CN107474371B - Polyolefin antistatic composition and preparation method thereof - Google Patents
Polyolefin antistatic composition and preparation method thereof Download PDFInfo
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- 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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
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- 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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- 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
- C08J2323/04—Homopolymers or copolymers of ethene
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- 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
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- 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
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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- C08L2201/04—Antistatic
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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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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
Abstract
The invention relates to a polyolefin antistatic composition and a preparation method thereof, belonging to the technical field of polyolefin compositions. The polyolefin antistatic composition is prepared from the following raw materials in parts by weight: 25-70 parts of high-density polyethylene, 5-15 parts of linear low-density polyethylene, 20-50 parts of antistatic master batch and 5-10 parts of conductive master batch; the preparation method is to blend and granulate the high-density polyethylene, the linear low-density polyethylene, the antistatic agent master batch and the conductive master batch. The invention solves the problems of poor antistatic effect and poor mechanical property of the material after the traditional polyolefin is subjected to antistatic modification, ensures that the material has good antistatic property, endows the material with better impact property and forming property, and has higher modulus, good steel toughness balance property and better antistatic property; the preparation method is simple and easy to operate.
Description
Technical Field
The invention relates to a polyolefin antistatic composition and a preparation method thereof, belonging to the technical field of polyolefin compositions.
Background
Polyethylene has excellent mechanical property, chemical stability, electrical insulation, processability, high cost performance and wide application range, but is not easy to eliminate once being electrified due to friction due to the excellent insulation of polyethylene, so that static electricity is generated, dust absorption and electric shock are caused, and even sparks are generated to explode. In order to avoid such accidents, the use of plastic articles in certain applications must be antistatic.
The traditional polyethylene antistatic modification is usually added with an antistatic agent or more conductive fillers. The common antistatic agent can migrate, so that the phenomenon of reduction or disappearance of the antistatic effect is caused along with the time extension, the high-molecular permanent antistatic agent is expensive, the addition amount is large, the cost is high, the effect is not prominent, and the use range is narrow; the effect of adding fillers such as conductive carbon black is better, but the defects are poor dispersion effect and poor processability.
CN20130655948 discloses a processing method of an ultra-high molecular weight polyethylene pipe, wherein 2-4% of carbon black, 1-1.5% of an antistatic agent, 1-2% of graphite, 1-2% of ethylene glycol coconut and 1-2% of a smoothing agent are added into the ultra-high molecular weight polyethylene, which mainly aims at improving the processing performance of the ultra-high molecular weight polyethylene, and the antistatic effect of the material is limited.
CN103739917A discloses an antistatic polyethylene plastic master batch, a conductive material for the master batch and an application method, and the components are as follows: 3-8% of conductive carbon black, 2-15% of conductive graphite, 1-5% of conductive fiber, 5-20% of high-density polyethylene, 0-15% of linear low-density polyethylene, 0.1-1% of titanate coupling agent, 0.1-1% of aluminate coupling agent and 0.2-4% of dispersing agent, wherein the antistatic effect of the material is 106 omega.
CN 200610040792 discloses an antistatic flame-retardant polyethylene composition and a preparation method thereof, wherein the content of conductive carbon black is as high as 10-19%, and the higher the content of conductive carbon black is, the greater the influence on the mechanical properties and processability of the material will be, and the mechanical properties are generally deteriorated.
In the research on antistatic PP, three antistatic agent masterbatches are prepared by taking PP as a base resin, but the surface resistivity of the antistatic agent masterbatches is the lowest, the surface resistivity is only reduced by 4 orders of magnitude to 1 x 1012 omega, and the antistatic effect is limited.
Therefore, it is necessary to further study the antistatic properties of polyolefins.
Disclosure of Invention
The invention aims to provide a polyolefin antistatic composition, which solves the problems of poor antistatic effect and poor mechanical properties of materials of traditional polyolefin after antistatic modification, and has the characteristics of good antistatic property, good impact and forming properties and high modulus; the invention also provides a preparation method thereof.
The polyolefin antistatic composition is prepared from the following raw materials in parts by weight:
wherein:
the mass flow rate of the 21.6kg melt of the high-density polyethylene (HDPE) is 8-12 g/10min, and the density is 0.947-0.952 g/cm3The polyethylene with the weight-average molecular weight of 250000-400000 comprises 1-hexene and ethylene as comonomers, and the molar ratio of the 1-hexene to the ethylene is 0.01-0.02.
The Linear Low Density Polyethylene (LLDPE) is selected from 2.16kg of melt with the mass flow rate of 1-2 g/10min and the density of 0.939-0.941 g/cm3And a polyethylene having a weight average molecular weight of 100000 to 250000, wherein when the comonomer is propylene and ethylene, the molar ratio of propylene to ethylene is 0.01 to 0.03. When the comonomers are butylene and ethylene, the molar ratio of the butylene to the ethylene is 0.002-0.004.
