WO2022110661A1 - 一种高韧高光泽gpps/cpe复合材料及其制备方法和应用 - Google Patents

一种高韧高光泽gpps/cpe复合材料及其制备方法和应用 Download PDF

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WO2022110661A1
WO2022110661A1 PCT/CN2021/092764 CN2021092764W WO2022110661A1 WO 2022110661 A1 WO2022110661 A1 WO 2022110661A1 CN 2021092764 W CN2021092764 W CN 2021092764W WO 2022110661 A1 WO2022110661 A1 WO 2022110661A1
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gpps
composite material
gloss
toughness
flame retardant
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French (fr)
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刘凯
黄险波
叶南飚
付锦锋
秦旺平
王亮
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金发科技股份有限公司
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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
    • 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
    • C08L25/06—Polystyrene
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K3/2279—Oxides; Hydroxides of metals of antimony
    • C08K2003/2282—Antimonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant

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  • the invention relates to the field of polymer plastics, and more particularly, to a high-toughness and high-gloss GPPS/CPE composite material and a preparation method and application thereof.
  • General purpose polystyrene can be understood as a linear polyethylene chain with many benzene rings attached to the side, which increases the glass transition temperature and the refractive index. Not easy to bend, high gloss, smooth and dimensional stability are the main characteristics of this material, and at the same time it has the advantages of easy processing and molding, transparency, cheapness, insulation, good printability, etc. It is widely used in household appliances, office equipment, power tools and automotive fields, but its toughness is poor; it cannot be used in products that require high toughness, which limits its application range.
  • HIPS high impact polystyrene
  • a widely adopted method is to modify general-purpose polystyrene by adding rubber to form high impact polystyrene (HIPS), although The addition of rubber endows HIPS with some special properties, but for impact performance, this method is at the expense of the high gloss of GPPS, which greatly limits the application of HIPS in the field of high gloss products.
  • HIPS is a flammable material, usually a considerable proportion of bromine antimony flame retardant is added to have flame retardancy.
  • brominated flame retardants are expensive, resulting in higher production costs.
  • Cia160036A discloses a flame-retardant high-impact polystyrene resin and a preparation method thereof.
  • the solution adopts a mixture of inorganic minerals and inorganic substances to partially replace antimony trioxide, which ensures the flame-retardant effect and mechanical properties. , but this solution still does not solve the problem of poor gloss, which limits its need to be used in high-gloss scenes.
  • the present invention provides a high toughness and high gloss GPPS/CPE composite material in order to overcome the defects of the GPPS and HIPS described in the prior art.
  • Another object of the present invention is to provide a preparation method of the high toughness and high gloss GPPS/CPE composite material.
  • Another object of the present invention is to provide the application of the high toughness and high gloss GPPS/CPE composite material.
  • a low-cost flame-retardant and high-gloss GPPS/CPE composite material comprising the following components calculated in parts by weight:
  • the present invention adopts GPPS resin (number average molecular weight Mn is 6.5-7.0*10 4 g/mol) and chlorinated polyethylene to compound, because CPE itself has high toughness, so the toughness of the composite material can be improved, and at the same time, CPE also has The flame retardant function can replace some brominated flame retardants, and under the premise of ensuring V-0 flame retardant, the addition of brominated flame retardants is reduced, so that the cost of the GPPS resin composition is lower; Compared with polybutadiene rubber, chlorinated polyethylene has less influence on the gloss of composite materials, so that chlorinated polyethylene can still maintain high gloss after compounding with GPPS resin.
  • the mass percentage of chlorine content in the chlorinated polyethylene is 30% to 40%.
  • the flame retardant effect will decrease; when the chlorine content is higher than 40%, the toughening effect will decrease. worse.
  • the chlorine content in the chlorinated polyethylene is determined by the following method:
