CN111621088A - Conductive polypropylene material and preparation method thereof - Google Patents
Conductive polypropylene material and preparation method thereof Download PDFInfo
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- CN111621088A CN111621088A CN201910148373.6A CN201910148373A CN111621088A CN 111621088 A CN111621088 A CN 111621088A CN 201910148373 A CN201910148373 A CN 201910148373A CN 111621088 A CN111621088 A CN 111621088A
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- 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
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- 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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—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
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The invention discloses a conductive polypropylene material and a preparation method thereof, wherein the conductive polypropylene material is prepared from 20-70 parts of PP; 20-60 parts of conductive carbon black master batch; 10-20 parts of calcium carbonate(ii) a 0.5-1.0 part of main antioxidant; 0.5-1.0 part of auxiliary antioxidant; 10.2 to 0.5 portion of dispersant is prepared by mixing, extruding and granulating; wherein the conductive carbon black master batch is prepared from 40 parts of high-pressure low-density polyethylene; 25 parts of a lubricant; and 35 parts of conductive carbon black by banburying. The surface resistivity of the conductive polypropylene material prepared by the invention can be reduced to 103The conductive carbon black master batch can make the conductivity of the conductive polypropylene material more uniform.
Description
Technical Field
The invention belongs to the technical field of polymer processing, and particularly relates to a conductive polypropylene material and a preparation method thereof.
Background
Polypropylene (PP) is a crystalline polymer with regular structure, usually white granules or powder, and is a tasteless, nontoxic, and light thermoplastic resin; the high-strength and high-flexibility composite material has the characteristics of easiness in processing, high impact strength, high flexibility, high electrical insulation and the like, has high chemical resistance, and is widely applied to the fields of automobile industry, household appliances, electronics, packaging, building materials, furniture and the like. Because the chemical resistance of the polypropylene material is good, the polypropylene material can be used as a material for batteries of electric automobiles, and thus the polypropylene material is required to have certain conductivity.
Chinese patent (CN 103739945B) discloses a conductive polypropylene composite material, which is realized by the following components: 50-70 parts of polypropylene, 5-20 parts of conductive carbon black, 2-10 parts of carbon fiber, 8-15 parts of antimony trioxide, 8-15 parts of strontium oxide, 2-8 parts of coupling agent and 10-15 parts of toughening agent. The surface resistivity of the conductive polypropylene composite material made of the material is 106Omega. Chinese patent (CN 107698870A) discloses a polypropylene composition and a preparation method thereof, wherein the polypropylene composition is prepared by adding components such as conductive carbon black, conductive grease, glass fiber, coupling agent, antioxidant and the like into the polypropylene composition, so that the surface resistivity of the polypropylene composition is 105Omega, and has certain antistatic capacity. The surface resistivity of the general conductive polypropylene material is required to reach 104Omega is less, but the modified polypropylene material is only a better antistatic material, and the surface resistivity of the material is 105Ω-106Omega, the requirement cannot be met.
Disclosure of Invention
In view of the above limitations of the prior art, the present invention aims to provide a conductive polypropylene material and a preparation method thereof.
The technical scheme of the invention is as follows:
the conductive polypropylene material is prepared from the following components in parts by weight:
the conductive carbon black master batch is prepared from the following components in parts by weight:
40 parts of high-pressure low-density polyethylene;
25 parts of a lubricant;
and 35 parts of conductive carbon black.
In a further scheme, the melt index of the high-pressure low-density polyethylene in the conductive carbon black master batch is 1.5g/10min under the condition of 190 ℃/2.16kg, the lubricant is silicone powder or erucamide, and the particle size of the conductive carbon black is 40 nm.
The polypropylene is homopolymerized polypropylene, and the melt index of the polypropylene is 40-60g/10min under the condition of 190 ℃/2.16 kg.
The mesh number of the calcium carbonate is 2000-5000 meshes.
The main antioxidant is hindered phenol antioxidant; the auxiliary antioxidant is phosphite antioxidant.
The hindered phenol antioxidant is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010) or beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester (antioxidant 1076); the phosphite ester antioxidant is tris [2, 4-di-tert-butylphenyl ] phosphite (antioxidant 168).
The dispersing agent 1 is white oil or polyethylene wax, and the dispersing agent 2 is erucamide or calcium stearate.
