CN104448197B - 耐热性聚氨酯弹性体的合成方法 - Google Patents

耐热性聚氨酯弹性体的合成方法 Download PDF

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CN104448197B
CN104448197B CN201410781513.0A CN201410781513A CN104448197B CN 104448197 B CN104448197 B CN 104448197B CN 201410781513 A CN201410781513 A CN 201410781513A CN 104448197 B CN104448197 B CN 104448197B
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刘兆阳
陈由亮
宿金明
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Shandong Inov Polyurethane Co Ltd
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Abstract

本发明涉及一种耐热性聚氨酯弹性体的合成方法，由聚酯多元醇、二异氰酸酯和扩链剂反应制得，所述的聚酯多元醇由己二酸和多元醇反应生成，所述的多元醇为乙二醇、丁二醇、三羟甲基丙烷、丙二醇、一缩二乙二醇中的两种或者两种以上的混合物。本发明所制得的耐热性聚氨酯弹性体，制品力学性能优良，在较高的温度下，性能保持率较高，永久压缩形变较小的聚氨酯弹性体制品，适用于环境温度较高的场所。

Description

耐热性聚氨酯弹性体的合成方法
技术领域
本发明属于聚氨酯弹性体领域，特别涉及一种耐热性聚氨酯弹性体的合成方法。
背景技术
聚氨酯是一种性能介于橡胶与塑料之间的高分子合成材料，其特点是硬度调整范围宽，既有橡胶的弹性又有塑料的硬度，但是普通的聚氨酯材料，高温下易加速聚氨酯的老化，性能明显降低。
发明内容
本发明的目的是提供一种耐热性聚氨酯弹性体的合成方法，得到的弹性体力学性能优良，在较高的温度下，性能保持率较高，永久压缩形变较小的聚氨酯弹性体制品，适用于环境温度较高的场所。
一种耐热性聚氨酯弹性体的合成方法，由聚酯多元醇、二异氰酸酯和扩链剂反应制得，所述的聚酯多元醇由己二酸和多元醇反应生成，所述的多元醇为乙二醇、丁二醇、三羟甲基丙烷、丙二醇、一缩二乙二醇中的两种或者两种以上的混合物。
所述多元醇为乙二醇、丁二醇、三羟甲基丙烷中的两种或者两种以上。
扩链剂为MOCA或丁二醇。
聚酯多元醇的制备步骤为：将己二酸、多元醇和催化剂钛酸四丁酯加入反应釜中加热，并通氮气保护，当温度升至140℃时反应，控制回流塔塔顶温度在100-102℃，然后将釜温缓慢升至160-180℃，保温2-3小时，再将温度升至220-230℃，当反应完毕后，保温2-3小时，然后采用氮气鼓泡工艺把缩聚产生的水分脱出，当釜内物料的酸值小于0.4mgKOH/g，水分含量在0.05％以下时，即产品合格，开始降温放料，得到分子量在1000-2000的聚酯多元醇。
根据权利要求1或4所述的一种耐热性聚氨酯弹性体的合成方法，其特征在于，己二酸和多元醇的摩尔比为1.15-1.21：1。
催化剂钛酸四丁酯50-100ppm。
耐热性聚氨酯弹性体的合成方法，将聚酯多元醇69.1-85.1wt％和二异氰酸酯14.9-30.9wt％混合均匀，在75-85℃条件下反应2-3小时，真空脱除气泡，得到-NCO含量在3.6％-7.5％的聚氨酯预聚体，按100:7.6-12.5的比例混合均匀，反应得到耐热性聚氨酯弹性体。
所述的二异氰酸酯为TDI-80、TDI-100、MDI-100的一种或者一种以上。
TDI‐80：含有80％的2,4‐甲苯二异氰酸酯和20％的2,6‐甲苯二异氰酸酯；TDI‐100：2,4‐甲苯二异氰酸酯含量大于97.5％；MDI‐100：4，4’‐二苯基甲烷二异氰酸酯。TDI‐80的生产厂家为上海巴斯夫有限公司。TDI‐100生产厂家为三井化学公司。MDI‐100为烟台万华聚氨酯股份有限公司。
MOCA：3，3′‐二氯‐4,4′‐二氨基二苯基甲烷。MOCA的生产厂家为苏州湘园特种精细化工有限公司。
本发明中所用产品均为市售产品。
与现有技术相比，本发明具有以下有益效果：
本发明所制得的耐热性聚氨酯弹性体，制品力学性能优良，在较高的温度下，性能保持率较高，永久压缩形变较小的聚氨酯弹性体制品，适用于环境温度较高的场所。
具体实施方式
下面结合实施例对本发明做进一步的说明。
以下实施例的百分数为质量百分数。
实施例1
聚酯多元醇的合成：己二酸：66.2wt％、乙二醇：32.4wt％、三羟甲基丙烷：1.4wt％，外加催化剂钛酸四丁酯50ppm合成分子量为1500聚酯多元醇A。
具体步骤为：将己二酸、乙二醇、三羟甲基丙烷和钛酸四丁酯，加入反应釜中加热，并通氮气保护，当温度升至140℃时反应出水，控制回流塔塔顶温度在100～102℃，然后将釜温缓慢升至160～180℃，保温2～3小时，再将温度升至220～230℃，当出水完毕后，保温2-3小时，然后采用氮气鼓泡工艺把缩聚产生的水分脱出，当釜内物料的酸值小于0.4mgKOH/g，水分含量在0.05％以下时，即产品合格，开始降温放料，得到分子量在1500的聚酯多元醇A。
耐热性聚氨酯弹性体合成：按照重量百分数计，取聚酯多元醇A：81.6％，TDI‐100：18.4％,在80℃反应3小时，真空脱除气泡，取样检测异氰酸酯含量，检测‐NCO含量在4.3％，得到聚氨酯预聚体，聚氨酯预聚体和MOCA按100:12.5比例，采用常规做法制得硬度在邵氏90A的聚氨酯弹性体产品。
实施例2
按照实施例1的制备方法。
聚酯多元醇合成：己二酸：58wt％、丁二醇：40.5wt％、三羟甲基丙烷：1.5wt％，外加催化剂钛酸四丁酯50ppm合成分子量为2000的聚酯多元醇B。
耐热性聚氨酯弹性体合成：按照重量百分数计，取聚酯多元醇B：85.1％，TDI‐80：14.9％,在80℃反应3小时，真空脱除气泡，取样检测异氰酸酯含量，检测‐NCO含量在3.6％，得到聚氨酯预聚体，聚氨酯预聚体和MOCA按100:10.3比例，采用常规做法制得硬度在邵氏85A的聚氨酯弹性体产品。
实施例3
聚酯多元醇采用实施例2的制备方法制得聚酯多元醇B。
耐热性聚氨酯弹性体合成：按照重量百分数计，取聚酯多元醇B：69.1％，MDI‐100：30.9％,在80℃反应3小时，真空脱除气泡，取样检测异氰酸酯含量，检测‐NCO含量在7.5％，得到聚氨酯预聚体，聚氨酯预聚体和丁二醇按100:7.6比例，采用常规做法制得硬度在邵氏90A的聚氨酯弹性体产品。
对比例1
己二酸合成的聚酯多元醇ODX‐150(烟台华大科技有限公司生产)：81.6％，TDI‐100：18.4％,在80℃反应3小时，真空脱除气泡，取样检测异氰酸酯含量，检测‐NCO含量在4.3％，得到聚氨酯预聚体。氨酯预聚体和MOCA按100:12.5比例，采用常规做法制作出硬度在邵氏90A的聚氨酯弹性体产品。
其中，ODX‐150：数均分子量1500的聚酯二元醇。
实施例1‐3和对比例1的性能数据如表1。
表1实施例1‐3和对比例1的性能数据表

