WO2021012888A1 - 一种热塑性耐寒汽车内饰pvc材料 - Google Patents

一种热塑性耐寒汽车内饰pvc材料 Download PDF

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WO2021012888A1
WO2021012888A1 PCT/CN2020/098739 CN2020098739W WO2021012888A1 WO 2021012888 A1 WO2021012888 A1 WO 2021012888A1 CN 2020098739 W CN2020098739 W CN 2020098739W WO 2021012888 A1 WO2021012888 A1 WO 2021012888A1
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parts
pvc material
cold
automotive interior
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French (fr)
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朱建良
朱伟
曹丽秋
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苏州爱得华塑化有限公司
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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    • C08J9/103—Azodicarbonamide
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    • C08J2327/00—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 a halogen; Derivatives of such polymers
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    • C08J2327/06—Homopolymers or copolymers of vinyl chloride
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    • 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
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    • C08J2425/08—Copolymers of styrene
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    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
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    • C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids

Definitions

  • the present invention generally relates to the field of automotive materials, and more specifically to a thermoplastic cold-resistant automotive interior PVC material.
  • the present invention provides a thermoplastic cold-resistant PVC material for automotive interior decoration.
  • the material still has good toughness when used at low temperatures.
  • thermoplastic cold-resistant automotive interior PVC material which includes the following components: PVC resin powder, phenyl silicone rubber grafted styrene-acrylonitrile (SAN), heat stabilizer, plasticizer Agents, inorganic fillers, foaming agents, lubricants and flame retardants.
  • the proportion of each component is: PVC resin powder 75-90 parts by weight, phenyl silicone rubber grafted styrene-acrylonitrile (SAN) 6-12 parts by weight, and heat stabilizer 8-90 parts by weight. 12 parts by weight, 50-70 parts by weight of plasticizer, 8-15 parts by weight of inorganic filler, 1-2 parts by weight of foaming agent, 2-4 parts by weight of lubricant, and 2-5 parts by weight of flame retardant.
  • SAN phenyl silicone rubber grafted styrene-acrylonitrile
  • phenyl silicone rubber grafted with styrene-acrylonitrile is prepared by seed emulsion polymerization. Specifically prepared by the following methods:
  • Step 1 Prepare seed latex; use deionized water, emulsifier, phenylsiloxane ring, octamethylcyclotetrasiloxane, and tetramethyldisiloxane to pre-emulsify in an emulsifier to prepare monomers
  • emulsifier phenylsiloxane ring, octamethylcyclotetrasiloxane, and tetramethyldisiloxane
  • Step 2 Preparation of grafted styrene-acrylonitrile (SAN) shell layer; continuously adding the shell layer mixture to the rubber core prepared in step 1; the shell layer mixture is composed of deionized water, emulsifier, aryl ethylene The compound and the blend of acrylonitrile and the molecular weight regulator are formed, and the reaction is stirred at the same time to prepare the composite material.
  • SAN grafted styrene-acrylonitrile
  • the plasticizer includes glyceride, isosorbide diester, vegetable oleyl ester, plant-derived polyol ester, adipate, polyadipate, adipate diester, amber One or more of acid ester, sebacic acid ester, and azelaic acid ester.
  • the blowing agent is azodicarbonamide.
  • the heat stabilizer is a calcium zinc heat stabilizer.
  • the inorganic filler includes one or more of talc, quartz, mica, kaolin, wollastonite, montmorillonite, nano calcium carbonate, calcium sulfate, and barium sulfate.
  • the lubricant includes one or more of wax, hydroxyethyl bis fatty acid amide, and ethylene bis oleamide.
  • the flame retardant is antimony trioxide and/or aluminum hydroxide.
  • thermoplastic cold-resistant automotive interior PVC material comprising the following steps:
  • the predetermined temperature is 140-180°C
  • the predetermined time is 2-8 minutes.
  • the phenyl silicone rubber has good low temperature resistance and can be elastic at minus 90°C.
  • the degree of crosslinking of rubber particles is controlled to a low level, which is conducive to its response to external forces, thereby improving the low temperature toughness of PVC resin;
  • SAN styrene-acrylonitrile
  • the phenyl silicone rubber grafted with styrene-acrylonitrile (SAN) was prepared by seed emulsion polymerization.
  • Step 1 Prepare seed latex; use 50-100 parts by weight of deionized water, 1-5 parts by weight of emulsifier, 20-60 parts by weight of phenylsiloxane ring, and 20-50 parts by weight of octamethylcyclotetrasiloxane Parts and 50-80 parts by weight of tetramethyldisiloxane are pre-emulsified in an emulsifier to prepare a pre-emulsified liquid of a monomer blend.
  • the above-mentioned emulsion is added to a mixer, and the ring is opened under the action of an acid catalyst The polymerization reaction is followed by washing with distilled water to neutrality.
  • Step 2 preparation of grafted SAN shell layer; continuously adding shell layer mixture to the rubber core prepared in step 1; the shell layer mixture consists of 24-80 parts by weight deionized water, 0.2-3 parts by weight emulsifier, It is composed of 24-54 parts by weight of a blend of arylethylene compound and acrylonitrile and 0.01-0.1 parts by weight of molecular weight regulator, the reaction temperature is 60°C-90°C, and the stirring speed is 100-500RPM.
  • the PVC material prepared according to the components and methods disclosed in the present invention meets the requirements of various indicators such as hardness, tensile strength, and elongation at break, and the impact brittleness at minus 50 degrees Celsius meets the requirements. Its low temperature performance is significantly improved.