Another object of the present invention is to provide a method for preparing the above conductive polypropylene material, which comprises the following steps:
(1) firstly, adding 40 parts of high-pressure low-density polyethylene, 25 parts of lubricant and 35 parts of conductive carbon black into an internal mixer for internal mixing, and then introducing the mixture into a single-screw extruder for granulation to obtain conductive carbon black master batches;
(2) firstly, 10.2 to 0.5 part of dispersant and 10 to 30 parts of calcium carbonate are put into a high-speed mixer and mixed for 3 to 8min at the temperature of between 80 and 90 ℃;
(3) cooling the high-speed mixer to room temperature, and adding 20-70 parts of polypropylene, 20-60 parts of conductive carbon black master batch, 0.5-1.0 part of main antioxidant, 0.5-1.0 part of auxiliary antioxidant and 20.2-0.5 part of dispersing agent; continuously mixing for 3-8 min;
(4) and (4) adding the mixed material obtained in the step (3) into a double-screw extruder for extrusion granulation to obtain the conductive polypropylene material.
Further, the temperature of the internal mixer in the step (1) is 160-180 ℃, and the temperature of each section of the single-screw extruder is 180-200 ℃; the temperature of each zone of the double-screw extruder in the step (4) is 180-220 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. the conductive carbon black master batch prepared from the high-pressure low-density polyethylene, the lubricant and the conductive carbon black is used, so that the conductive carbon black is favorably and uniformly dispersed in a polypropylene matrix to achieve the uniformity of the conductivity of the polypropylene composition; on the other hand, the conductive carbon black master batch is used instead of the conductive carbon black directly so as to ensure that the workshop processing environment is better.
2. In the preparation method of the composition, the dispersant 1 and the calcium carbonate are mixed firstly, so that the surface of the calcium carbonate is treated, and the calcium carbonate can be more uniformly dispersed in a polypropylene matrix. The calcium carbonate is added for reducing cost and improving elongation at break, the calcium carbonate in the formula is added with the conductive carbon black, the inorganic filler has high filling amount, and the aim of pretreatment is to plasticize uniformly when passing through a double-screw extruder. The purpose of adding the dispersant 2 is as follows: the external lubricity of the double-screw extruder is increased, and the condition that the material is easy to generate by high inorganic filling amount and the material is easy to generate and is emitted from a vacuum port due to back pressure increase is avoided.
3. The matrix of the conductive carbon black master batch is LDPE, the melting point is about 112 ℃, the premixing temperature is 80-90 ℃, the conductive carbon black master batch can be softened at the high temperature of premixing to cause mixing and agglomeration, so that the temperature of a high-speed mixer is reduced after the calcium carbonate is premixed.
Detailed Description
The present invention will be further described with reference to the following examples.
The length-diameter ratio of the twin-screw extruder used in the examples of the present invention was 40: 1, the manufacturer is the company BraBEBDER, Germany.
The flow rate of the polypropylene melt used below is 50g/10min at 190 ℃/2.16kg, and the calcium carbonate is 3000 meshes;
the antioxidant 1010, antioxidant 168, white oil, polyethylene wax, erucamide and silicone powder are commercially available.
The product of the invention adopts ISO standard to test, the extruded granules are molded by an injection molding machine to obtain a test sample strip, and the performance test is carried out after the test sample strip is stabilized for 24 hours under the conditions of 23 ℃ and 50 percent of relative humidity, and the physical and mechanical performance tests are carried out as follows:
melt index: preparing and testing according to ISO 1133 standard;
surface resistivity: the samples were tested according to IEC 62631 standard.
