CN103087486B - 一种共混纳米复合材料及其制备方法 - Google Patents

一种共混纳米复合材料及其制备方法 Download PDF

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CN103087486B
CN103087486B CN201310033209.3A CN201310033209A CN103087486B CN 103087486 B CN103087486 B CN 103087486B CN 201310033209 A CN201310033209 A CN 201310033209A CN 103087486 B CN103087486 B CN 103087486B
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composite material
nano composite
polyhedral oligomeric
preparation
lactic acid
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CN103087486A (zh
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王保民
刘丰田
万向毅
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Jinan Saichen Polymer Material Co ltd
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SHANDONG PLASTIC RESEARCH DEVELOPMENT CENTER
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885—Screw or gear
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Biological Depolymerization Polymers (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

本发明属于塑料生产技术领域，特别公开了一种共混纳米复合材料及其制备方法。该共混纳米复合材料，以聚乳酸和聚乙烯醇为原料，其特征在于：在聚乳酸和聚乙烯醇中添加多面体齐聚硅倍半氧烷和热塑性弹性体，将上述物料混合分散，经过熔融共混、挤出、冷却造粒制得。本发明操作简单，生产成本低，产品质量好，有效地增强了纳米材料与PLA/PVA基体间的界面作用，提高了复合材料的力学性能，增强了多面体齐聚硅倍半氧烷的成核性，提高了复合材料的结晶温度。

Description

一种共混纳米复合材料及其制备方法
（一）        技术领域
    本发明属于塑料生产技术领域，特别涉及一种共混纳米复合材料及其制备方法。
（二）        背景技术
随着经济的发展，本来已比较短缺的能源更趋紧张，日趋减少的不可再生资源更显贫乏，脆弱的环境问题日加严峻，因此从可持续发展的视角，节约能源和资源的替代已成为形势所迫，是一股不可抗拒的潮流，在这样的历史背景下，生物降解塑料的研发和加快实用化、产业化进程已成为全球瞩目的热点。
聚乳酸（PLA）和聚乙烯醇（PVA）是两种极其重要的可降解材料，具有良好的生物兼容性和生物降解性。但PLA材料具有亲水性差，细胞吸附力较弱，性脆，降解速度难以控制，价格高等缺点。多面体齐聚硅倍半氧烷（POSS）作为一种新型的有机-无机纳米杂化材料，可通过其顶角的活性官能团（如乙烯基、环氧基、氨基、羧基等）经开环聚合、活性自由基聚合、无规共聚等反应引入到聚合物中，并通过调整顶角有机基团类型与活性基团类型和活性大小可以控制聚合物体系的立体化学结构，以提高聚合物的使用温度、分解温度、韧性和力学性能等。热塑性弹性体（TPE）是一种常用的共混改性增韧材料。为了克服PLA材料疏水性及脆性，采用价格低廉的PVA材料与其共混改性，使材料达到一个所需的综合性能，消除单一组分的性能弱点，并可大大降低材料成本，将产生客观的经济效益。
（三）        发明内容
    本发明为了弥补现有技术的不足，提供了一种生产成本低、产品质量好的共混纳米复合材料及其制备方法。
本发明是通过如下技术方案实现的：
一种共混纳米复合材料，以聚乳酸和聚乙烯醇为原料，其特征在于：在聚乳酸和聚乙烯醇中添加多面体齐聚硅倍半氧烷和热塑性弹性体，将上述物料混合分散，经过熔融共混、挤出、冷却造粒制得。
本发明的更优方案为：
所述聚乳酸、聚乙烯醇、多面体齐聚硅倍半氧烷和热塑性弹性体的重量配比为20%:60%:7%:13%，其中，热塑性弹性体中含有占物料总重量3%的增容剂TPE-g-MAH。
本发明所述的共混纳米复合材料的制备方法，包括如下步骤：
（1）在180~190℃下，将多面体齐聚硅倍半氧烷置于高速混合机中预分散；
（2）将高速混合机温度冷却至80~90℃后，加入聚乳酸、聚乙烯醇和热塑性弹性体的混合物，将上述物料混合；
（3）将混合后的物料加入双螺杆挤出机挤出造粒得到产品，螺杆各区温度为160~200℃，螺杆转速为20~80rpm。
其中，步骤（1）中，多面体齐聚硅倍半氧烷的预分散时间为10min；步骤（2）中，物料混合时间为10min。
本发明将热塑性弹性体和多面体齐聚倍半硅氧烷为填充改性剂，通过分散预处理，提高了多面体齐聚倍半硅氧烷的分散性和PLA/PVA复合材料的热稳定性及耐水性，改善了螺杆挤出的加工性能，并在PLA/PVA中产生新晶相，提高了制品的质量。
本发明操作简单，生产成本低，产品质量好，有效地增强了纳米材料与PLA/PVA基体间的界面作用，提高了复合材料的力学性能，增强了多面体齐聚硅倍半氧烷的成核性，提高了复合材料的结晶温度。
（四）        具体实施方式
实施例：
主要包括如下步骤：
（1）采用高速混合机，在180至190摄氏度温度下，对聚乳酸、聚乙烯醇、多面体齐聚硅倍半氧烷和热塑性弹性体四元体系中重量份占7%的多面体齐聚硅倍半氧烷预分散10分钟。
（2）将高速混合机温度冷却至80至90摄氏度，加入重量份为20%的聚乳酸，重量份60%的聚乙烯醇，重量份为13%热塑性弹性体混合物（其中含有重量份为3%的热塑性弹性体增容剂TPE-g-MAH），混合10分钟。
（3）将混合后的物料加入双螺杆挤出机挤出造粒，螺杆各区温度在160到200摄氏度，螺杆转速20~80rpm。
本发明的先进性表现在采用聚乳酸、聚乙烯醇、多面体齐聚硅倍半氧烷和热塑性弹性体四元纳米复合材料，克服了普通生物降解产品在耐高温、耐湿的情况下，干、湿强度不高的缺点，使用热塑性弹性体起到复合材料的增韧作用。
另外产品使用增容剂TPE-g-MAH，能有效地增强纳米材料与PLA/PVA基体间的界面作用，提高复合材料的力学性能，增强了多面体齐聚硅倍半氧烷的成核性，提高复合材料的结晶温度。

