WO2022242289A1 - Mélange maître antistatique, son procédé de préparation et son utilisation - Google Patents

Mélange maître antistatique, son procédé de préparation et son utilisation Download PDF

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Publication number
WO2022242289A1
WO2022242289A1 PCT/CN2022/081587 CN2022081587W WO2022242289A1 WO 2022242289 A1 WO2022242289 A1 WO 2022242289A1 CN 2022081587 W CN2022081587 W CN 2022081587W WO 2022242289 A1 WO2022242289 A1 WO 2022242289A1
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Prior art keywords
antistatic
resin
wax
antistatic masterbatch
parts
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PCT/CN2022/081587
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English (en)
Chinese (zh)
Inventor
王培涛
陈平绪
叶南飚
岑茵
艾军伟
丁超
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金发科技股份有限公司
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Publication of WO2022242289A1 publication Critical patent/WO2022242289A1/fr

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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/20—Carboxylic acid amides
    • 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
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
    • C08L25/02—Homopolymers or copolymers of hydrocarbons
    • C08L25/04—Homopolymers or copolymers of styrene
    • C08L25/08—Copolymers of styrene
    • C08L25/12—Copolymers of styrene with unsaturated nitriles
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
    • C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/12—Polyester-amides
    • 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
    • C08J2355/00—Characterised by the use of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08J2323/00 - C08J2353/00
    • C08J2355/02—Acrylonitrile-Butadiene-Styrene [ABS] polymers
    • 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
    • C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
    • 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
    • C08J2423/08—Copolymers of ethene
    • 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
    • C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2425/02—Homopolymers or copolymers of hydrocarbons
    • C08J2425/04—Homopolymers or copolymers of styrene
    • C08J2425/08—Copolymers of styrene
    • C08J2425/12—Copolymers of styrene with unsaturated nitriles
    • 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
    • C08K2201/017—Additives being an antistatic agent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/04—Antistatic

