 parts of homopolymerized polypropylene resin;
1-3 parts of carbon black;
the nitrogen adsorption specific surface area of the carbon black is more than or equal to 300m2/g；
0-30 parts of filler.
2. The polypropylene composite material according to claim 1, wherein the carbon black has a nitrogen adsorption specific surface area of 350m or more2/g。
3. The polypropylene composite of claim 1, wherein the polypropylene composite has a dielectric constant of less than 2.40.
4. The polypropylene composite material according to claim 1, wherein the melt mass flow rate of the homo-polypropylene is 1-100 g/10min at 230 ℃ and under a load of 2.16 Kg.
5. The polypropylene composite of claim 1, wherein the filler is at least one selected from the group consisting of calcium carbonate and barium sulfate.
6. The polypropylene composite according to claim 5, selected from calcium carbonate.
7. The polypropylene composite according to claim 5, wherein the mesh size of the calcium carbonate and barium sulfate is less than 5000 mesh.
8. The polypropylene composite of claim 1, further comprising 0 to 25 parts by weight of a toughening agent; the toughening agent is selected from at least one of POE, SEBS and EPDM.
9. The polypropylene composite material according to claim 1, further comprising 0 to 2 parts by weight of an auxiliary; the auxiliary agent is at least one selected from an antioxidant, a lubricant and a light stabilizer.
10. A process for the preparation of a polypropylene composite according to any one of claims 1 to 9, comprising the steps of: firstly, mixing carbon black and polypropylene with the weight 1-5 times of that of the carbon black to obtain carbon black/polypropylene particles, uniformly mixing the carbon black/polypropylene particles with the rest polypropylene and other components, adding the mixture into a double-screw extruder, carrying out melt mixing at the temperature of 170-220 ℃ and the screw rotation speed of 350-450 rpm, and carrying out extrusion granulation to obtain a polypropylene composite material; the screw rod original paper adopts high shear setting.
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| CN201911337340.2A CN111117064B (en) | 2019-12-23 | 2019-12-23 | Polypropylene composite material and preparation method thereof |
| PCT/CN2020/124011 WO2021129115A1 (en) | 2019-12-23 | 2020-10-27 | Polypropylene composite material and preparation method therefor |
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| CN201911337340.2A CN111117064B (en) | 2019-12-23 | 2019-12-23 | Polypropylene composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021129115A1 (en) * | 2019-12-23 | 2021-07-01 | 金发科技股份有限公司 | Polypropylene composite material and preparation method therefor |
| CN114835927A (en) * | 2022-06-13 | 2022-08-02 | 昆山禾振瑞新复合材料有限公司 | Carbon black master batch for piano black high-impact polypropylene material capable of eliminating surface pits and preparation method of carbon black master batch |
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| CN111117064B (en) * | 2019-12-23 | 2021-11-12 | 金发科技股份有限公司 | Polypropylene composite material and preparation method thereof |
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| EP3495410A1 (en) * | 2017-12-11 | 2019-06-12 | Borealis AG | Polypropylene composition comprising carbonaceous structures and having improved mechanical properties |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021129115A1 (en) * | 2019-12-23 | 2021-07-01 | 金发科技股份有限公司 | Polypropylene composite material and preparation method therefor |
| CN114835927A (en) * | 2022-06-13 | 2022-08-02 | 昆山禾振瑞新复合材料有限公司 | Carbon black master batch for piano black high-impact polypropylene material capable of eliminating surface pits and preparation method of carbon black master batch |
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| Publication number | Publication date |
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| WO2021129115A1 (en) | 2021-07-01 |
| CN111117064B (en) | 2021-11-12 |
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