Claims (4)

1.一种共混纳米复合材料，以聚乳酸和聚乙烯醇为原料，其特征在于：在聚乳酸和聚乙烯醇中添加多面体齐聚硅倍半氧烷和热塑性弹性体，将上述物料混合分散，经过熔融共混、挤出、冷却造粒制得；所述聚乳酸、聚乙烯醇、多面体齐聚硅倍半氧烷和热塑性弹性体的重量配比为20%:60%:7%:13%，其中，热塑性弹性体中含有占物料总重量3%的增容剂TPE-g-MAH。
2.根据权利要求1所述的共混纳米复合材料的制备方法，其特征为，包括如下步骤：（1）在180~190℃下，将多面体齐聚硅倍半氧烷置于高速混合机中预分散；（2）将高速混合机温度冷却至80~90℃后，加入聚乳酸、聚乙烯醇和热塑性弹性体的混合物，将上述物料混合；（3）将混合后的物料加入双螺杆挤出机挤出造粒得到产品，螺杆各区温度为160~200℃，螺杆转速为20~80rpm。
3.根据权利要求2所述的共混纳米复合材料的制备方法，其特征在于：步骤（1）中，多面体齐聚硅倍半氧烷的预分散时间为10min。
4.根据权利要求2所述的共混纳米复合材料的制备方法，其特征在于：步骤（2）中，物料混合时间为10min。
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Patentee before: SHANDONG PLASTIC RESEARCH DEVELOPMENT CENTER