WO2022077862A1 - 一种pmma/离聚体/pc三元合金及其制备方法 - Google Patents

一种pmma/离聚体/pc三元合金及其制备方法 Download PDF

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WO2022077862A1
WO2022077862A1 PCT/CN2021/082013 CN2021082013W WO2022077862A1 WO 2022077862 A1 WO2022077862 A1 WO 2022077862A1 CN 2021082013 W CN2021082013 W CN 2021082013W WO 2022077862 A1 WO2022077862 A1 WO 2022077862A1
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pmma
ionomer
ternary alloy
alloy according
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王培涛
艾军伟
黄险波
叶南飚
岑茵
丁超
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Kingfa Science and Technology Co Ltd
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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
    • 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
    • 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
    • C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing atoms other than carbon or hydrogen
    • C08L23/0869—Copolymers of ethene with unsaturated hydrocarbons containing atoms other than carbon or hydrogen with unsaturated acids, e.g. [meth]acrylic acid; with unsaturated esters, e.g. [meth]acrylic acid esters
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • the invention relates to the technical field of polymer materials, in particular to a PMMA/ionomer/PC ternary alloy and a preparation method thereof.
  • Polycarbonate (referred to as PC) is a high molecular polymer containing carbonate groups in the molecular chain. According to the structure of the ester groups, it can be divided into aliphatic, aromatic, aliphatic-aromatic and other types. Due to the special structure of polycarbonate, it has become the fastest growing general engineering plastic among the five major engineering plastics. Polycarbonate is a synthetic material developed in the late fifties. Polycarbonate resin has outstanding impact resistance, creep resistance and dimensional stability, and is widely used in electronic appliances, rail transit and aerospace fields.
  • polycarbonate also has defects such as surface gloss, surface scratch resistance, and insufficient strength.
  • the general solution is to blend with PMMA (polymethyl methacrylate) to form a PMMA/PC alloy.
  • PMMA polymethyl methacrylate
  • the light is refracted in the resin matrix and a pearlescent effect occurs.
  • Chinese patent application 2018108054686 discloses a PC/PMMA composite material, in which the difference in gloss between the two is used to produce a pearlescent effect, avoiding the easy formation of the surface of the workpiece caused by the addition of aluminum powder or pearlescent powder to conventional silver pearlescent spray-free materials. Flow marks or weld line problems.
  • Chinese patent application 2016104106339 discloses a transparent scratch-resistant PC/PMMA alloy, by using metal organic compound stabilizer A, phosphorus-containing compound stabilizer B, and adding stabilizer B into the molten system by side feeding , which can solve the problems of pearl luster and yellowing in the preparation of transparent scratch-resistant PC resin compositions in the prior art.
  • Chinese patent application No. 2018106764638 discloses a transparent high-hardness PC composition. By blending polyester copolymer, styrene copolymer and PC, it solves the problems of poor compatibility, poor toughness, and opacity between PC and PMMA alloy in the prior art. Pearlescent phenomenon.
  • the main chain of the polycarbonate molecule is relatively rigid, and the adjustment of the molecular chain during the injection molding process is relatively slow, resulting in a high molding stress.
  • the purpose of the present invention is to overcome the above-mentioned technical defects and provide a PMMA/ionomer/PC ternary alloy, which can greatly improve the pearlescent effect, and has the advantages of low forming stress, which is conducive to the preparation of high-toughness products with complex structures.
  • Another object of the present invention is to provide a method for preparing the above-mentioned ternary alloy.
  • the carboxylic acid group ionomer is an ethylene/methacrylic acid copolymer, wherein 40mol%-90mol% of the carboxyl groups of the methacrylic acid units are neutralized by metal ions.
  • the metal ion is selected from at least one of sodium ion, zinc ion, magnesium ion and potassium ion.
  • the melt index of the carboxylic acid-based ionomer is between 0.5-5g/10min, and the test conditions are 190°C and 2.16kg.
  • the PMMA melt index is between 12-22g/10min, and the test conditions are 230°C and 3.8kg.
  • the polycarbonate melt index is between 3-22g/10min, and the test conditions are 300°C and 1.2kg.
  • Polycarbonates are branched thermoplastic polymers or copolymers obtained from the reaction of dihydroxy compounds or a small amount of polyhydroxy compounds with phosgene or carbonic acid diesters.
  • Polycarbonate resins can be produced by a phosgene method (interfacial polymerization method) or a melt method (transesterification method).
  • the polycarbonate resin is also provided by subjecting the polycarbonate resin produced by the melt method to a post-treatment to adjust the amount of terminal hydroxyl groups.
  • the repeating unit is formed by the reaction of bisphenol A and phosgene.
  • the repeating unit is formed by the reaction of diphenyl carbonate and bisphenol A.
  • 0-3 parts by weight of lubricant can also be added.
  • Described lubricant is selected from at least one in stearate class lubricant, fatty acid class lubricant, stearate class lubricant; Described stearate class lubricant is selected from calcium stearate, At least one in magnesium stearate, zinc stearate; Described fatty acid lubricant is selected from at least one in fatty acid, fatty acid derivative, fatty acid ester; Described stearic ester lubricant is selected from At least one of glycerol monostearate and pentaerythritol stearate.
  • the preparation method of the above-mentioned PMMA/ionomer/PC ternary alloy comprises the following steps: according to the proportion, after mixing the components uniformly, extruding and granulating through a twin-screw extruder, the screw temperature range is 200-270 °C, the rotating speed range is 180-500r/min, and the PMMA/ionomer/PC ternary alloy is obtained.
  • the PMMA/ionomer/PC ternary alloy of the present invention obviously improves the pearlescent defect of the PMMA/PC binary alloy.
  • a carboxylic acid-based ionomer with a flexible molecular chain it can be alloyed with PC/PMMA to reduce the stress generated during the molding process, and can also improve the surface hardness of the ternary alloy.
  • the sources of raw materials used in the present invention are as follows:
  • Carboxylic ionomer A the main chain is an 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 units are neutralized by sodium ions.
  • Carboxylic acid group 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 units are neutralized by zinc ions.
  • Carboxylic ionomer C the main chain is an ethylene/methacrylic acid copolymer, the melt index is 5.9 g/10min, the test conditions are 190° C., 2.16 kg, and 26 mol% of the carboxyl groups of the methacrylic acid units are neutralized by zinc ions.
  • Polycarbonate brand TRIREX 3025PJ, melt index is 10g/10min, test condition is 300°C, 1.2kg;
  • Zinc stearate ZINC STEARATE (BS-2818), commercially available, added as a lubricant;
  • Examples and comparative examples PMMA ionomer PC ternary alloy preparation method according to the proportion, after mixing the components uniformly, extruding and granulating through a twin-screw extruder, the screw temperature range is 200-270 ° C, and the rotating speed is 200-270 ° C. The range is 360-400 r/min, and the alloy is obtained.
  • Comparative Examples 2-4 It can be seen from Comparative Examples 2-4 that, without adding carboxylic acid-based ionomer or the addition amount is insufficient, the pearlescence is obvious, and the hardness is low and stress cracking is easy.