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

一种热塑性耐寒汽车内饰PVC材料及其制备方法。该材料包括以下组分：PVC树脂粉、苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)、热稳定剂、增塑剂、无机填料、发泡剂、润滑剂和阻燃剂。通过对材料的组分进行优化，改善PVC材料的低温韧性，同时提高了其冲击吸收能力。

Description

一种热塑性耐寒汽车内饰PVC材料 技术领域
本发明总体涉及汽车材料领域，并且更具体地涉及一种热塑性耐寒汽车内饰PVC材料。
背景技术
汽车内饰材料越来越向着高档化发展，手感柔软，耐折是基本要求，但是，普通PVC材料的柔软性随着温度的变化性能会发生很大改变。在常温下正常使用的材料，在低温状态下，产品会***，柔韧性降低，同时使用寿命也降低。通常的做法是添加增塑剂和丁腈橡胶来增加产品的柔韧性，不过在实际使用过程中还是差强人意。因此，仍需研究改善PVC材料低温韧性的方法。
发明内容
针对上述问题，本发明提供一种热塑性耐寒汽车内饰PVC材料。该材料在低温使用时仍具有良好的韧性。
根据本发明的一方面，提供一种热塑性耐寒汽车内饰PVC材料，该材料包括以下组分：PVC树脂粉、苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)、热稳定剂、增塑剂、无机填料、发泡剂、润滑剂和阻燃剂。
根据本发明的一个实施例，各组分的配比为：PVC树脂粉75-90重量份、苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)6-12重量份、热稳定剂8-12重量份、增塑剂50-70重量份、无机填料8-15重量份、发泡剂1-2重量份、润滑剂2-4重量份、阻燃剂2-5重量份。
根据本发明的一个实施例，苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)通 过种子乳液聚合法制得。具体通过以下方法制备：
步骤1，制备种子胶乳；采用去离子水、乳化剂、苯基硅氧烷环体、八甲基环四硅氧烷、四甲基二硅氧烷在乳化机中进行预乳化，制备单体共混物的预乳化液，将上述乳液加入搅拌器中，在酸性催化剂的作用下进行开环聚合反应，之后用蒸馏水洗涤至中性；
步骤2，接枝苯乙烯-丙烯腈(SAN)壳层的制备；向步骤1制备的橡胶核中连续加入壳层混合液；所述壳层混合液由去离子水、乳化剂、芳基乙烯化合物和丙烯腈的共混物、分子量调节剂构成，反应同时搅拌，制备复合材料。
根据本发明的一个实施例，增塑剂包括甘油酯、异山梨醇二酯、植物油基酯、植物来源的多元醇酯、己二酸酯、聚己二酸酯、己二酸双酯、琥珀酸酯、癸二酸酯、壬二酸酯中的一种或多种。
根据本发明的一个实施例，发泡剂为偶氮二甲酰胺。
根据本发明的一个实施例，热稳定剂是钙锌热稳定剂。
根据本发明的一个实施例，无机填料包括滑石、石英、云母、高岭土、硅灰石、蒙脱石、纳米碳酸钙、硫酸钙、硫酸钡中的一种或多种。
根据本发明的一个实施例，润滑剂包括蜡、羟乙基双脂肪酰胺、亚乙基双油酰胺中的一种或多种。
根据本发明的一个实施例，阻燃剂为三氧化二锑和/或氢氧化铝。
根据本发明的另一方面，提供一种用于制备上述热塑性耐寒汽车内饰PVC材料的方法，该方法包括下列步骤：
按配比称取PVC树脂粉、苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)、热稳定剂、增塑剂、无机填料、发泡剂、润滑剂和阻燃剂；
将上述所有物质加入高速混合机上混合，混合预定时间后升温至预定温度塑化混炼；
然后经过双螺杆挤出加工，然后经过单螺杆挤出造粒，旋风分离机送 料，振动筛筛分然后包装，即获得耐寒阻燃PVC电缆材料。
根据本发明的一个实施例，预定温度为140-180℃，预定时间为2-8分钟。
本发明所公开的热塑性耐寒汽车内饰PVC材料和方法可以获得以下多种有益效果：
(1)通过对材料的组分进行优化，尤其是采用了苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)，苯基硅橡胶的耐低温性能好，能够在零下90℃具有弹性，将橡胶粒子的交联程度控制的较低，有利于其对外力进行响应，从而改善PVC树脂的低温韧性；