Definitions

  • the invention relates to the technical field of polymer materials, in particular to an antistatic masterbatch and its preparation method and application.
  • the antistatic technology of polycarbonate is mainly realized by adding antistatic agents.
  • the direct addition of antistatic agents has the defects of uneven dispersion and difficult processing; on the other hand, antistatic agents need to be concentrated on the surface of the workpiece to form a sufficiently uniform and dense conductive network.
  • the traditional antistatic masterbatch can improve the dispersion performance to a certain extent, but it cannot solve the problem of differences in different positions of the same part. If the method of increasing the content of the antistatic agent will cause local uneven dispersion, increase the risk of electrical breakdown, and affect the mechanical properties.
  • the object of the present invention is to provide an antistatic masterbatch, which can achieve uniform antistatic surface resistance and maintain good mechanical properties when applied to ABS/PC alloys.
  • a kind of antistatic masterbatch, by weight, comprises following components:
  • the carboxylic ionomer is an ethylene/methacrylic acid copolymer, wherein 25mol%-90mol% of the carboxyl groups in the methacrylic acid unit are neutralized by metal ions; preferably, 40mol% of the methacrylic acid unit -80 mol% of carboxyl groups are neutralized by metal ions.
  • the amount of carboxyl group neutralized by metal ions can be calculated according to the characteristic absorption peak area of carboxylate after acid-base titration or Fourier transform infrared detector test.
  • the metal ion is at least one selected from sodium ion, zinc ion, magnesium ion and potassium ion, the melt index of the carboxylic acid-based ionomer is between 0.5-6g/10min, and the test condition is 190°C , 2.16kg.
  • the content of AN in the AS resin is 18-36wt%; preferably, the content of AN in the AS resin is 25-28wt%.
  • AS resin is a styrene-acrylonitrile copolymer, and the characteristics of AS resin can be adjusted by adjusting the content of styrene monomer (S) and acrylonitrile monomer (AN).
  • S styrene monomer
  • AN acrylonitrile monomer
  • the invention selects AS resins with different AN contents to improve the uniform dispersion of the antistatic agent in the PC/ABS alloy resin matrix.
  • the antistatic agent is selected from the group consisting of ethoxylated alkylamine, ethoxylated lauryl amide, glyceric acid ester, higher alcohol sulfate ester salt, polyethylene oxide, polyether ester amide, polyether ester imide At least one of; Preferably, the antistatic agent is selected from at least one of polyethylene oxide and polyether ester amide.
  • the wax polymer is selected from one or more of polyethylene wax, oxidized polyethylene wax, maleic anhydride modified polyethylene wax, and low molecular weight copolyamide wax; preferably, the wax polymer At least one selected from oxidized polyethylene wax and maleic anhydride modified polyethylene wax.
  • auxiliary agents are also included; said auxiliary agents are selected from at least one of antioxidants and lubricants.
  • the preparation method of the antistatic masterbatch of the present invention comprises the following steps: according to the proportion, the carboxylic acid-based ionomer, AS resin, antistatic agent and wax polymer are uniformly mixed and then extruded by a twin-screw extruder to produce pellets, the screw temperature is 200-270°C, and the speed range is 180-500r/min.
  • antistatic masterbatch of the present invention is used to prepare antistatic PC/ABS alloy, and comprises the following components in parts by weight:
  • the antistatic masterbatch of the present invention is not particularly limited to PC resin and ABS resin.
  • the present invention provides an antistatic masterbatch.
  • the dispersion in the polymer is good.
  • the addition of AS resin can improve the compatibility of the carboxylic acid-based ionomer and ABS, making it tend to the ABS resin.
  • the third, carboxylic acid-based ionomer has certain compatibility with PC resin and tends to disperse on the surface of PC resin, so that the antistatic masterbatch of the present invention can make the antistatic agent in PC/ABS alloy
  • the PC/ABS alloy has uniform and high-density dispersion on the surface, and at the same time forms a uniform antistatic network inside, which solves the problem of surface resistivity differences caused by dispersion at different positions of the alloy, and can maintain good mechanical properties at the same time.
  • the raw material sources used in the present invention are as follows:
  • PC resin brand PC S-2000F, weight average molecular weight 22000-25000.
  • ABS resin grade is ABS 8391
  • AN content is 26.5wt%, grade SAN NF2200AK;
  • AS resin B AN content is 19.5wt%, grade SAN 310N TR;
  • AS resin C AN content is 35wt%, grade SAN 350N;
  • AS resin D AN content is 17wt%, grade SAN 310TR;
  • Carboxylic acid-based ionomer A the main chain is ethylene/methacrylic acid copolymer, the melt index is 3.5g/10min, the test conditions are 190°C, 2.16kg, and 78mol% of the carboxyl groups of the methacrylic acid unit are neutralized by sodium ions.
  • Carboxylic acid-based ionomer B the main chain is ethylene/methacrylic acid copolymer, the melt index is 1.4g/10min, the test conditions are 190°C, 2.16kg, and 45mol% of the carboxyl groups of the methacrylic acid unit are neutralized by zinc ions.
  • Carboxylic acid-based ionomer C The main chain is ethylene/methacrylic acid copolymer, the melt index is 5.9g/10min, the test conditions are 190°C, 2.16kg, and 26mol% of the carboxyl groups of the methacrylic acid unit are neutralized by zinc ions.
  • Carboxylic acid-based ionomer D the main chain is ethylene/methacrylic acid copolymer, the melt index is 4.0g/10min, the test conditions are 190°C, 2.16kg, and 86mol% of the carboxyl groups of the methacrylic acid unit are neutralized by zinc ions.
  • Antistatic agent A polyethylene oxide, manufacturer Sanyo Chemical industries
  • Antistatic agent B polyether ester amide, manufacturer IonPhasE;
  • Antistatic agent C Ethoxylauramide, manufacturer Adeka;
  • Wax polymer A oxidized polyethylene wax, manufactured by Honeywell;
  • Wax polymer B maleic anhydride modified polyethylene wax, Mitsui Chemicals;
  • Wax polymer C low molecular weight copolyamide wax, SUNMIDE 50, manufacturer Evonik;
  • the preparation method of A series and B series antistatic masterbatch According to the proportion, mix carboxylic acid ionomer, AS resin, antistatic agent and wax polymer evenly, and then extrude and granulate through twin-screw extruder.
  • the screw temperature is 200-270°C, and the speed range is 180-500r/min.
  • PC resin PC resin
  • ABS resin ABS resin
  • antistatic masterbatch or antistatic agent
  • extrude granulation by twin-screw extruder screw speed is 180-450r /min, the temperature range is 200-270°C
  • Table 1 Distribution ratio of each component of A 1-4 antistatic masterbatch (parts by weight)
  • Table 2 Distribution ratio of each component of A 5-9 antistatic masterbatch (parts by weight)
  • Table 3 Distribution ratio of each component of A 10-15 antistatic masterbatch (parts by weight)
  • Table 4 Distribution ratio of each component of B antistatic masterbatch (parts by weight)
  • Table 5 The distribution ratio (parts by weight) and test results of each component of the PC/ABS alloy of the embodiment and the comparative example
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 PC resin 50 50 50 50 50 50
  • Antistatic masterbatch types A1 A2 A3 A4 A5 Antistatic masterbatch, dosage 30 30 30 30 30 antistatic agent - - - - - - Surface Resistance - Front ⁇ 10 ⁇ 9 10 ⁇ 9 10 ⁇ 8 10 ⁇ 9 10 ⁇ 8 Surface resistance - reverse side ⁇ 10 ⁇ 9 10 ⁇ 9 10 ⁇ 10 10 ⁇ 9 Izod notched impact strength kJ/m 2 40 36 33 35 41
  • Example 6 Example 7
  • Example 8 Example 9 PC resin 50 50 50 50 50 ABS resin 50 50 50 50 50 Antistatic masterbatch, types A6 A7 A8 A9 Antistatic masterbatch, dosage 30 30 30 30 antistatic agent - - - - Surface Resistance - Front ⁇ 10 ⁇ 10 10 ⁇ 8 10 ⁇ 10 10 ⁇ 9 Surface resistance - reverse side ⁇ 10 ⁇ 11 10 ⁇ 9 10 ⁇ 10 10 ⁇ 10 Izod notched impact strength kJ/m 2 34 38 43 39
  • the AS resin preferably has an AN content of 25-28 wt%, and the resistance value of the front and back surfaces is more stable.
  • the antistatic agent is preferably polyethylene oxide or polyether ester amide, not only the front and back resistance values are more stable, but also the Izod notched impact strength is better.
  • the waxy polymer is preferably oxidized polyethylene wax, maleic anhydride modified polyethylene wax, although the notched Izod impact strength value of Example 9 using low molecular weight copolyamide wax is higher, but Oxidized polyethylene wax and maleic anhydride modified polyethylene wax have better resistance dispersion uniformity.
  • Comparative Example 1 It can be seen from Comparative Example 1 that the antistatic masterbatch without carboxylic acid-based ionomer has a large difference in resistance value between the front and back sides, and the resistance value is relatively low.

