WO2015101242A1 - 一种高填充高回弹软质发泡聚乙烯材料及其制备方法 - Google Patents

一种高填充高回弹软质发泡聚乙烯材料及其制备方法 Download PDF

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WO2015101242A1
WO2015101242A1 PCT/CN2014/095237 CN2014095237W WO2015101242A1 WO 2015101242 A1 WO2015101242 A1 WO 2015101242A1 CN 2014095237 W CN2014095237 W CN 2014095237W WO 2015101242 A1 WO2015101242 A1 WO 2015101242A1
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parts
calcium carbonate
foaming agent
polyethylene material
polyethylene
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PCT/CN2014/095237
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English (en)
French (fr)
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曾聪
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广州石头造环保科技有限公司
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Application filed by 广州石头造环保科技有限公司 filed Critical 广州石头造环保科技有限公司
Priority to US14/770,825 priority Critical patent/US9828480B2/en
Priority to AU2014375530A priority patent/AU2014375530A1/en
Priority to JP2016504485A priority patent/JP6403752B2/ja
Priority to EP14876228.9A priority patent/EP2957594B1/en
Publication of WO2015101242A1 publication Critical patent/WO2015101242A1/zh

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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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    • 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
    • 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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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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    • 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
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    • 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
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    • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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    • C08J2201/00—Foams characterised by the foaming process
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    • C08J2203/18—Binary blends of expanding agents
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    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—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
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Definitions