(2)采用苯乙烯-丙烯腈(SAN)提高苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)与PVC基体的界面亲合力，增加界面的相容性。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，下面结合具体实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
实施例1
通过种子乳液聚合法制备苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)。
步骤1，制备种子胶乳；采用去离子水50-100重量份、乳化剂1-5重量份、苯基硅氧烷环体20-60重量份、八甲基环四硅氧烷20-50重量份和四甲基二硅氧烷50-80重量份在乳化机中进行预乳化，制备单体共混物的预乳化液，将上述乳液加入搅拌器中，在酸性催化剂的作用下进行开环聚合反应，之后用蒸馏水洗涤至中性。
步骤2，接枝SAN壳层的制备；向步骤1制备的橡胶核中连续加入壳层混合液；所述壳层混合液由24-80重量份去离子水、0.2-3重量份乳化剂、24-54重量份芳基乙烯化合物和丙烯腈的共混物、0.01-0.1重量份分子量调节剂构成，反应温度为60℃-90℃，搅拌转速为100-500RPM。
实施例2
首先按以下配比分别称取：PVC树脂粉75重量份、由实施例1制备的苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)6重量份、钙锌热稳定剂8重量份、己二酸酯50重量份、纳米碳酸钙8重量份、偶氮二甲酰胺1重量份、硬脂酸锌2重量份、三氧化二锑2重量份。
将上述所有物质加入高速混合机上混合，混合2分钟后升温至180℃塑化混炼。
然后经过双螺杆挤出加工，然后经过单螺杆挤出造粒，旋风分离机送料，振动筛筛分然后包装，即获得耐寒阻燃PVC电缆材料。
实施例3
首先按以下配比分别称取：PVC树脂粉80重量份、由实施例1制备的苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)8重量份、钙锌热稳定剂9重量份、聚己二酸酯55重量份、石英8重量份、偶氮二甲酰胺1.3重量份、蜡3重量份、三氧化二锑3重量份。
将上述所有物质加入高速混合机上混合，混合4分钟后升温至170℃塑化混炼。
然后经过双螺杆挤出加工，然后经过单螺杆挤出造粒，旋风分离机送料，振动筛筛分然后包装，即获得耐寒阻燃PVC电缆材料。
实施例4
首先按以下配比分别称取：PVC树脂粉85重量份、由实施例1制备的苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)10重量份、钙锌热稳定剂10重量份、癸二酸酯60重量份、云母12重量份、偶氮二甲酰胺1.5重量份、羟乙基双脂肪酰胺3重量份、氢氧化铝4重量份。
将上述所有物质加入高速混合机上混合，混合6分钟后升温至150℃塑化混炼。
然后经过双螺杆挤出加工，然后经过单螺杆挤出造粒，旋风分离机送 料，振动筛筛分然后包装，即获得耐寒阻燃PVC电缆材料。
实施例5
首先按以下配比分别称取：PVC树脂粉90重量份、由实施例1制备的苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)12重量份、钙锌热稳定剂12重量份、壬二酸酯70重量份、高岭土15重量份、偶氮二甲酰胺2重量份、亚乙基双油酰胺4重量份、三氧化二锑2重量份、氢氧化铝3重量份。
将上述所有物质加入高速混合机上混合，混合8分钟后升温至140℃塑化混炼。
然后经过双螺杆挤出加工，然后经过单螺杆挤出造粒，旋风分离机送料，振动筛筛分然后包装，即获得耐寒阻燃PVC电缆材料。
上述实施例的性能测试结果如下：
Figure PCTCN2020098739-appb-000001
由上述测试结果可以看出，按照本发明公开的组分和方法制备的PVC材料满足硬度、拉伸强度、及断裂伸长率等各项指标的要求，并且在零下50摄氏度冲击脆性满足要求，其低温性能显著提高。
以上所述实施例仅表达了本发明的实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本 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。