The antistatic master batch is prepared from the following raw materials in parts by mass:
wherein:
the melt mass flow rate of the polypropylene is 12-28 g/10min, and the density is 0.9g/cm3；
The antioxidant is phenol antioxidant with model number of 1010;
the nucleating agent is a dimethylene sorbitol derivative;
the dispersant A is polyethylene wax;
the lubricant is erucamide;
the coupling agent is a silane coupling agent with the model of KH 550;
the conductive carbon black has a specific volume of 3.5 to 5.0cm3The iodine absorption value is 500-700 g/kg, the ash content is less than 2.0 percent, the average particle diameter is 26-29 nm, and the specific surface area is 96m2(iv)/g, pH value is 6.2-7.2;
the graphitization degree of the conductive graphite is 99%, the average particle size is 36nm, and the true density is 2.16-2.26 g/cm3Oil absorption of 40-60 g/100g, ash content of 0.1-0.6% and water content of 0.06%;
the density of the ethylene propylene rubber is 0.86g/cm3The ethylene content is 58-62 wt%, the glass transition temperature is-56 ℃ to-62 ℃, the Mooney viscosity ML (1+4) is 62-81 at 100 ℃, the molecular weight is 260000-610000, and the molecular weight distribution index is 2.6-3.5.
The preparation method of the antistatic master batch comprises the following steps:
(1) adding polypropylene, a nucleating agent and an antioxidant into an extruder, and performing extrusion granulation at 210 ℃ to obtain a composition A, wherein only half of the amount of the polypropylene is added;
(2) adding conductive carbon black, conductive graphite, a dispersing agent and a coupling agent into a stirrer, mixing for 3-10min, then adding the other half of polypropylene, continuously mixing for 3-5 min, adding the uniformly mixed materials into an internal mixer, and internally mixing for 10min to obtain a composition B;
(3) and uniformly mixing the composition A, the composition B and the ethylene propylene rubber, and then banburying to obtain the polyolefin antistatic composition.
The conductive master batch is prepared from high-density polyethylene, conductive carbon black, a dispersant B and a coupling agent; wherein the mass ratio of the high-density polyethylene to the conductive carbon black to the dispersing agent to the coupling agent is 70:20:5: 5; the dispersant B is polyethylene wax or liquid paraffin; the coupling agent is a silane coupling agent.
The preparation method of the conductive master batch comprises the following steps:
firstly, mixing the conductive carbon black, the dispersant B and the coupling agent in a stirrer for 3-10min, then adding the high-density polyethylene for mixing for 3-5 min, then adding the uniformly mixed materials into an internal mixer for internal mixing at the temperature of 180-200 ℃ for 10-30 min, and finally carrying out extrusion granulation at the temperature of 180-200 ℃ by using a single-screw extruder to obtain the conductive master batch.
The preparation method of the polyolefin antistatic composition is to blend and granulate high-density polyethylene, linear low-density polyethylene, antistatic agent master batch and conductive master batch.
The invention has the following beneficial effects:
the polyolefin antistatic composition ensures that the material has good antistatic performance, endows the material with better impact performance and formability, and has higher modulus, good steel toughness balance performance and good antistatic performance; the preparation method is simple and easy to operate.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The composition of the raw material parts by mass of the polyolefin antistatic composition is shown in table 1.
The preparation method of the polyolefin antistatic composition is to blend and granulate high-density polyethylene, linear low-density polyethylene, antistatic agent master batch and conductive master batch.
The antistatic polyolefin compositions obtained in this example were compression-moulded with the operating parameters indicated in Table 4 and then tested for the following properties:
melt Mass Flow Rate (MFR): the test is carried out according to GB/T3682, and the test conditions are as follows: the temperature is 190 ℃, and the load is 21.6 kg;
impact strength of the simply supported beam notch: testing according to GB/T1043, wherein the test temperature is 23 ℃, and a sample strip of 4mm is used;
tensile yield stress: testing according to GB/T1040, stretching speed 50mm/min, 4mm sample strip;
surface resistivity: testing according to GB/T1414 rules, 1mm sample;
flexural modulus: the test was carried out according to the GB/T9341-2000 specification, 4mm coupons.
The results are shown in Table 5.
Example 2
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 3
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 4
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 5
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 6
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 7
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 8
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 9
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
Example 10
The composition of the raw materials in parts by mass of the polyolefin antistatic composition is shown in table 1; the preparation of the antistatic polyolefin composition was carried out as in example 1.
The polyolefin antistatic compositions obtained in this example were compression molded with the operating parameters shown in Table 4 and then tested for the properties shown in example 1 with the test results shown in Table 5.