  • the invention relates to a polyethylene material, in particular to a high-filling, high-rebound soft foamed polyethylene material and a preparation method thereof.
  • Foamed polyethylene material has smooth surface, excellent impact absorption, excellent cushioning shock absorption and resilience, high tensile strength, excellent chemical stability, good environmental aging resistance and weather resistance, insulation and heat insulation.
  • the low price is the most widely used foaming material.
  • polyethylene foaming materials still have insufficient bending strength, poor compressive strength and heat resistance, and low rigidity and hardness, which limits their application.
  • people often add inorganic fillers in the material molding process on the one hand can improve the rigidity, hardness and other mechanical properties of foamed polyethylene materials, on the other hand, can reduce the cost of materials, but the actual product performance is still not ideal.
  • One of the objects of the present invention is to provide a high-fill, high-rebound soft foamed polyethylene material which can improve rigidity, hardness and compressive strength and has low cost, and a preparation method thereof.
  • Another object of the present invention is to provide a process for preparing a highly filled, high resilience soft foamed polyethylene material.
  • a high-filled high-rebound soft foamed polyethylene material including the following parts by weight:
  • the polyethylene (PE) may be at least one of low density polyethylene (LDPE), high density polyethylene (HDPE), and linear low density polyethylene (LLDPE).
  • LDPE low density polyethylene
  • HDPE high density polyethylene
  • LLDPE linear low density polyethylene
  • the elastomer is at least one of POE, EVA, SEBS, SBS, EPDM, and EPR.
  • the modified calcium carbonate is a coupling agent modified calcium carbonate.
  • the preparation method of the coupling agent modified calcium carbonate includes the following steps:
  • the coupling agent may be one or more mixtures of a titanate coupling agent, a silane coupling agent, and an aluminum zirconate coupling agent.
  • the modified calcium carbonate has a mesh number of ⁇ 500 mesh.
  • the chemical foaming agent is composed of azodicarbonamide, zinc oxide and zinc stearate in a mass ratio of 1: (1-1.5): (0.15-2).
  • the crosslinking agent includes dicumyl peroxide or 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane.
  • the physical foaming agent is an expandable microsphere foaming agent, and is a novel special foaming agent produced by Matsumoto Corporation of Japan.
  • the expandable microsphere foaming agent is a milky white micro spherical plastic particle with a diameter of 10- 30 microns. When heated at a certain temperature, the thermoplastic shell softens, the gas inside the casing expands, the volume of the foaming agent can be increased to several tens of times, and the core-shell structure is not destroyed, thereby achieving the foaming effect.
  • a preparation method of a high-filling high-rebound soft foamed polyethylene material comprising the following steps:
  • the kneaded material in the mold place the mold in the flat vulcanizing machine, and heat-expand it for 5 to 15 minutes at 160-180 ° C, 5 to 15 MPa, remove the mold, and lightly press and shape.
  • the foamed polyethylene material can be obtained; or the kneaded material is placed in a mold, and the mold is placed in a flat vulcanizing machine, and foamed at 145-165 ° C, 5-15 MPa for 3 to 10 minutes, and cooled to After demolding at room temperature, the foamed material after demolding is secondarily foamed at 170 to 180 ° C for 5 to 10 minutes to obtain a foamed polyethylene material.
  • the invention has the beneficial effects that a high-filled calcium carbonate high-rebound soft foamed polyethylene material with a calcium carbonate filling amount of 55 to 75% can be prepared, and the elasticity of the foamed material is maintained. Improve the rigidity, hardness and compressive strength of the material while reducing the material density.
  • the invention has simple production process, can greatly reduce cost, and is economical and practical.
  • a high-filled, high-rebound soft foamed polyethylene material comprising the following parts by weight:
  • a high-filled, high-rebound soft foamed polyethylene material comprising the following parts by weight:
  • a high-filled, high-rebound soft foamed polyethylene material comprising the following parts by weight:
  • the polyethylene (PE) may be at least one of low density polyethylene (LDPE), high density polyethylene (HDPE), linear low density polyethylene (LLDPE) or low density polyethylene (LDPE),
  • LDPE low density polyethylene
  • the mass ratio of high density polyethylene (HDPE) and linear low density polyethylene (LLDPE) is 1: (0-1.0): (0.5-2).
  • the elastomer is one of POE, EVA, SEBS, and EPDM.
  • the modified calcium carbonate is a coupling agent modified calcium carbonate, and the modified calcium carbonate has a mesh number of ⁇ 500 mesh.
  • the chemical foaming agent is composed of azodicarbonamide, zinc oxide and zinc stearate in a mass ratio of 1: (1-1.5): (0.15-2).
  • the chemical foaming agent is azodicarbonamide, zinc oxide and zinc stearate according to a mass ratio of 1: 1.3: 1.5 mixed composition, this ratio can make the mixture foam rapidly and stable at 160-180 °C.
  • the crosslinking agent includes dicumyl peroxide or 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane.
  • the physical foaming agent is an expandable microsphere foaming agent, preferably, an expandable microsphere foaming agent of the type MSH-500 produced by Matsumoto Corporation of Japan, and the expandable microsphere foaming agent is a milky white microsphere.
  • Plastic pellets 10-30 microns in diameter. When heated at a certain temperature, the thermoplastic shell softens, the gas inside the casing expands, the volume of the foaming agent can be increased to several tens of times of itself, and the core-shell structure is not destroyed, thereby achieving the foaming effect.
  • the preparation method of the above high-filled high-rebound soft foamed polyethylene material comprises the following steps:
  • the kneaded material in the mold place the mold in the flat vulcanizing machine, and heat-expand it for 5 to 15 minutes at 160-180 ° C, 5 to 15 MPa, remove the mold, and lightly press and shape.
  • the foamed polyethylene material can be obtained; or the kneaded material is placed in a mold, and the mold is placed in a flat vulcanizing machine, and foamed at 145-165 ° C, 5-15 MPa for 3 to 10 minutes, and cooled to After demolding at room temperature, the foamed material after demolding is secondarily foamed at 170 to 180 ° C for 5 to 10 minutes to obtain a foamed polyethylene material.
  • the method for preparing the above high-filled high-rebound soft foamed polyethylene material comprises the following steps:
  • the kneaded material is placed in a mold, and then the mold is placed in a flat vulcanizing machine, and reacted at 165 ° C, 10 MPa for 10 minutes, the material is taken out by mold opening, and the target foaming material is obtained by light pressure cooling.