Example 1
(1) Firstly, 0.2 part of white oil and 10 parts of calcium carbonate are put into a high-speed mixer and mixed for 3min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 70 parts of PP, 20 parts of conductive carbon black master batches, 10100.5 parts of antioxidant, 1680.5 part of antioxidant and 0.2 part of erucamide; continuously mixing for 3 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
Example 2
(1) Firstly, putting 0.35 part of polyethylene wax and 20 parts of calcium carbonate into a high-speed mixer, and mixing for 8min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 20 parts of PP, 60 parts of conductive carbon black master batch, 10101.0 parts of antioxidant, 1681.0 parts of antioxidant and 0.5 part of silicone powder; continuously mixing for 8 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
Example 3
(1) Firstly, 0.5 part of white oil and 30 parts of calcium carbonate are put into a high-speed mixer and mixed for 5min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 20 parts of PP, 50 parts of conductive carbon black master batch, 10100.7 parts of antioxidant, 1680.7 parts of antioxidant and 0.4 part of erucamide; continuously mixing for 6 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
Example 4
(1) Firstly, 0.3 part of white oil and 20 parts of calcium carbonate are put into a high-speed mixer and mixed for 6min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 40 parts of PP, 40 parts of conductive carbon black master batch, 10100.8 parts of antioxidant, 1680.8 parts of antioxidant and 0.3 part of erucamide; continuously mixing for 5 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
Example 5
(1) Firstly, putting 0.4 part of polyethylene wax and 20 parts of calcium carbonate into a high-speed mixer, and mixing for 4min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 50 parts of PP, 30 parts of conductive carbon black master batch, 10100.6 parts of antioxidant, 1680.6 parts of antioxidant and 0.4 part of silicone powder; mixing for 4 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
Example 6
(1) Firstly, putting 0.3 part of polyethylene wax and 20 parts of calcium carbonate into a high-speed mixer, and mixing for 7min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 30 parts of PP, 50 parts of conductive carbon black master batch, 10100.6 parts of antioxidant, 1680.7 parts of antioxidant and 0.4 part of silicone powder; continuously mixing for 7 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
Comparative example 1
(1) Firstly, 0.3 part of white oil and 20 parts of calcium carbonate are put into a high-speed mixer and mixed for 7min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 80 parts of PP, 10100.6 parts of antioxidant, 1680.7 parts of antioxidant and 0.4 part of erucamide; continuously mixing for 7 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
Comparative example 2
(1) Firstly, putting 0.35 part of polyethylene wax and 20 parts of calcium carbonate into a high-speed mixer, and mixing for 8min at the temperature of 80-90 ℃;
(2) cooling the high-speed mixer to room temperature, and adding 30 parts of PP, 29 parts of LDPE, 21 parts of conductive carbon black, 10101.0 parts of antioxidant, 1681.0 parts of antioxidant and 0.5 part of silicone powder; continuously mixing for 8 min;
(3) and adding the mixed material into a double-screw extruder with the temperature of 180-220 ℃ in each zone for extrusion granulation to obtain the conductive polypropylene material.
The results of the performance tests are shown in Table 1.
TABLE 1
As can be seen from Table 1, compared with comparative example 1, the surface resistivity of the material can be greatly reduced by adding the conductive carbon black master batch into the polypropylene base material in the invention, and when the addition amount is 20%, the surface resistivity is 106And when the addition amount is increased to 50% and 60%, the surface resistivity can be reduced to 103The requirements of conductive materials can be greatly met; and greatly reduce the materialThe cost of (a). In addition, because the addition amount of the conductive carbon black master batch is high, the flowability of the material is influenced, and therefore, the high-flowability PP resin (40-60 g/10min under the condition of 190 ℃/2.16 kg) is selected as the base material, so that the flowability of the final material is ensured.
Compared with the comparative example 2, the conductive carbon black master batch is used in the example 2, the conductive carbon black is used in the comparative example 2, and although the addition amount is 21 parts, the surface resistivity of the material prepared in the comparative example 2 is two orders of magnitude lower than that of the material prepared in the example 2; the conductive carbon black used in the background technology is 5-20%, the conductive carbon black master batch (20-60%) is used in the invention, the addition amount of the conductive carbon black is 7-21%, the use amount of the conductive carbon black is not increased, but the surface resistivity is reduced by 2 orders of magnitude.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (9)
1. An electrically conductive polypropylene material, characterized by: the composition is prepared from the following components in parts by weight:
20-70 parts of polypropylene;
20-60 parts of conductive carbon black master batch;
10-20 parts of calcium carbonate;
0.5-1.0 part of main antioxidant;
0.5-1.0 part of auxiliary antioxidant;
10.2-0.5 parts of a dispersant;
20.2-0.5 parts of a dispersing agent;
the conductive carbon black master batch is prepared from the following components in parts by weight:
40 parts of high-pressure low-density polyethylene;
25 parts of a lubricant;
and 35 parts of conductive carbon black.
2. The conductive polypropylene material of claim 1, wherein: the melt index of the high-pressure low-density polyethylene in the conductive carbon black master batch is 1.5g/10min under the condition of 190 ℃/2.16kg, the lubricant is silicone powder or erucamide, and the particle size of the conductive carbon black is 40 nm.