The raw material composition of the polyolefin antistatic compositions of examples 1 to 10 was:
the high density polyethylene has 21.6kg melt mass flow rate of 12g/10min and density of 0.948g/cm3Polyethylene with a weight average molecular weight of 260000 and the comonomers 1-hexene and ethylene in a molar ratio 1-hexene to ethylene of 0.015.
The linear low density polyethylene has 2.16kg melt mass flow rate of 6g/10min and density of 0.941g/cm3The weight average molecular weight is 160000, the comonomers are butylene and ethylene, and the molar ratio of butylene to ethylene is 0.004.
The composition of the raw materials in parts by mass of the antistatic masterbatch is shown in table 2. Wherein the melt mass flow rate of the polypropylene is 12-28 g/10min, and the density is 0.9g/cm3(ii) a The antioxidant is phenol antioxidant with model number of 1010; the nucleating agent is DBS which is a commercially available dimethylene sorbitol derivative; the dispersant A is polyethylene wax; the lubricant is erucamide; the coupling agent is a commercial silane coupling agent KH 550. The conductive carbon black is a commercially available product and has a specific volume of 5.0cm3Iodine absorption value of 666g/kg, ash content of 1.0%, average particle diameter of 28nm, specific surface area of 96m2(iv)/g, pH 6.8; the graphitization degree of the conductive graphite is 99 percent, the average grain diameter is 19nm, and the true density is 2.19g/cm3Oil absorption of 58g/100g, ash content of 0.1%, and water content of 0.06 wt%; the density of the ethylene propylene rubber is 0.86g/cm3The ethylene content was 62% by weight, the glass transition temperature was-56 ℃, the Mooney viscosity ML (1+4) at 100 ℃ was 66, the molecular weight was 290000, and the molecular weight distribution index was 2.6.
The preparation method of the antistatic master batch comprises the following steps:
(1) adding polypropylene, a nucleating agent and an antioxidant into an extruder, and performing extrusion granulation at 210 ℃ to obtain a composition A, wherein only half of the amount of the polypropylene is added;
(2) adding conductive carbon black, conductive graphite, a dispersing agent and a coupling agent into a stirrer to be mixed for 8min, then adding the other half of polypropylene to be continuously mixed for 4min, and adding the uniformly mixed materials into an internal mixer to be internally mixed for 10min to obtain a composition B;
(3) and uniformly mixing the composition A, the composition B and the ethylene propylene rubber, and then banburying to obtain the polyolefin antistatic composition.
The results of the performance tests of the antistatic masterbatch are shown in table 3.
The conductive master batch is prepared from high-density polyethylene, conductive carbon black, a dispersant B and a coupling agent; wherein the mass ratio of the high-density polyethylene to the conductive carbon black to the dispersing agent to the coupling agent is 70:20:5: 5; the dispersant B is commercial polyethylene wax; the coupling agent is a commercial silane coupling agent KH 550.
The preparation method of the conductive master batch comprises the following steps:
firstly, mixing conductive carbon black, a dispersant B and a coupling agent in a stirrer for 8min, then adding high-density polyethylene for mixing for 4min, then adding the uniformly mixed materials into an internal mixer for internal mixing for 20min, and finally carrying out extrusion granulation by using a single-screw extruder at 190 ℃ to obtain the conductive master batch.
TABLE 1 raw material compositions for examples 1-10
Table 2 raw material composition of antistatic masterbatch in examples 1 to 10
TABLE 3 results of testing the properties of the antistatic masterbatches of examples 1 to 10
TABLE 4 compression Molding operating parameters
TABLE 5 EXAMPLES 1-10 Performance test indexes
Comparative example
The composition of the raw materials in comparative examples 1-10 in parts by mass is shown in Table 6, the raw materials in Table 6 are directly mixed according to the mixture ratio, then banburying is carried out, the banburying process is the same as that in examples 1-10, the performance is measured by tabletting after discharging, the performance detection indexes are the same as those in example 1, and the detection results are shown in Table 7.
TABLE 6 raw material compositions in comparative examples 1 to 10
TABLE 7 Performance test indexes of comparative examples 1 to 10
As can be seen from the test results of examples 1-10 and comparative examples 1-10, the invention ensures that the polyolefin antistatic composition has good antistatic property, and simultaneously endows the material with better impact property and formability, and has higher modulus and good steel toughness balance property.