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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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

本发明公开一种高填充高回弹软质发泡聚乙烯材料，包括以下重量份的原料：聚乙烯15-20份、弹性体5-20份、改性碳酸钙60-80份、化学发泡剂1-10份、交联剂0.5-1.5份和物理发泡剂1-5份。本发明还公开一种高填充高回弹软质发泡聚乙烯材料的制备方法。本发明的有益效果是：本发明可以制备碳酸钙填充量高达55～75%的高填充碳酸钙高回弹软质发泡聚乙烯材料，在保持发泡材料弹性的基础上，提高该材料的刚性、硬度和压缩强度，同时降低材料密度。本发明生产工艺简单，可极大降低成本，经济实用。

Description

一种高填充高回弹软质发泡聚乙烯材料及其制备方法 技术领域
本发明涉及一种聚乙烯材料，尤其是一种高填充高回弹软质发泡聚乙烯材料及其制备方法。
背景技术
发泡聚乙烯材料表面光滑，冲击吸收性优良，缓冲减震性和回弹性优异，拉伸强度高，有优良的化学稳定性、良好的耐环境老化性和耐候性，绝缘，隔热，而且价格低廉，是目前应用最多的发泡材料。但是目前聚乙烯发泡材料仍存在弯曲强度、压缩强度和耐热性差，刚性和硬度低等不足，限制了它的应用。为此，人们常在材料成型加工过程中加入无机填料，一方面可提高发泡聚乙烯材料的刚性、硬度和其他力学性能，另一方面又能降低材料的成本，但是实际得到产品性能还是不理想。
发明内容
本发明的目的之一针对以上所述现有技术存在的不足，提供一种可提高刚性、硬度和压缩强度，且成本低的高填充高回弹软质发泡聚乙烯材料及其制备方法。
本发明的另一目的是提供一种高填充高回弹软质发泡聚乙烯材料的制备方法。
为达到上述目的，本发明采用了如下的技术方案：一种高填充高回弹软质发泡聚乙烯材料，包括下重量份数的原料：
聚乙烯 15-20份、弹性体5-20份、改性碳酸钙60-80份、化学发泡剂1-10份、交联剂0.5-1.5份和物理发泡剂1-5份。
所述聚乙烯（PE）可以为低密度聚乙烯（LDPE）、高密度聚乙烯（HDPE）、线型低密度聚乙烯（LLDPE）中的至少一种。
所述弹性体为POE、EVA、SEBS、SBS、EPDM、EPR中的至少一种。
所述改性碳酸钙为偶联剂改性碳酸钙。
所述偶联剂改性碳酸钙的制备方法包括的步骤如下：
（1）将目数大于≥500目的碳酸钙粉干燥至水分质量比含量≤0.1%；
（2）将第（1）步中所制备的碳酸钙粉与偶联剂按质量比100：0.5～3加入到高速搅拌混合机中，混合5～20分钟。
所述偶联剂可以为钛酸酯偶联剂、硅烷偶联剂和铝锆酸酯偶联剂的一种或多种混合物。
所述改性碳酸钙的目数≥500目。
所述化学发泡剂为偶氮二甲酰胺、氧化锌、硬脂酸锌按照质量比1:（1-1.5）:（0.15-2）混合组成。
所述交联剂包括过氧化二异丙苯或者2,5-二甲基-2,5-二（叔丁过氧基）己烷。
所述物理发泡剂为可膨胀微球发泡剂，是日本松本公司生产的一种新型的特种发泡剂，可膨胀微球发泡剂是一种乳白色的微小球状塑料颗粒，直径10-30微米。当加热的一定温度时，热塑性壳体软化，壳体里面的气体膨胀，发泡剂的体积可以增大到自身得几十倍，同时核壳结构并不破坏，从而达到发泡的效果。
一种高填充高回弹软质发泡聚乙烯材料的制备方法，包括以下步骤：
1）将改性碳酸钙干燥至水分质量比含量≤0.1%；
2）将聚乙烯与弹性体置于开炼机中进行塑炼，塑炼温度110～120℃，塑炼时间2～5分钟；
3）将改性碳酸钙、物理发泡剂、化学发泡剂、交联剂按顺序加入上步的体系进行混炼，混炼温度120～130℃，混炼时间10～15分钟；
4）将混炼后的物料放在模具中，将模具置于平板硫化机中，在160～180℃，5～15MPa条件下热压发泡5～15分钟，开模取出，轻压定型即可制得发泡聚乙烯材料；或将混炼后的物料放在模具中，将模具置于平板硫化机中，在145～165℃，5～15MPa条件下发泡3～10分钟，冷却至室温脱模，将脱模后的发泡物在170～180℃下二次发泡5～10分钟即可制得发泡聚乙烯材料。
与现有技术相比，本发明的有益效果是：可以制备碳酸钙填充量高达55～75%的高填充碳酸钙高回弹软质发泡聚乙烯材料，在保持发泡材料弹性的基础上，提高该材料的刚性、硬度和压缩强度,同时降低材料密度。本发明生产工艺简单，可极大降低成本，经济实用。