3. The conductive polypropylene material of claim 1, wherein: the polypropylene is homopolymerized polypropylene, and the melt index of the polypropylene is 40-60g/10min under the condition of 190 ℃/2.16 kg.
4. The conductive polypropylene material of claim 1, wherein: the mesh number of the calcium carbonate is 2000-5000 meshes.
5. The conductive polypropylene material of claim 1, wherein: the main antioxidant is hindered phenol antioxidant; the auxiliary antioxidant is phosphite antioxidant.
6. The conductive polypropylene material according to claim 5, wherein: the hindered phenol antioxidant is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester or beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester; the phosphite ester antioxidant is tris [2, 4-di-tert-butylphenyl ] phosphite.
7. The conductive polypropylene material of claim 1, wherein: the dispersing agent 1 is white oil or polyethylene wax, and the dispersing agent 2 is erucamide or calcium stearate.
8. A method for preparing an electrically conductive polypropylene material according to any one of claims 1 to 7, wherein: the method comprises the following steps:
(1) firstly, adding 40 parts of high-pressure low-density polyethylene, 25 parts of lubricant and 35 parts of conductive carbon black into an internal mixer for internal mixing, and then introducing the mixture into a single-screw extruder for granulation to obtain conductive carbon black master batches;
(2) firstly, 10.2 to 0.5 part of dispersant and 10 to 30 parts of calcium carbonate are put into a high-speed mixer and mixed for 3 to 8min at the temperature of between 80 and 90 ℃;
(3) cooling the high-speed mixer to room temperature, and adding 20-70 parts of polypropylene, 20-60 parts of conductive carbon black master batch, 0.5-1.0 part of main antioxidant, 0.5-1.0 part of auxiliary antioxidant and 20.2-0.5 part of dispersing agent; continuously mixing for 3-8 min;
(4) and (4) adding the mixed material obtained in the step (3) into a double-screw extruder for extrusion granulation to obtain the conductive polypropylene material.
9. The method of claim 8, wherein: the temperature of the internal mixer in the step (1) is 160-180 ℃, and the temperature of each section of the single-screw extruder is 180-200 ℃; the temperature of each zone of the double-screw extruder in the step (4) is 180-220 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778762A (en) * | 2020-12-31 | 2021-05-11 | 上海聚威新材料股份有限公司 | Conductive PPS composite material and preparation method thereof |
| CN113512251A (en) * | 2021-05-17 | 2021-10-19 | 安徽洁纯生物科技有限公司 | Lining barrel and preparation process thereof |
| CN114644793A (en) * | 2022-03-07 | 2022-06-21 | 江苏金发科技新材料有限公司 | High-toughness electromagnetic shielding polypropylene composite material and preparation method and application thereof |
| CN114716763A (en) * | 2022-03-23 | 2022-07-08 | 华润化学材料科技股份有限公司 | Anti-aging conductive polypropylene functional material and preparation method thereof |
| CN115536936A (en) * | 2021-06-30 | 2022-12-30 | 合肥杰事杰新材料股份有限公司 | Conductive polypropylene and preparation method thereof |
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2019
- 2019-02-27 CN CN201910148373.6A patent/CN111621088A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778762A (en) * | 2020-12-31 | 2021-05-11 | 上海聚威新材料股份有限公司 | Conductive PPS composite material and preparation method thereof |
| CN113512251A (en) * | 2021-05-17 | 2021-10-19 | 安徽洁纯生物科技有限公司 | Lining barrel and preparation process thereof |
| CN115536936A (en) * | 2021-06-30 | 2022-12-30 | 合肥杰事杰新材料股份有限公司 | Conductive polypropylene and preparation method thereof |
| CN114644793A (en) * | 2022-03-07 | 2022-06-21 | 江苏金发科技新材料有限公司 | High-toughness electromagnetic shielding polypropylene composite material and preparation method and application thereof |
| CN114644793B (en) * | 2022-03-07 | 2023-05-05 | 江苏金发科技新材料有限公司 | High-toughness electromagnetic shielding polypropylene composite material and preparation method and application thereof |
| CN114716763A (en) * | 2022-03-23 | 2022-07-08 | 华润化学材料科技股份有限公司 | Anti-aging conductive polypropylene functional material and preparation method thereof |
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Application publication date: 20200904 |