WO2021012897A1 - 一种免辐照耐高温pvc材料 - Google Patents

一种免辐照耐高温pvc材料 Download PDF

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WO2021012897A1
WO2021012897A1 PCT/CN2020/098919 CN2020098919W WO2021012897A1 WO 2021012897 A1 WO2021012897 A1 WO 2021012897A1 CN 2020098919 W CN2020098919 W CN 2020098919W WO 2021012897 A1 WO2021012897 A1 WO 2021012897A1
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parts
weight
temperature
radiation
temperature resistant
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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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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—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 a halogen; Compositions of derivatives of such polymers
    • C08L27/02—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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04—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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06—Homopolymers or copolymers of vinyl chloride
    • 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
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • 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
    • C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

Definitions

  • the present invention generally relates to the field of automotive materials, and more specifically relates to a radiation-free high-temperature PVC material.
  • the automotive wire insulation materials with a temperature resistance of 125°C on the market are mainly radiation cross-linking, but the investment in irradiation equipment is large, and a large amount of waste water is generated during irradiation, which causes great environmental pollution. At the same time, the cost of waste water treatment is too high. There is physical damage to the operator, and the material is easy to crack during the irradiation crosslinking process.
  • heat stabilizers are added to improve the high temperature stability of PVC materials, but there is still room for further improving the high temperature stability of PVC materials.
  • the present invention provides a radiation-free high-temperature PVC material.
  • the material uses modified hydrotalcite, which not only improves the dispersibility of the hydrotalcite in the matrix material, but also improves its compatibility with the matrix material, thereby significantly improving the high-temperature thermal stability of the PVC material.
  • a radiation-free high-temperature resistant PVC material which includes the following components: PVC resin powder, modified hydrotalcite, heat stabilizer, plasticizer, processing softening aid, modification aid Agents, antioxidants, flame retardants, ultraviolet absorbers.
  • the proportion of each component is 90-110 parts by weight of PVC resin powder, 12-15 parts by weight of modified hydrotalcite, 8-16 parts by weight of heat stabilizer, and 40-60 parts by weight of plasticizer. Parts by weight, 1-2 parts by weight of processing softening aids, 4-8 parts by weight of modification aids, 2-4 parts by weight of flame retardants, 0.5-1 parts by weight of antioxidants, and 0.5-1 parts by weight of ultraviolet absorbers.
  • the modified hydrotalcite is obtained by replacing part of the anions in the hydrotalcite with terephthalate. Specifically prepared by the following methods:
  • Nano hydrotalcite material dispersion take appropriate amount of nano hydrotalcite, such as MgAl-CO 3 type, ZnMgAl-CO 3 type and similar LDH materials containing rare earth elements, put it in an appropriate amount of ethylene glycol, and adjust the pH to acidity , At about 5, ultrasonic stirring is made into a suspension for use;
  • nano hydrotalcite such as MgAl-CO 3 type, ZnMgAl-CO 3 type and similar LDH materials containing rare earth elements
  • the plasticizer includes one or more of glyceride, polyadipate, diester of adipate, and azelate.
  • the heat stabilizer is one or more of calcium-zinc heat stabilizer and zinc stearate.
  • the processing softening aid is ACR401 processing softening aid.
  • the antioxidant includes one or more of 1076 antioxidant or phosphite.
  • the modification aid is NR188.
  • the feed is conveyed to the twin-screw extruder, and after granulation by the twin-screw extruder, it is water-cooled and hot-cut.
  • the first predetermined temperature is 110°C-130°C
  • the second predetermined temperature is 40°C-60°C.
  • the temperature of each zone in the twin-screw extruder is controlled as follows, the feed zone is 173°C -185 °C, the plasticizing zone is 175°C-185°C, the head temperature is 180°C-190°C, and the water cooling temperature is 10°C-30°C.
  • the radiation-free, high-temperature resistant PVC material and method disclosed in the present invention can obtain the following beneficial effects:
  • the groups introduced between the layers can inhibit the agglomeration between particles, thereby improving the dispersibility of the hydrotalcite in the matrix material;
  • Nano-hydrotalcite material dispersion Take 0.5g of ZnMgAl-CO 3 type nano-hydrotalcite, put it into 80ml ethylene glycol, adjust the pH value to acidity, raise the temperature to 60°C, and ultrasonically stir for 2h to make a suspension Liquid ready for use;
  • the mass ratio of acid and hydrotalcite of 2:1 weigh the terephthalic acid and dissolve it in 150ml of ethylene glycol, add the dispersed hydrotalcite suspension to the ethylene glycol with terephthalic acid, and heat up The temperature is about 100-150°C, stirred, the two react for 30 minutes, centrifuged to obtain powder, washed to neutrality, and dried at 80°C to obtain modified nano hydrotalcite powder.
  • the raw materials are put into the extrusion feeder for extruding and feeding.
  • the feed is conveyed to the twin-screw extruder. After granulation by the twin-screw extruder, it is water-cooled and hot-cut.
  • the temperature of each zone in the twin-screw extruder is controlled as follows, the feeding zone is 173°C, and the plasticizing zone is 175°C , The head temperature is 180°C, and the water-cooled temperature is 10°C.
  • the raw materials are put into the extrusion feeder for extruding and feeding.
  • the feed is conveyed to the twin-screw extruder. After granulation by the twin-screw extruder, it is water-cooled and hot-cut.
  • the temperature of each zone in the twin-screw extruder is controlled as follows, the feeding zone is 178°C, and the plasticization zone is 180°C , The head temperature is 183°C, and the water-cooled temperature is 15°C.
  • the raw materials are put into the extrusion feeder for extruding and feeding.
  • the feed is conveyed to the twin-screw extruder. After granulation by the twin-screw extruder, it is water-cooled and eagerly cut.
  • the temperature of each zone in the twin-screw extruder is controlled as follows, the feeding zone is 183°C, and the plasticization zone is 185°C , The head temperature is 185°C, and the water-cooled temperature is 20°C.
  • the raw materials are put into the extrusion feeder for extruding and feeding.
  • the feed is conveyed to the twin-screw extruder. After granulation by the twin-screw extruder, it is water-cooled and hot-cut.
  • the temperature of each zone in the twin-screw extruder is controlled as follows, the feeding zone is 185°C, and the plasticizing zone is 185°C , The head temperature is 190°C, and the water-cooled temperature is 30°C.