  • the determination of chlorine content is carried out in accordance with GB-T7139-2002 "Determination of Chlorine Content of Plastic Vinyl Chloride Homopolymers and Copolymers", the sample is oxidized with sodium peroxide or gaseous oxygen, and then titrated by potentiometric titration or volumetric titration to generate of chloride.
  • the brominated flame retardant is bromotriazine and/or decabromodiphenylethane.
  • the brominated flame retardant is bromotriazine.
  • the antimony-based flame retardant is antimony trioxide and/or antimony pentoxide, which is combined with a brominated flame retardant to improve flame retardancy.
  • the antioxidant is a hindered phenolic antioxidant and/or a phosphite antioxidant to improve the antioxidant capacity of the composite material.
  • the lubricant is one or both of zinc stearate, magnesium stearate or ethylene bis-stearamide.
  • the heat stabilizer is any one or both of methyl tin mercaptide stabilizer and calcium zinc stabilizer.
  • the present invention also includes the preparation method of the high-toughness and high-gloss GPPS/CPE composite material, comprising the following steps:
  • the premix prepared in S1. is sent to an extruder for kneading, extrusion and post-processing.
  • the post-processing includes the steps of drawing, cooling, dicing and the like.
  • the invention provides a high-toughness and high-gloss GPPS/CPE composite material.
  • CPE enables the composite material to have high toughness and high gloss, the gloss reaches more than 70, and the notched impact strength of the cantilever beam reaches more than 9KJ/m 2 , And while reducing the brominated flame retardant, the high flame retardant grade of the composite material is ensured, the cost of the composite material is effectively reduced, and the method can be applied to the preparation of household appliances and office equipment.
  • reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the technical field.
  • GPPS resin GPPS-123P, the number average molecular weight Mn is 6.5*10 4 g/mol, Shanghai SECCO Petrochemical Co., Ltd.;
  • HIPS resin PS 350K, Taiwan Guoqiao Petrochemical Co., Ltd.;
  • Chlorinated polyethylene A CPE-132C, chlorine content of 32%, Keli Chemical Co., Ltd.;
  • Chlorinated polyethylene B chlorine content 20%, Rizhao Sanxing Chemical Co., Ltd.;
  • Chlorinated polyethylene C chlorine content 45%, Changrui Chemical Co., Ltd.;
  • Brominated flame retardant A bromotriazine, FR-245 provided by Israel Dead Sea Bromine Company;
  • Brominated flame retardant B decabromodiphenylethane, SAYTEX4010 provided by Albemarle Corporation;
  • Brominated flame retardant C Tetrabromobisphenol A, FR-1524 provided by Israel Dead Sea Bromine Company;
  • Antimony flame retardant A antimony trioxide, Huachang Antimony Industry Company
  • Antimony flame retardant B sodium antimonate, Ruifeng Antimony Industry Co., Ltd.;
  • Antioxidant hindered phenolic antioxidant THANOX 1010, Ciba CIBA Refining Company
  • Lubricant Zinc stearate, Dongguan Nuojia Plastic & Chemical Co., Ltd.;
  • Heat stabilizer SW-977 thiol methyl tin stabilizer, Hubei Benxing Chemical Co., Ltd.
  • the GPPS/CPE composite materials of each embodiment of the present invention and the comparative example are prepared through the following process:
  • the premix prepared in S1 is sent to an extruder for kneading, extrusion, drawing, cooling and pelletizing.
  • the extrusion process temperature is 190-200°C, and the feeding rate is 80kg/h.
  • the present embodiment and comparative example provide a series of GPPS/CPE composite materials, the formula of which is shown in Table 3
  • Izod notched impact strength ISO 180-2000;
  • Flame retardant grade UL 94-2018, the thickness of the test sample is 2.0mm.
  • Example 9 adding chlorinated polyethylene B (chlorine content 20%), its flame retardant effect is It can reach V-0, but the extinguishing time is relatively long, and the flame retardant effect is slightly poor; in Example 10, adding chlorinated polyethylene C (chlorine content 45%), its impact strength is only 9.0kJ/m 2 , and the chlorinated polyethylene C increases.
  • the toughness effect is slightly worse than that of chlorinated polyethylene A.
  • the former has extremely high gloss, but the impact strength is only 3.8J/m 2 , which cannot meet the application requirements; the latter has higher impact strength and low gloss. And both, under the condition of adding the same flame retardant as in the example, the flame retardant grade is only V-2, which is lower than V-0.
  • the impact strength of the comparative example 3 is not enough, the flame retardant grade is only V-1, and the glossiness of the comparative example 4 is low.
  • Examples 1-13 Compared with Comparative Examples 1-4, Examples 1-13 have better toughness and gloss at the same time, and can also achieve V-0 flame retardant, which can meet the demand.