Claims (1)

1.一种耐热性聚氨酯弹性体的合成方法，其特征在于，聚酯多元醇的合成：己二酸：66.2wt%、乙二醇：32.4 wt%、三羟甲基丙烷：1.4 wt%，外加催化剂钛酸四丁酯50ppm合成分子量为1500聚酯多元醇A；
具体步骤为：将己二酸、乙二醇、三羟甲基丙烷和钛酸四丁酯，加入反应釜中加热，并通氮气保护，当温度升至140℃时反应出水，控制回流塔塔顶温度在100～102℃，然后将釜温缓慢升至160～180℃，保温2～3小时，再将温度升至220～230℃，当出水完毕后，保温2-3小时，然后采用氮气鼓泡工艺把缩聚产生的水分脱出，当釜内物料的酸值小于0.4mgKOH/g，水分含量在0.05％以下时，即产品合格，开始降温放料，得到分子量在1500的聚酯多元醇A；
耐热性聚氨酯弹性体合成：按照重量百分数计，取聚酯多元醇A：81.6%，TDI-100：18.4%, 在80℃反应3小时，真空脱除气泡，取样检测异氰酸酯含量，检测-NCO含量在4.3%，得到聚氨酯预聚体，聚氨酯预聚体和MOCA按100:12.5比例，采用常规做法制得硬度在邵氏90A的聚氨酯弹性体产品。
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