CN105885295A - 一种高温凝胶的pvc溶胶及其制备方法 - Google Patents

一种高温凝胶的pvc溶胶及其制备方法 Download PDF

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CN105885295A
CN105885295A CN201610437728.XA CN201610437728A CN105885295A CN 105885295 A CN105885295 A CN 105885295A CN 201610437728 A CN201610437728 A CN 201610437728A CN 105885295 A CN105885295 A CN 105885295A
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pvc
colloidal sol
high temperature
plasticizer
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CN105885295B (zh
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吉玉碧
谭红
杨照
徐国敏
罗恒
石敏
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Beijing University of Chemical Technology
Guizhou Material Industrial Technology Research Institute
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Guizhou Material Industrial Technology Research Institute
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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
    • 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
    • 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
    • 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
    • C08J2327/02—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 not modified by chemical after-treatment
    • C08J2327/04—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 not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06—Homopolymers or copolymers of vinyl chloride
    • 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
    • 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
    • C08J2483/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/14—Applications used for foams

Abstract

本申请涉及一种高温凝胶的PVC溶胶及其制备方法，由按照重量份计算的以下成分构成：PVC糊树脂100份；增塑剂己二酸二异壬酯(DINA)65份；滑石粉5份；液态钙‑锌稳定剂3份；助剂5份，具有凝胶温度高且凝胶时间长的优点。

Description

一种高温凝胶的PVC溶胶及其制备方法
技术领域
本发明涉及一种PVC溶胶及其制备方法，特别是涉及一种凝胶温度高的PVC溶胶及其制备方法。
背景技术
聚氯乙烯(PVC)溶胶是将PVC糊树脂和其他助剂，如填充剂、稳定剂和颜料等搅拌分散在液态增塑剂中所形成的溶胶体系。其在汽车、玩具、包装等各领域均有广泛应用。在应用过程中，均需要将PVC溶胶控制在一定的温度和时间工艺条件下进行加热塑化成型。当加热时，PVC溶胶的黏度先降低，后由缓慢上升到快速升高，并很快达到一个峰值。快速上升的过程通常称为凝胶过程，峰值对应的温度通常称为凝胶温度。在凝胶阶段，PVC粒子在增塑剂中溶胀并且相互影响，产生了一个几乎没有机械强度的凝胶结构。PVC胶体的凝胶温度对产品生产工艺条件的选择和最终产品的质量都有着重要的影响。如：在旋转成型工艺中，为使产品壁厚均匀，要求胶体有较高的凝胶温度；又如：在有机械输送溶胶的生产工艺过程中，由于机械摩擦会产生热量传递，也要求溶胶具有较高的凝胶温度以避免堵胶、塞胶。此外，还要求溶胶具有较长的凝胶时间来保证产品连续稳定的生产。PVC溶胶制备过程中所用的各种原料助剂均会对其凝胶温度和凝胶时间产生影响。
发明内容
本发明的目的在于提供一种凝胶温度高的PVC溶胶及其制备方法，并且具有凝胶时间长的优点，能满足产品生产工艺和最终产品质量的要求。
为了解决上述技术问题，本发明采用如下的技术方案：
一种高温凝胶的PVC溶胶，由按照重量份计算的以下成分构成：
PVC糊树脂100份；增塑剂己二酸二异壬酯(DINA)65份；滑石粉5份；液态钙-锌稳定剂3份；助剂5份。
进一步地，所述助剂为发泡剂、颜料、硅油和/或润滑剂。
进一步地，在所述助剂中，包括发泡剂2份；钛白粉0.8份；硅油0.8份以及润滑剂1.4份。
进一步地，所述PVC糊树脂的聚合度为1900。
所述的高温凝胶的PVC溶胶制备方法，按上述配置比例称好各原料，在200～240r/min转速下将发泡剂、液态钙-锌稳定剂、钛白粉、滑石粉依次加入到装有80％增塑剂的杯中，加料完成后调整转速至1000～1200r/min，分散5～10min；分散均匀后调整转速至200～240r/min，加入PVC糊树脂和剩余的20％增塑剂，直至树脂完全浸润；再次调整转速至1000～1200r/min，分散5～10min；调整转速至200～240r/min，加入硅油，再调整转速为1000～1200r/min，继续分散3～5min后，过滤，制得所述温凝胶的PVC溶胶。
本申请的PVC溶胶具有凝胶温度高且凝胶时间长的优点。
具体实施方式
一、原料及配比(按重量计)
PVC糊树脂(100份)：树脂1，聚合度为1250；树脂2，聚合度为1900；树脂3，聚合度为800；树脂4，聚合度为1000；树脂5，聚合度为1700；树脂6，聚合度为1900。增塑剂(65份)：增塑剂1，对苯二甲酸二辛酯(DOTP)；增塑剂2，乙酰柠檬酸三正丁酯(ATBC)；增塑剂3，环己烷二羧酸二异壬基酯(DINCH)；增塑剂4，己二酸二异壬酯(DINA)；增塑剂5，邻苯二甲酸二辛酯(DOP)。填料(5份)：填料1是滑石粉；填料2是蒙托土；填料3是二氧化硅。稳定剂(3份)：稳定剂1是钙-锌稳定剂；稳定剂2是液态钙-锌稳定剂；稳定剂3是有机锡稳定剂。其余助剂(5份)：发泡剂、颜料、硅油和/或润滑剂。
二、制备方法
按配置比例称好各原料，在200～240r/min转速下将发泡剂、稳定剂、钛白粉、填料依次加入到装有80％增塑剂的杯中。加料完成后调整转速至1000～1200r/min，分散5～10min。分散均匀后调整转速至200～240r/min，加入PVC糊树脂和剩余的20％增塑剂，直至树脂完全浸润。再次调整转速至1000～1200r/min，分散5～10min。调整转速至200～240r/min，加入硅油等助剂。再调整转速为1000～1200r/min，继续分散3～5min后，过滤，制得光滑均匀的PVC溶胶。
凝胶温度和凝胶时间的测试
将配置好PVC溶胶置于25℃的水浴锅中平衡1h，然后取50g溶胶于正弦波振动黏度计(SV-10，日本A&D公司)的标准杯中，置于预先加热到100℃的油浴锅中进行测试，测试温度为25—100℃。定义达到仪器最大黏度值时所对应的温度和时间为样品的凝胶温度和凝胶时间。
三、原料助剂的影响
由上表可知，除了糊树脂和增塑剂两种主料外，对凝胶温度和时间影响较大的还有稳定剂和填料。后续配方中主要考虑了糊树脂类型、增塑剂类型、填料类型和稳定剂类型来做配方优化。
四、糊树脂种类的影响
由上表可知，树脂2制备的溶胶凝胶温度最高，凝胶时间也最长；树脂4制备的次之。后续配方中选用树脂2和树脂4做优化配方。
五、增塑剂种类的影响
由上表可知，当选用增塑剂4时，凝胶温度最高且凝胶时间最长；选用增塑剂3的次之。后续配方中选用增塑剂3和增塑剂4做优化配方。
六、填料种类的影响
由上表可知，当选用填料1时，凝胶温度最高且凝胶时间最长。后续配方中选用填料1做优化配方。
七、稳定剂种类的影响
由上表可知，当选用稳定剂2时，凝胶温度最高且凝胶时间最长。后续配方中选用稳定剂2做优化配方。
八、优化配方
由上分析及实验结果可知，采用优化配方2的配比可获得，凝胶温度最高且凝胶时间最长的PVC溶胶。