Claims (6)
1. A polyolefin antistatic composition characterized by: the feed is prepared from the following raw materials in parts by mass:
the high-density polyethylene is selected from 21.6kg of melt with the mass flow rate of 8-12 g/10min and the density of 0.947-0.952 g/cm3Polyethylene with the weight-average molecular weight of 250000-400000, wherein the comonomer is 1-hexene and ethylene, and the molar ratio of the 1-hexene to the ethylene is 0.01-0.02;
the linear low density polyethylene is selected from 2.16kg of melt with the mass flow rate of 1-6 g/10min and the density of 0.939-0.941 g/cm3Weight average molecular weightThe molar ratio of propylene to ethylene is 0.01-0.03 when the comonomer of 100000-250000 polyethylene is propylene and ethylene, and the molar ratio of butylene to ethylene is 0.002-0.004 when the comonomer is butylene and ethylene;
the antistatic master batch is prepared from the following raw materials in parts by mass:
the melt mass flow rate of the polypropylene is 12-28 g/10min, and the density is 0.9g/cm3(ii) a The antioxidant is phenol antioxidant with model number of 1010; the nucleating agent is a dimethylene sorbitol derivative; the dispersant A is polyethylene wax; the lubricant is erucamide; the coupling agent is a silane coupling agent with the model of KH 550.
2. The polyolefin antistatic composition of claim 1, characterized in that: the conductive carbon black has a specific volume of 3.5 to 5.0cm3The iodine absorption value is 500-700 g/kg, the ash content is less than 2.0 percent, the average particle diameter is 26-29 nm, and the specific surface area is 96m2(iv)/g, pH value is 6.2-7.2; the graphitization degree of the conductive graphite is 99 percent, the average particle size is 18-36nm, and the true density is 2.16-2.26 g/cm3Oil absorption of 40-60 g/100g, ash content of 0.1-0.6% and water content of 0.06%; the density of the ethylene propylene rubber is 0.86g/cm3The ethylene content is 58-62 wt%, the glass transition temperature is-56 ℃ to-62 ℃, the Mooney viscosity ML (1+4) is 62-81 at 100 ℃, the molecular weight is 260000-610000, and the molecular weight distribution index is 2.6-3.5.
3. The polyolefin antistatic composition of claim 1, characterized in that: the preparation method of the antistatic master batch comprises the following steps:
(1) adding polypropylene, a nucleating agent and an antioxidant into an extruder, and performing extrusion granulation at 210 ℃ to obtain a composition A, wherein only half of the amount of the polypropylene is added;
(2) adding conductive carbon black, conductive graphite, a dispersing agent and a coupling agent into a stirrer to be mixed for 3-10min, then adding the other half of polypropylene to be continuously mixed for 3-5 min, and adding the mixture after uniform mixing into an internal mixer to be internally mixed for 10min to obtain a composition B;
(3) and uniformly mixing the composition A, the composition B and the ethylene propylene rubber, and then banburying to obtain the polyolefin antistatic composition.
4. The polyolefin antistatic composition of claim 1, characterized in that: the conductive master batch is prepared from high-density polyethylene, conductive carbon black, a dispersant B and a coupling agent; wherein the mass ratio of the high-density polyethylene to the conductive carbon black to the dispersant B to the coupling agent is 70:20:5: 5; the dispersant B is polyethylene wax or liquid paraffin; the coupling agent is a silane coupling agent with the model of KH-550.
5. Antistatic polyolefin composition according to claim 4, characterized in that: the preparation method of the conductive master batch comprises the following steps:
firstly, mixing the conductive carbon black, the dispersant B and the coupling agent in a stirrer for 3-10min, then adding the high-density polyethylene for mixing for 3-5 min, then adding the uniformly mixed materials into an internal mixer for internal mixing at the temperature of 180-200 ℃ for 10-30 min, and finally extruding and granulating at the temperature of 180-200 ℃ by using a single-screw extruder to obtain the conductive master batch.
6. A process for the preparation of antistatic compositions of polyolefins according to any of claims 1 to 5, characterized in that: the antistatic agent is prepared by blending and granulating high-density polyethylene, linear low-density polyethylene, antistatic agent master batch and conductive master batch.
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| TWI815868B (en) * | 2018-03-28 | 2023-09-21 | 美商陶氏全球科技有限責任公司 | Composite of polar organic copolymer and ultra-low-wettability carbon black |
| CN110746755A (en) * | 2019-09-28 | 2020-02-04 | 江苏兆鋆新材料股份有限公司 | Antistatic bulk molding compound, preparation method and application thereof |
| CN110922664A (en) * | 2019-12-11 | 2020-03-27 | 湖北凯科塑业有限公司 | Antistatic PE pipe and manufacturing method thereof |
| CN113512251B (en) * | 2021-05-17 | 2023-04-25 | 安徽洁纯生物科技有限公司 | Lining barrel and preparation process thereof |
| CN115386166B (en) * | 2022-09-19 | 2023-08-29 | 成都金发科技新材料有限公司 | Polypropylene composite material, and preparation method and application thereof |
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