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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)

Abstract

本发明公开了一种高韧高光泽GPPS/CPE复合材料及其制备方法和应用。所述复合材料包括如下按重量份计算的组分：GPPS树脂50～60份；氯化聚乙烯30～40份；溴系阻燃剂6～15份；锑系阻燃剂3～5份；抗氧剂0.2～1份；润滑剂0.2～1份；热稳定剂0.2～1份。所述复合材料具有高韧性和高光泽度，光泽度达到70以上，缺口冲击强度达到9kJ/m 2以上，并且在降低溴系阻燃剂的同时保证复合材料的高阻燃等级，有效降低了复合材料的成本，能够应用于制备家用电器、办公设备中。

Description

一种高韧高光泽GPPS/CPE复合材料及其制备方法和应用 技术领域
本发明涉及高分子塑料领域，更具体地，涉及一种高韧高光泽GPPS/CPE复合材料及其制备方法和应用。
背景技术
通用聚苯乙烯(general purpose polystyrene，GPPS)可以理解为一条线性聚乙烯链的侧面连接了许多苯环，从而使得玻璃化转变温度升高以及折射率变大。不易弯曲、高光泽、光滑和尺寸稳定性是这种材料的主要特征，同时具有易加工成型，透明、廉价、绝缘、印刷性好等优点的优点，广泛应用于家用电器、办公设备、电动工具和汽车等领域，但是其韧性较差；不能应用于需要韧性较高的产品中，限制了其应用范围。
虽然目前针对通用聚苯乙烯冲击性能较差的缺陷，一种广泛采用的方式是通过加入橡胶对通用聚苯乙烯进行改性，形成了高抗冲聚苯乙烯(high impact polystyrene，HIPS)，尽管橡胶的加入赋予了HIPS一些特殊的性能，但是对于冲击性能来说，这种方法是以牺牲GPPS的高光泽作为代价，这极大限制了HIPS在高光泽产品领域中的应用。另外，HIPS是易燃材料，通常要加入相当多比例的溴锑阻燃剂，才能具有阻燃性。但是，溴系阻燃剂价格昂贵，导致生产成本较高。
中国专利(CN103160036A)公开了一种阻燃高抗冲击性聚苯乙烯树脂及其制备方法，该方案采用了无机矿物和无机物的混合物部分替代三氧化二锑，保证了阻燃效果和力学性能，但是该方案依旧没有解决光泽度差的问题，限制了其需要应用在高光泽的场景。
因此，目前GPPS和HIPS均有缺陷，不能满足高光泽和高韧性的聚苯烯树脂组合物。
发明内容
本发明为克服上述现有技术所述GPPS和HIPS的缺陷，提供一种高韧高光泽GPPS/CPE复合材料。
本发明的另一目的在于提供所述高韧高光泽GPPS/CPE复合材料的制备方 法。
本发明的另一目的在于提供所述高韧高光泽GPPS/CPE复合材料的应用。
为实现上述目的，本发明采用的技术方案是：
一种低成本阻燃高光泽GPPS/CPE复合材料，包括如下按重量份计算的组分：
Figure PCTCN2021092764-appb-000001
本发明采用GPPS树脂(数均分子量Mn为6.5-7.0*10 4g/mol)和氯化聚乙烯复配，因为CPE本身具有很高的韧性，因此可以提高复合材料的韧性，同时CPE还具有阻燃的功能，能够替代部分溴系阻燃剂，保证V-0阻燃前提下，减少溴系阻燃剂的添加，使得GPPS树脂组合物的成本更低；此外，发明人意外发现，氯化聚乙烯相对于聚丁二烯橡胶对复合材料的光泽性影响更小，使得氯化聚乙烯与GPPS树脂复配后，依然能够保持高光泽。
优选地，所述氯化聚乙烯中氯含量的质量百分比为30％～40％，当氯含量低于30％时，阻燃效果会下降；当氯含量高于40％时，增韧效果会变差。
所述氯化聚乙烯中氯含量通过以下方法测定：
氯含量的测定按照GB-T7139-2002《塑料氯乙烯均聚物和共聚物氯含量的测定》执行，试样用过氧化钠或气态氧氧化，然后用电位滴定法或容量滴定法滴定生成的氯化物。
优选地，所述溴系阻燃剂为溴代三嗪和/或十溴二苯乙烷。
优选地，所述溴系阻燃剂为溴代三嗪。
优选地，所述锑系阻燃剂为三氧化二锑和/或五氧化二锑，是与溴系阻燃剂配合提高阻燃。
优选地，所述抗氧剂为受阻酚类抗氧剂和/或亚磷酸酯类抗氧剂，提高复合材料的抗氧化能力。
优选地，所述润滑剂为硬脂酸锌、硬脂酸镁或乙撑双硬脂酰胺中的一种或两种。
优选地，所述热稳定剂为硫醇甲基锡稳定剂、钙锌稳定剂中的任一种或两种。
本发明还包括所述高韧高光泽GPPS/CPE复合材料的制备方法，包括以下步骤：
S1.称取GPPS树脂、氯化聚乙烯、溴系阻燃剂、锑系阻燃剂、抗氧剂、润滑剂和热稳定剂加入混合机中混合均匀，得到预混物；