Claims (5)

1.一种高温凝胶的PVC溶胶，其特征在于，由按照重量份计算的以下成分构成：
PVC糊树脂100份；增塑剂己二酸二异壬酯(DINA)65份；滑石粉5份；液态钙-锌稳定剂3份；助剂5份。
2.根据权利要求1所述的高温凝胶的PVC溶胶，其特征在于，所述助剂为发泡剂、颜料、硅油和/或润滑剂。
3.根据权利要求1或2所述的高温凝胶的PVC溶胶，其特征在于，在所述助剂中，包括发泡剂2份；钛白粉0.8份；硅油0.8份以及润滑剂1.4份。
4.根据权利要求3所述的高温凝胶的PVC溶胶，其特征在于，PVC糊树脂的聚合度为1900。
5.一种根据权利要求3或4所述的高温凝胶的PVC溶胶制备方法，其特征在于，按上述配置比例称好各原料，在200～240r/min转速下将发泡剂、液态钙-锌稳定剂、钛白粉、滑石粉依次加入到装有80％增塑剂的杯中，加料完成后调整转速至1000～1200r/min，分散5～10min；分散均匀后调整转速至200～240r/min，加入PVC糊树脂和剩余的20％增塑剂，直至树脂完全浸润；再次调整转速至1000～1200r/min，分散5～10min；调整转速至200～240r/min，加入硅油和润滑剂，再调整转速为1000～1200r/min，继续分散3～5min后，过滤，制得所述温凝胶的PVC溶胶。
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