Abstract

一种免辐照耐高温PVC材料，该材料包括以下组分：PVC树脂粉、改性水滑石、热稳定剂、增塑剂、加工软化助剂、改性助剂、抗氧剂、阻燃剂、紫外线吸收剂。该材料采用对苯二甲酸根置换处理的改性水滑石，在层间引入的基团可以抑制粒子间的团聚，进而改善了水滑石在基体材料中的分散性。苯基团的引入可以改善水滑石与基体材料的相容性。

Description

一种免辐照耐高温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免辐照耐高温PVC材料。
背景技术
现在市面上耐温125℃的汽车线绝缘料以辐照交联为主，但是辐照设备投资大，辐照时产生大量的废水对环境污染大，同时废水处理成本太高，辐照时射线存在对操作人员的身体伤害，同时在辐照交联过程中材料容易开裂。另外还采用添加热稳定剂的方式来改善PVC材料的高温稳定性，但仍存在进一步改善PVC材料高温稳定性的空间。
发明内容
针对上述问题，本发明提供一种免辐照耐高温PVC材料。该材料使用改性水滑石，不仅提高了水滑石在基体材料中的分散性，还改善了其与基体材料的相容性，进而显著提高了PVC材料的高温热稳定性。
根据本发明的一方面，提供一种免辐照耐高温PVC材料，该材料包括以下组分：PVC树脂粉、改性水滑石、热稳定剂、增塑剂、加工软化助剂、改性助剂、抗氧剂、阻燃剂、紫外线吸收剂。
根据本发明的一个实施例，各组分的配比为：PVC树脂粉90-110重量份、改性水滑石12-15重量份、热稳定剂8-16重量份、增塑剂40-60重量份、加工软化助剂1-2重量份、改性助剂4-8重量份、阻燃剂2-4重量份、抗氧剂0.5-1重量份、紫外线吸收剂0.5-1重量份。
根据本发明的一个实施例，改性水滑石是采用对苯二甲酸根对水滑石 中的部分阴离子置换处理获得。具体通过以下方法制备：
纳米水滑石材料分散：取适量的纳米水滑石，例如MgAl-CO 3型、ZnMgAl-CO 3型以及与含有稀土元素的类似LDH材料，将其放入适量乙二醇中，调节pH值至酸性，在5左右，超声搅拌制成悬浊液待用；
称取定量的对苯二甲酸溶于乙二醇中，将分散好的水滑石悬浊液加入溶有对苯二甲酸的乙二醇中，升温至100-150℃左右，搅拌，使两者反应30分钟，离心获得粉体，洗涤至中性，干燥获得改性纳米水滑石粉。
根据本发明的一个实施例，增塑剂包括甘油酯、聚己二酸酯、己二酸双酯、壬二酸酯中的一种或多种。
根据本发明的一个实施例，热稳定剂是钙锌热稳定剂、硬脂酸锌中的一种或多种。
根据本发明的一个实施例，加工软化助剂为ACR401加工软化助剂。
根据本发明的一个实施例，抗氧剂包括1076抗氧剂或亚磷酸酯中的一种或多种。
根据本发明的一个实施例，改性助剂为NR188。
根据本发明的另一方面，提供一种用于制备上述免辐照耐高温PVC材料的方法，该方法包括下列步骤：
按配比称取PVC树脂粉、改性水滑石、热稳定剂、增塑剂、加工软化助剂、改性助剂、抗氧剂、阻燃剂、紫外线吸收剂；
将上述所有物质加入高速螺杆捏和机内进行调整捏和，待达到第一预定温度时排料至冷混机进行冷却；
当混合料在冷混机中温度下降到第二预定温度时，将原料放入挤出喂料机挤出喂料；
将喂料输送至双螺杆挤出机，经双螺杆挤出机造粒后，进行水冷热切。
根据本发明的一个实施例，第一预定温度为110℃-130℃，第二预定温度为40℃-60℃，双螺杆挤出机中各区的温度控制如下，进料区为173℃ -185℃，塑化区为175℃-185℃，机头温度为180℃-190℃，水冷的温度为10℃-30℃。