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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)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

本发明公开了一种PMMA/离聚体/PC三元合金，按重量份计，包括以下组分：羧酸基离聚体5-60份；聚碳酸酯5-95份；PMMA1-35份。通过三种树脂的复配，不仅能够明显改善PMMA/PC合金的珠光缺陷，而且三元合金具有低成型应力的优点，有利于制备结构复杂的高韧性产品。

Description

一种PMMA/离聚体/PC三元合金及其制备方法 技术领域
本发明涉及高分子材料技术领域，特别是涉及一种PMMA/离聚体/PC三元合金及其制备方法。
背景技术
聚碳酸酯(简称PC)是分子链中含有碳酸酯基的高分子聚合物，根据酯基的结构可分为脂肪族、芳香族、脂肪族-芳香族等多种类型。由于聚碳酸酯结构上的特殊性，现已成为五大工程塑料中增长速度最快的通用工程塑料。聚碳酸酯是五十年代末开始发展起来的合成材料。聚碳酸酯树脂具有突出的抗冲击能力、耐蠕变、尺寸稳定性，被广泛应用于电子电器、轨道交通及航空航天领域，近年来用量超过尼龙，跃居首位。
但是，聚碳酸酯也具有表面光泽、表面耐划性、强度不足等缺陷，一般解决方法是与PMMA(聚甲基丙烯酸甲酯)共混形成PMMA/PC合金。但是，由于PMMA/PC两种树脂基体的折光率不同，导致光线在树脂基体中折射从而发生了珠光效果。中国专利申请2018108054686公开了一种PC/PMMA复合材料，其中就利用了两者光泽度的不同而发生珠光效果，避免常规银色珠光免喷涂材料因铝粉或珠光粉的加入导致制件表面易形成流痕或熔接痕问题。中国专利申请2016104106339公开了一种透明耐刮擦的PC/PMMA合金，通过采用金属有机化合物稳定剂A、含磷化合物的稳定剂B，并且通过侧喂的方式将稳定剂B加入到熔融体系中，能够解决现有技术中制备透明耐刮擦PC树脂组合物时存在的珠光、发黄等问题。中国专利申请2018106764638公开了一种透明高硬度PC组合物，通过采用聚酯共聚物、苯乙烯共聚物与PC共混，解决了现有技术中PC与PMMA合金相容性差、韧性差、不透明有珠光现象的问题。
关于成型应力，聚碳酸酯分子主链刚性较强，在注塑成型的过程中分子链调整相对会慢，导致其成型应力较高。一般的，降低应力的方式主要有以下3种：1.降低聚碳酸酯粘度，但是会导致力学性能的大幅下降；2.通过在成型的过程中调节成型参数来降低应力；3.引入ABS树脂制成PC/ABS合金，但是该合金表面硬度低，耐划擦性能差。
发明内容
本发明的目的在于，克服上述技术缺陷，提供一种PMMA/离聚体/PC三元合金，能够极大改善珠光效果，并且具有低成型应力的优点，有利于制备结构复杂的高韧性产品。
本发明的另一目的在于，提供上述三元合金的制备方法。
本发明是通过以下技术方案实现的：
一种PMMA/离聚体/PC三元合金，按重量份计，包括以下组分：
羧酸基离聚体         5-60份；
聚碳酸酯             5-95份；
PMMA                 1-35份。
优选的，按重量份计，包括以下组分：
羧酸基离聚体         15-35份；
聚碳酸酯             25-75份；
PMMA                 10-25份。
所述的羧酸基离聚体为乙烯/甲基丙烯酸类共聚物，其中甲基丙烯酸单元的40mol％-90mol％的羧基被金属离子中和。
所述的金属离子选自钠离子、锌离子、镁离子、钾离子中的至少一种。
所述的羧酸基离聚体的熔融指数在0.5-5g/10min之间，测试条件为190℃、2.16kg。
所述的PMMA熔融指数在12-22g/10min之间，测试条件为230℃、3.8kg。
所述的聚碳酸酯熔融指数在3-22g/10min之间，测试条件为300℃、1.2kg。
聚碳酸酯，为由二羟基化合物或其和少量的多羟基化合物与光气(phosgene)或碳酸二酯的反应获得的支化热塑性聚合物或共聚物。可使用由光气法(界面聚合法)或熔融法(酯交换法)生产聚碳酸酯树脂。聚碳酸酯树脂还通过由熔融法生产的聚碳酸酯树脂经过调节末端羟基的量的后处理来提供。