S2.将S1.制备得到的预混物送入挤出机中混炼、挤出、后加工制得。
所述后加工包括拉条、冷却、切粒等步骤。
所述高韧高光泽GPPS/CPE复合材料在制备家用电器、办公设备制品中的应用。
与现有技术相比，本发明的有益效果是：
本发明提供了一种高韧高光泽GPPS/CPE复合材料，通过CPE的加入，使得复合材料具有高韧性和高光泽度，光泽度达到70以上，悬臂梁缺口冲击强度达到9KJ/m 2以上，并且在降低溴系阻燃剂的同时保证复合材料的高阻燃等级，有效降低了复合材料的成本，能够应用于制备家用电器、办公设备中。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，但本发明的实施方式不限于此。
本发明所采用的试剂、方法和设备，如无特殊说明，均为本技术领域常规试剂、方法和设备。
以下实施例及对比例中采用的原料如下：
GPPS树脂：GPPS-123P，数均分子量Mn为6.5*10 4g/mol，上海赛科石油化工有限公司；
HIPS树脂：PS 350K，台湾国乔石油化学股份有限公司；
氯化聚乙烯A：CPE-132C，氯元素含量为32％，科利化工有限公司；
氯化聚乙烯B：氯元素含量20％，日照市三星化工有限公司；
氯化聚乙烯C：氯元素含量45％，昌瑞化工有限公司；
溴系阻燃剂A：溴代三嗪，以色列死海溴公司提供的FR-245；
溴系阻燃剂B：十溴二苯乙烷，美国雅宝公司提供的SAYTEX4010；
溴系阻燃剂C：四溴双酚A，以色列死海溴公司提供的FR-1524；
锑系阻燃剂A：三氧化二锑，华昌锑业公司；
锑系阻燃剂B：锑酸钠，瑞锋锑业有限公司；
抗氧剂：受阻酚类抗氧剂THANOX 1010，汽巴CIBA精化公司；
润滑剂：硬脂酸锌，东莞市诺佳塑化有限公司；
热稳定剂：SW-977硫醇甲基锡稳定剂，湖北犇星化工有限公司。
本发明各实施例及对比例的GPPS/CPE复合材料通过如下过程制备得到：
S1.称取GPPS树脂、氯化聚乙烯、溴系阻燃剂、锑系阻燃剂、抗氧剂、润滑剂和热稳定剂加入混合机中混合均匀，得到预混物；
S2.将S1制备得到的预混物送入挤出机中混炼、挤出、拉条、冷却、切粒制得，挤出工艺温度为190～200℃，喂料速度为80kg/h。
实施例1～8
表1实施例1～8复合材料的配方(份)
Figure PCTCN2021092764-appb-000002
实施例9～13和对比例1～4
本实施例和对比例提供一系列的GPPS/CPE复合材料，其配方如表3
表3实施例9～13与对比例1～4的配方(份)
Figure PCTCN2021092764-appb-000003
Figure PCTCN2021092764-appb-000004
材料性能测试标准：
光泽度：GB/T 8807-1988；
悬臂梁缺口冲击强度：ISO 180-2000；
阻燃等级：UL 94-2018，测试样品厚度为2.0mm。
表4各实施例和对比例的性能测试结果
Figure PCTCN2021092764-appb-000005
Figure PCTCN2021092764-appb-000006
从实施例1～3看，随着GPPS树脂比例的增加，GPPS/CPE复合材料的光泽度随之提高，冲击强度随之下降，但是下降幅度不大。
从实施例3～5看，随着CPE含量的增加，GPPS/CPE复合材料的冲击强度不断提高，CPE具有较好的增韧效果，同时光泽度会略微下降。
从实施例3和6～8看，当随着阻燃燃剂A的分数从6-15份范围内增大，复合材料的冲击强度略有下降，但依然在9.1以上。
从实施例3和9～10看，与实施例3加入氯化聚乙烯A(氯含量32％)相比，实施例9加入氯化聚乙烯B(氯含量20％)，其阻燃效果虽然能达到V-0，但是熄灭时间比较久，阻燃效果稍差；实施例10加入氯化聚乙烯C(氯含量45％)，其冲击强度只有9.0kJ/m 2，氯化聚乙烯C增韧效果相比氯化聚乙烯A稍差。
实施例11-13采用不同的溴系阻燃剂和锑系阻燃剂组合也能实现上述目的，保持高光泽和高韧性，并具有V-0阻燃。
从对比例1和2看，前者光泽度极高，但是冲击强度只有3.8J/m 2，不能满足使用要求；后者冲击强度较高，光泽度很低。并且二者，在加入与实施例相同的阻燃剂条件下，阻燃等级只有V-2，低于V-0。
从对比例3和4看，对比例3的冲击强度不够，阻燃等级只有V-1，对比例4的光泽度偏低。
相比对比例1-4，实施例1-13同时具有较好的韧性和光泽度，还能实现V-0阻燃，能够满足需求。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明权利要求的保护范围之内。