具体实施方式
以下结合具体实施例对本发明进行详细的说明。
实施例1
一种高填充高回弹软质发泡聚乙烯材料，包括以下重量份的原料：
聚乙烯 16份、弹性体6份、改性碳酸钙61份、化学发泡剂2份、交联剂0.6份和物理发泡剂2份。
实施例2
一种高填充高回弹软质发泡聚乙烯材料，包括以下重量份的原料：
聚乙烯 19份、弹性体19份、改性碳酸钙79份、化学发泡剂9份、交联剂1.4份和物理发泡剂4份。
实施例3
一种高填充高回弹软质发泡聚乙烯材料，包括以下重量份的原料：
聚乙烯 15份、弹性体13份、改性碳酸钙71份、化学发泡剂6份、交联剂1.1份和物理发泡剂3份。
其中，所述聚乙烯（PE）可以为低密度聚乙烯（LDPE）、高密度聚乙烯（HDPE）、线型低密度聚乙烯（LLDPE）中的至少一种或者低密度聚乙烯（LDPE）、高密度聚乙烯（HDPE）、线型低密度聚乙烯（LLDPE）的质量比为1：（0-1.0）：（0.5-2）。
所述弹性体为POE、EVA、SEBS、EPDM中的一种。
所述改性碳酸钙为偶联剂改性碳酸钙，所述改性碳酸钙的目数≥500目。
所述化学发泡剂为偶氮二甲酰胺、氧化锌、硬脂酸锌按照质量比1:（1-1.5）:（0.15-2）混合组成。优选的，所述化学发泡剂为偶氮二甲酰胺、氧化锌、硬脂酸锌按照质量比1: 1.3: 1.5混合组成，此配比可以使混合物在160-180℃下快速稳定发泡。所述交联剂包括过氧化二异丙苯或者2,5-二甲基-2,5-二（叔丁过氧基）己烷。所述物理发泡剂为可膨胀微球发泡剂，优选，日本松本公司生产的型号为MSH-500的可膨胀微球发泡剂，可膨胀微球发泡剂是一种乳白色的微小球状塑料颗粒，直径10-30微米。当加热的一定温度时，热塑性壳体软化，壳体里面的气体膨胀，发泡剂的体积可以增大到自身的几十倍，同时核壳结构并不破坏，从而达到发泡的效果。
上述高填充高回弹软质发泡聚乙烯材料的制备方法，包括以下步骤：
1）将改性碳酸钙干燥至水分质量比含量≤0.1%；
2）将聚乙烯与弹性体置于开炼机中进行塑炼，塑炼温度110～120℃，塑炼时间2～5分钟；
3）将改性碳酸钙、物理发泡剂、化学发泡剂、交联剂按顺序加入上步的体系进行混炼，混炼温度120～130℃，混炼时间10～15分钟；
4）将混炼后的物料放在模具中，将模具置于平板硫化机中，在160～180℃，5～15MPa条件下热压发泡5～15分钟，开模取出，轻压定型即可制得发泡聚乙烯材料；或将混炼后的物料放在模具中，将模具置于平板硫化机中，在145～165℃，5～15MPa条件下发泡3～10分钟，冷却至室温脱模，将脱模后的发泡物在170～180℃下二次发泡5～10分钟即可制得发泡聚乙烯材料。
优选的，上述高填充高回弹软质发泡聚乙烯材料的制备方法，包括以下步骤：
1）将改性碳酸钙干燥至水分质量比含量≤0.1%；
2）将聚乙烯与弹性体置于开炼机中进行塑炼，塑炼温度115-120℃，塑炼时间4分钟；
3）将改性碳酸钙、物理发泡剂、化学发泡剂、交联剂按顺序加入上步的体系进行混炼，混炼温度125℃，混炼时间13分钟；
4）将混炼后的物料放在模具中，将模具置于平板硫化机中，在170℃，10MPa条件下热压发泡10分钟，开模取出，轻压定型即可制得发泡聚乙烯材料；或将混炼后的物料放在模具中，将模具置于平板硫化机中，在155℃，10MPa条件下发泡7分钟，冷却至室温脱模，将脱模后的发泡物在175℃下二次发泡8分钟即可制得发泡聚乙烯材料。
实施例4
首先取50克低密度聚乙烯和50克POE混合均匀放入双辊开炼机115℃塑炼3分钟，再依次加入200克500目的钛酸酯改性碳酸钙（钛酸酯偶联剂型号：AT2-TMC-311w），5克物理发泡剂，6克偶氮二甲酰胺、4克氧化锌、1克硬脂酸锌、0.5克过氧化二异丙苯在130℃混炼15分钟。然后将混炼后的物料置于模具中，再将模具放入平板硫化机中，在165℃，10MPa下反应10分钟，开模将材料取出，轻压冷却即制得目标发泡材料。
以上详细描述了本发明的较佳具体实施例，应当理解，本领域的普通技术无需创造性劳动就可以根据本发明的构思做出诸多修改和变化。因此，凡本技术领域中技术人员依本发明构思在现有技术基础上通过逻辑分析、推理或者根据有限的实验可以得到的技术方案，均应该在由本权利要求书所确定的保护范围之中。