通过光气法反应得到的聚碳酸酯链段中，重复单元由双酚A和光气反应组成。酯交换法得到的聚碳酸酯链段中，重复单元是由碳酸二苯酯和双酚A反应组成。
为了提升熔融加工性能，按重量份计，还可以加入0-3份的润滑剂。
所述的润滑剂选自硬脂酸盐类润滑剂、脂肪酸类润滑剂、硬脂酸酯类润滑剂中的至少一种；所述的硬脂酸盐类润滑剂选自硬脂酸钙、硬脂酸镁、硬脂酸锌中的至少一种；所述的脂肪酸类润滑剂选自脂肪酸、脂肪酸衍生物、脂肪酸酯中的至少一种；所述的硬脂酸酯类润滑剂选自单硬脂酸甘油酯、季戊四醇硬脂酸酯中的至少一种。
上述的PMMA/离聚体/PC三元合金的制备方法，包括以下步骤：按照配比，将各组分混合均匀后，通过双螺杆挤出机挤出造粒，螺杆温度范围是200-270℃，转速范围是180-500r/min，得到PMMA/离聚体/PC三元合金。
上述的PMMA/离聚体/PC三元合金的应用，用于制备耐刮擦、高光泽制件。
本发明具有如下有益效果：
本发明的PMMA/离聚体/PC三元合金，明显改善了PMMA/PC二元合金的珠光缺陷。通过引入了分子链柔顺的羧酸基离聚体，与PC/PMMA做成合金后能降低成型过程中产生的应力，并且还能提升三元合金的表面硬度。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。
本发明所用原料来源如下：
羧酸基离聚体A：主链为乙烯/甲基丙烯酸共聚物，熔融指数3.5g/10min，测试条件为190℃、2.16kg，甲基丙烯酸单元的78mol％的羧基被钠离子中和。
羧酸基离聚体B：主链为乙烯/甲基丙烯酸共聚物，熔融指数1.4g/10min，测试条件为190℃、2.16kg，甲基丙烯酸单元的45mol％的羧基被锌离子中和。
羧酸基离聚体C：主链为乙烯/甲基丙烯酸共聚物，熔融指数5.9g/10min，测试条件为190℃、2.16kg，甲基丙烯酸单元的26mol％的羧基被锌离子中和。
聚碳酸酯：牌号TRIREX 3025PJ，熔融指数为10g/10min，测试条件为300℃，1.2kg；
PMMA：牌号PMMA LG，熔融指数为9g/10min，测试条件为230℃、3.8kg；
硬脂酸锌：ZINC STEARATE(BS-2818)，市售，作为润滑剂添加；
各项性能测试方法：
(1)内应力测试：将ISO527.2-2012拉伸样条固定在曲率为1.0的夹具上，涂抹甲苯：乙醇＝1:3的溶剂，观察样条开裂时间以及开裂形态。涂抹溶剂后1h内断裂记做1级，在1-4h内开裂的记做2级，在4-12h内开裂记做3级，在12-24h内记做4级，超过24h的均记做5级。开裂形态方面，分为微裂纹和大裂纹两种形态。
(2)表面硬度测试：使用铅笔硬度方法评估，参考ASTM D3363-2005标准进行测试，测试砝码重量为750g。评价等级分为：6B、5B、4B、3B、2B、B、HB、F、H、2H、3H、4H、5H、6H。
(3)珠光效果：观察是否有珠光效果(在侧光源下观察是否可以看到彩色色纹，计算单位面积内珠光效果的产生面积)。
实施例和对比例PMMA离聚体PC三元合金的制备方法：按照配比，将各组分混合均 匀后，通过双螺杆挤出机挤出造粒，螺杆温度范围是200-270℃，转速范围是360-400r/min，得到合金。
表1：实施例1-6合金各组分配比及各项性能测试结果
Figure PCTCN2021082013-appb-000001
由实施例1/3/5可知，虽然理论上PMMA含量越高表面硬度越高，但是如三元合金的树脂配比不在本发明优选的范围内，PMMA提高表面硬度的优势就很难体现出来。
由实施例1-6可知，优选的三元合金配比范围，三项性能中至少有两种性能较好。
表2：实施例7-9合金各组分配比及各项性能测试结果
Figure PCTCN2021082013-appb-000002
表3：对比例合金各组分配比及各项性能测试结果
Figure PCTCN2021082013-appb-000003
由于对比例1中无PMMA，因此无珠光效果；但是，表面硬度低，易应力开裂。
由对比例2-4可知，不加入羧酸基离聚体或加入量不足，珠光明显，并且表明硬度低，易应力开裂。
由对比例5可知，羧酸基离聚体加入量过大，材料珠光不能消除，并且降低材料模量。