Claims (10)

  1. 一种高韧高光泽GPPS/CPE复合材料，其特征在于，包括如下按重量份计算的组分：
    Figure PCTCN2021092764-appb-100001
  2. 如权利要求1所述高韧高光泽GPPS/CPE复合材料，其特征在于，所述氯化聚乙烯中氯元素的质量百分比含量为30％～40％。
  3. 如权利要求1所述高韧高光泽GPPS/CPE复合材料，其特征在于，所述溴系阻燃剂为溴代三嗪和/或十溴二苯乙烷。
  4. 如权利要求1所述高韧高光泽GPPS/CPE复合材料，其特征在于，所述溴系阻燃剂为溴代三嗪。
  5. 如权利要求1所述高韧高光泽GPPS/CPE复合材料，其特征在于，所述锑系阻燃剂为三氧化二锑和/或五氧化二锑。
  6. 如权利要求1所述高韧高光泽GPPS/CPE复合材料，其特征在于，所述抗氧剂为受阻酚类抗氧剂和/或亚磷酸酯类抗氧剂。
  7. 如权利要求1所述高韧高光泽GPPS/CPE复合材料，其特征在于，所述润滑剂为硬脂酸锌、硬脂酸镁或乙撑双硬脂酰胺中的一种或两种。
  8. 如权利要求1所述高韧高光泽GPPS/CPE复合材料，其特征在于，所述热稳定剂为硫醇甲基锡稳定剂和/或钙锌稳定剂。
  9. 如权利要求1～8任一项所述高韧高光泽GPPS/CPE复合材料的制备方法，其特征在于，包括以下步骤：
    S1.称取GPPS树脂、氯化聚乙烯、溴系阻燃剂、锑系阻燃剂、抗氧剂、润滑剂和热稳定剂加入混合机中混合均匀，得到预混物；
    S2.将S1制备得到的预混物送入挤出机中混炼、挤出、后加工制得。
  10. 如权利要求1～8任一项所述高韧高光泽GPPS/CPE复合材料在制备家用 电器、办公设备中的应用。
PCT/CN2021/092764 2020-11-26 2021-05-10 一种高韧高光泽gpps/cpe复合材料及其制备方法和应用 WO2022110661A1 (zh)

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