本发明所公开的免辐照耐高温PVC材料和方法可以获得以下多种有益效果：
(1)采用对苯二甲酸根置换处理的改性水滑石，在层间引入的基团可以抑制粒子间的团聚，进而改善了水滑石在基体材料中的分散性；
(2)苯基团的引入可以改善水滑石与基体材料的相容性；
(3)水滑石中的部分CO 3 2+被置换，但仍有一部分被保留以保持其吸收HCl的能力；
(4)当将改性水滑石与硬脂酸锌复配使用时，两者协同，取得了比使用双份量的单一组分物质更好的热稳定性改善作用，尤其是改善长期热稳定性方面。
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
制备改性纳米水滑石材料。
步骤1，纳米水滑石材料分散：取0.5g的ZnMgAl-CO 3型纳米水滑石，将其放入80ml乙二醇中，调节pH值至酸性，升温至60℃，超声搅拌2h制成悬浊液待用；
按酸和水滑石的质量比为2:1称取对苯二甲酸溶于150ml的乙二醇中，将分散好的水滑石悬浊液加入溶有对苯二甲酸的乙二醇中，升温至100-150℃左右，搅拌，使两者反应30分钟，离心获得粉体，洗涤至中性，80℃干燥获得改性纳米水滑石粉。
实施例2
首先按以下配比分别称取：PVC树脂粉90重量份、改性水滑石12重量份、钙锌热稳定剂8重量份、甘油酯40重量份、ACR401加工软化助剂1重量份、NR188改性助剂4重量份、三氧化二锑2重量份、1076抗氧剂0.5重量份、UV531紫外线吸收剂0.5重量份。
将上述所有物质加入高速螺杆捏和机内进行调整捏和，待达到110℃时排料至冷混机进行冷却。
当混合料在冷混机中温度下降到40℃时，将原料放入挤出喂料机挤出喂料。
将喂料输送至双螺杆挤出机，经双螺杆挤出机造粒后，进行水冷热切，双螺杆挤出机中各区的温度控制如下，进料区为173℃，塑化区为175℃，机头温度为180℃，水冷的温度为10℃。
实施例3
首先按以下配比分别称取：PVC树脂粉90重量份、改性水滑石13重量份、硬脂酸锌热稳定剂10重量份、聚己二酸酯45重量份、ACR401加工软化助剂1.5重量份、NR188改性助剂5重量份、三氧化二锑3重量份、1076抗氧剂0.7重量份、UV531紫外线吸收剂0.7重量份。
将上述所有物质加入高速螺杆捏和机内进行调整捏和，待达到120℃时排料至冷混机进行冷却。
当混合料在冷混机中温度下降到50℃时，将原料放入挤出喂料机挤出喂料。
将喂料输送至双螺杆挤出机，经双螺杆挤出机造粒后，进行水冷热切，双螺杆挤出机中各区的温度控制如下，进料区为178℃，塑化区为180℃，机头温度为183℃，水冷的温度为15℃。
实施例4
首先按以下配比分别称取：PVC树脂粉100重量份、改性水滑石14重 量份、硬脂酸锌稳定剂14重量份、己二酸双酯55重量份、ACR401加工软化助剂1.8重量份、NR188改性助剂6重量份、三氧化二锑3重量份、1076抗氧剂0.8重量份、UV531紫外线吸收剂0.8重量份。
将上述所有物质加入高速螺杆捏和机内进行调整捏和，待达到120℃时排料至冷混机进行冷却。
当混合料在冷混机中温度下降到55℃时，将原料放入挤出喂料机挤出喂料。
将喂料输送至双螺杆挤出机，经双螺杆挤出机造粒后，进行水冷热切，双螺杆挤出机中各区的温度控制如下，进料区为183℃，塑化区为185℃，机头温度为185℃，水冷的温度为20℃。
实施例5
首先按以下配比分别称取：PVC树脂粉110重量份、改性水滑石15重量份、硬脂酸锌热稳定剂16重量份、壬二酸酯60重量份、ACR401加工软化助剂2重量份、NR188改性助剂8重量份、三氧化二锑4重量份、1076抗氧剂1重量份、UV531紫外线吸收剂1重量份。