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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)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Divulgué dans la présente invention est un mélange maître antistatique. Le mélange maître antistatique comprend les composants suivants, en parties en poids : De 20 à 50 parties d'un ionomère à base d'acide carboxylique; de 10 à 45 parties d'une résine AS; de 20 à 60 parties d'un agent antistatique; et de 2 à 8 parties d'un polymère de cire. Le mélange maître antistatique selon la présente invention est appliqué à un alliage ABS/PC, de telle sorte qu'une résistance de surface antistatique uniforme peut être obtenue et de bonnes propriétés mécaniques sont maintenues.
PCT/CN2022/081587 2021-05-17 2022-03-18 Mélange maître antistatique, son procédé de préparation et son utilisation WO2022242289A1 (fr)

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CN202110535653.XA CN115368721B (zh) 2021-05-17 2021-05-17 一种抗静电母粒及其制备方法和应用
CN202110535653.X 2021-05-17

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116120843A (zh) * 2023-02-23 2023-05-16 东莞市富颖电子材料有限公司 一种导热贴承载基材及其制备方法

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US3264272A (en) * 1961-08-31 1966-08-02 Du Pont Ionic hydrocarbon polymers
US20080132628A1 (en) * 2006-11-30 2008-06-05 Karlheinz Hausmann Antistatic styrenic polymer compositions and articles therefrom
CN105153670A (zh) * 2015-10-27 2015-12-16 上海锦湖日丽塑料有限公司 一种高耐冲击永久抗静电的pc/abs材料及其制备方法
CN105175924A (zh) * 2015-10-27 2015-12-23 上海锦湖日丽塑料有限公司 一种抗静电母粒和含有该母粒的pc合金及其制备方法
CN112280273A (zh) * 2020-10-16 2021-01-29 金发科技股份有限公司 一种pmma/离聚体/pc三元合金及其制备方法
CN112322015A (zh) * 2020-10-16 2021-02-05 金发科技股份有限公司 一种聚碳酸酯/聚苯乙烯合金及其制备方法和应用
CN112391045A (zh) * 2020-10-16 2021-02-23 金发科技股份有限公司 一种聚碳酸酯组合物及其制备方法及应用

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3264272A (en) * 1961-08-31 1966-08-02 Du Pont Ionic hydrocarbon polymers
US20080132628A1 (en) * 2006-11-30 2008-06-05 Karlheinz Hausmann Antistatic styrenic polymer compositions and articles therefrom
CN105153670A (zh) * 2015-10-27 2015-12-16 上海锦湖日丽塑料有限公司 一种高耐冲击永久抗静电的pc/abs材料及其制备方法
CN105175924A (zh) * 2015-10-27 2015-12-23 上海锦湖日丽塑料有限公司 一种抗静电母粒和含有该母粒的pc合金及其制备方法
CN112280273A (zh) * 2020-10-16 2021-01-29 金发科技股份有限公司 一种pmma/离聚体/pc三元合金及其制备方法
CN112322015A (zh) * 2020-10-16 2021-02-05 金发科技股份有限公司 一种聚碳酸酯/聚苯乙烯合金及其制备方法和应用
CN112391045A (zh) * 2020-10-16 2021-02-23 金发科技股份有限公司 一种聚碳酸酯组合物及其制备方法及应用

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116120843A (zh) * 2023-02-23 2023-05-16 东莞市富颖电子材料有限公司 一种导热贴承载基材及其制备方法
CN116120843B (zh) * 2023-02-23 2023-08-18 东莞市富颖电子材料有限公司 一种导热贴承载基材及其制备方法

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