Claims (10)

  1. 一种PMMA/离聚体/PC三元合金，其特征在于，按重量份计，包括以下组分：
    羧酸基离聚体         5-60份；
    聚碳酸酯             5-95份；
    PMMA                1-35份。
  2. 根据权利要求1所述的PMMA/离聚体/PC三元合金，其特征在于，按重量份计，包括以下组分：
    羧酸基离聚体         15-35份；
    聚碳酸酯             25-75份；
    PMMA                10-25份。
  3. 根据权利要求1所述的PMMA/离聚体/PC三元合金，其特征在于，所述的羧酸基离聚体为乙烯/甲基丙烯酸类共聚物，其中甲基丙烯酸单元中的40mol％-90mol％的羧基被金属离子中和。
  4. 根据权利要求3所述的PMMA/离聚体/PC三元合金，其特征在于，所述的金属离子选自钠离子、锌离子、镁离子、钾离子中的至少一种。
  5. 根据权利要求1-4任一项所述的PMMA/离聚体/PC三元合金，其特征在于，所述的羧酸基离聚体的熔融指数在0.5-5g/10min之间，测试条件为190℃、2.16kg。
  6. 根据权利要求1所述的PMMA/离聚体/PC三元合金，其特征在于，所述的PMMA熔融指数在12-22g/10min之间，测试条件为230℃、3.8kg。
  7. 根据权利要求1所述的PMMA/离聚体/PC三元合金，其特征在于，所述的聚碳酸酯熔融指数在3-22g/10min之间，测试条件为300℃、1.2kg。
  8. 根据权利要求1所述的PMMA/离聚体/PC三元合金，其特征在于，按重量份计，还包括0-3份的润滑剂。
  9. 权利要求1-8任一项所述的PMMA/离聚体/PC三元合金的制备方法，其特征在于，包括以下步骤：按照配比，将各组分混合均匀后，通过双螺杆挤出机挤出造粒，螺杆温度范围是200-270℃，转速范围是180-500r/min，得到PMMA/离聚体/PC三元合金。
  10. 权利要求1-8任一项所述的PMMA/离聚体/PC三元合金的应用，其特征在于，用于制备耐刮擦、高光泽制件。
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CN115368721B (zh) * 2021-05-17 2023-09-19 金发科技股份有限公司 一种抗静电母粒及其制备方法和应用
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