将上述所有物质加入高速螺杆捏和机内进行调整捏和，待达到130℃时排料至冷混机进行冷却。
当混合料在冷混机中温度下降到60℃时，将原料放入挤出喂料机挤出喂料。
将喂料输送至双螺杆挤出机，经双螺杆挤出机造粒后，进行水冷热切，双螺杆挤出机中各区的温度控制如下，进料区为185℃，塑化区为185℃，机头温度为190℃，水冷的温度为30℃。
上述实施例的性能测试结果如下：
Figure PCTCN2020098919-appb-000001
Figure PCTCN2020098919-appb-000002
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材料热稳定性较好，其它性能也符合要求。
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. 一种免辐照耐高温PVC材料，其特征在于，所述材料包括以下组分：PVC树脂粉、改性水滑石、热稳定剂、增塑剂、加工软化助剂、改性助剂、抗氧剂、阻燃剂、紫外线吸收剂。
  2. 根据权利要求1所述的免辐照耐高温PVC材料，其特征在于，各组分的配比为：PVC树脂粉90-110重量份、改性水滑石12-15重量份、热稳定剂8-16重量份、增塑剂40-60重量份、加工软化助剂1-2重量份、改性助剂4-8重量份、阻燃剂2-4重量份、抗氧剂0.5-1重量份、紫外线吸收剂0.5-1重量份。
  3. 根据权利要求1所述的免辐照耐高温PVC材料，其特征在于，所述改性水滑石是采用对苯二甲酸根对水滑石中的部分阴离子置换处理获得。
  4. 根据权利要求1所述的免辐照耐高温PVC材料，其特征在于，所述增塑剂包括甘油酯、聚己二酸酯、己二酸双酯、壬二酸酯中的一种或多种。
  5. 根据权利要求1所述的免辐照耐高温PVC材料，其特征在于，所述热稳定剂是钙锌热稳定剂、硬脂酸锌中的一种或多种。
  6. 根据权利要求1所述的免辐照耐高温PVC材料，其特征在于，所述加工软化助剂为ACR401加工软化助剂。
  7. 根据权利要求1所述的免辐照耐高温PVC材料，其特征在于，所述抗氧剂包括1076抗氧剂或亚磷酸酯中的一种或多种。
  8. 根据权利要求1所述的免辐照耐高温PVC材料，其特征在于，所述改性助剂为NR188。
  9. 一种用于制备根据权利要求1-8中任一项所述的免辐照耐高温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、改性水滑石、热稳定剂、增塑剂、加工软化助剂、改性助剂、抗氧剂、阻燃剂、紫外线吸收剂；
    将上述所有物质加入高速螺杆捏和机内进行调整捏和，待达到第一预定 温度时排料至冷混机进行冷却；
    当混合料在冷混机中温度下降到第二预定温度时，将原料放入挤出喂料机挤出喂料；
    将喂料输送至双螺杆挤出机，经双螺杆挤出机造粒后，进行水冷热切。
  10. 根据权利要求9所述的方法，其特征在于，所述第一预定温度为110℃-130℃，所述第二预定温度为40℃-60℃，双螺杆挤出机中各区的温度控制如下，进料区为173℃-185℃，塑化区为175℃-185℃，机头温度为180℃-190℃，水冷的温度为10℃-30℃。
PCT/CN2020/098919 2019-07-19 2020-06-29 一种免辐照耐高温pvc材料 WO2021012897A1 (zh)

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