Claims (10)

  1. 一种热塑性耐寒汽车内饰PVC材料，其特征在于，所述材料包括以下组分：PVC树脂粉、苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)、热稳定剂、增塑剂、无机填料、发泡剂、润滑剂和阻燃剂。
  2. 根据权利要求1所述的热塑性耐寒汽车内饰PVC材料，其特征在于，各组分的配比为：PVC树脂粉75-90重量份、苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)6-12重量份、热稳定剂8-12重量份、增塑剂50-70重量份、无机填料8-15重量份、发泡剂1-2重量份、润滑剂2-4重量份、阻燃剂2-5重量份。
  3. 根据权利要求1所述的热塑性耐寒汽车内饰PVC材料，其特征在于，所述苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)通过种子乳液聚合法制得。
  4. 根据权利要求1所述的热塑性耐寒汽车内饰PVC材料，其特征在于，所述增塑剂包括甘油酯、异山梨醇二酯、植物油基酯、植物来源的多元醇酯、己二酸酯、聚己二酸酯，己二酸双酯、琥珀酸酯、癸二酸酯、壬二酸酯中的一种或多种。
  5. 根据权利要求1所述的热塑性耐寒汽车内饰PVC材料，其特征在于，所述热稳定剂是钙锌热稳定剂。
  6. 根据权利要求1所述的热塑性耐寒汽车内饰PVC材料，其特征在于，所述无机填料包括滑石、石英、云母、高岭土、硅灰石、蒙脱石、纳米碳酸钙、硫酸钙、硫酸钡中的一种或多种。
  7. 根据权利要求1所述的热塑性耐寒汽车内饰PVC材料，其特征在于，所述阻燃剂为三氧化二锑和/或氢氧化铝。
  8. 根据权利要求1所述的热塑性耐寒汽车内饰PVC材料，其特征在于，所述润滑剂包括蜡、羟乙基双脂肪酰胺、亚乙基双油酰胺中的一种或多种。
  9. 一种用于制备根据权利要求1-8中任一项所述的热塑性耐寒汽车内饰PVC材料的方法，其特征在于，所述方法包括下列步骤：
    按配比称取PVC树脂粉、苯基硅橡胶接枝苯乙烯-丙烯腈(SAN)、热稳定剂、增塑剂、无机填料、发泡剂、润滑剂和阻燃剂；
    将上述所有物质加入高速混合机上混合，混合预定时间后升温至预定温度塑化混炼；
    然后经过双螺杆挤出加工，然后经过单螺杆挤出造粒，旋风分离机送料，振动筛筛分然后包装，即获得耐寒阻燃PVC电缆材料。
  10. 根据权利要求9所述的方法，其特征在于，所述预定温度为140-180℃，所述预定时间为2-8分钟。
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