Claims (8)

  1. 一种高填充高回弹软质发泡聚乙烯材料，其特征在于，包括以下重量份的原料：
    聚乙烯 15-20份、弹性体5-20份、改性碳酸钙60-80份、化学发泡剂1-10份、交联剂0.5-1.5份和物理发泡剂1-5份。
  2. 按照权利要求1所述的一种高填充高回弹软质发泡聚乙烯材料，其特征在于，所述聚乙烯为低密度聚乙烯、高密度聚乙烯、线型低密度聚乙烯中的至少一种。
  3. 按照权利要求1所述的一种高填充高回弹软质发泡聚乙烯材料，其特征在于，所述弹性体为POE、EVA、SEBS、SBS、EPDM、EPR中的至少一种。
  4. 按照权利要求1所述的一种高填充高回弹软质发泡聚乙烯材料，其特征在于，所述改性碳酸钙为偶联剂改性碳酸钙，所述改性碳酸钙的目数≥500目。
  5. 按照权利要求1所述的一种高填充高回弹软质发泡聚乙烯材料，其特征在于，所述化学发泡剂为偶氮二甲酰胺、氧化锌、硬脂酸锌按照质量比1:（1-1.5）:（0.15-2）混合组成。
  6. 按照权利要求1所述的一种高填充高回弹软质发泡聚乙烯材料，其特征在于，所述交联剂包括过氧化二异丙苯或者2,5-二甲基-2,5-二（叔丁过氧基）己烷。
  7. 按照权利要求1所述的一种高填充高回弹软质发泡聚乙烯材料，其特征在于，所述物理发泡剂为可膨胀微球发泡剂。
  8. 按照权利要求1-7任一所述的一种高填充高回弹软质发泡聚乙烯材料的制备方法，其特征在于，包括以下步骤：
    1）将改性碳酸钙干燥至水分质量比含量≤0.1%；
    2）将聚乙烯与弹性体置于开炼机中进行塑炼，塑炼温度110～120℃，塑炼时间2～5分钟；
    3）将改性碳酸钙、物理发泡剂、化学发泡剂、交联剂按顺序加入上步的体系进行混炼，混炼温度120～130℃，混炼时间10～15分钟；
    4）将混炼后的物料放在模具中，将模具置于平板硫化机中，在160～180℃，5～15MPa条件下热压发泡5～15分钟，开模取出，轻压定型即可制得发泡聚乙烯材料；或将混炼后的物料放在模具中，将模具置于平板硫化机中，在145～165℃，5～15MPa条件下发泡3～10分钟，冷却至室温脱模，将脱模后的发泡物在170～180℃下二次发泡5～10分钟即可制得发泡聚乙烯材料。
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US20160009885A1 (en) 2016-01-14
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