CN104829811A - 一种水性聚氨酯树脂的制备工艺 - Google Patents
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Abstract
一种水性聚氨酯树脂的制备工艺，属于化工技术领域，包括预聚、回流、中和反应、分散乳化、扩链反应和成品包装等步骤。本发明水性聚氨酯树脂生产工艺过程简单，原料利用率高，产品转化率高达99％以上，未转化部分99％以上均回收利用，生产对环境和社会无负影响；制备工艺以无离子水为溶剂，采用节能设备，能耗减少，生产成本低；最终制备产品绿色环保，具有无毒、节能、成本低、安全、不污染环境等优点。
Description
技术领域：
本发明属于化工技术领域，涉及一种水性聚氨酯树脂的制备工艺。
技术背景：
传统的聚氨酯（英文名：Polyurethane Resin，缩写为PU），分子式C3H8N2O，它是指主链中含有氨基甲酸酯（酯(-NHCOO-)特征单元的一类高分子，通常由异氰酸酯（含有-NCO基团）与多元醇在溶剂和催化剂的作用下聚合而成，生产反应如下所示。
聚氨酯的力学性能具有很大的可调性，通过控制结晶的硬段和不结晶的软段之间的比例，聚氨酯可以获得不同的力学性能。因此其制品具有耐磨、耐温、密封、隔音、加工性能好、可降解等优点。聚氨酯还具有抗多种酸碱和有机溶剂腐蚀的性能，因此经常被用作橡胶制品在恶劣环境下的替代品。
传统聚氨酯制备方法：传统的聚氨酯为溶剂型聚氨酯，由多元醇、异氰酸酯、扩链剂聚合而成，由于分子中不含亲水基团，因此只能溶解于有机溶剂中。常用溶剂有DMF、甲苯、二甲苯、丙酮、丁酮、乙酸乙酯等，这些溶剂毒副作用大，不仅易造成环境污染，危害身体，而且易燃易爆，极易引发火灾等事故。
发明内容：
本发明针对现有技术存在的缺陷，提供一种水性聚氨酯树脂制备工艺。该生产工艺过程简单，原料利用率高，产品转化率高，未转化部分均回收利用，生产对环境和社会无负影响；制备工艺以去离子水为溶剂，采用节能设备，能耗减少，生产成本低；最终制备产品绿色环保，具有无毒、节能、成本低、安全、不污染环境等优点；可应用于皮革、合成革、纸张印刷和涂料生产等方面。
为此，本发明采取如下技术方案：
一种水性聚氨酯树脂制备工艺，由以下步骤实现：
a：预聚：常温常压下将质量份聚酯760-800份的多元醇，160-200份的二苯基甲烷二异氰酸酯和18-22份的二羟甲基丁酸用泵送入聚氨酯树脂反应釡，开启搅拌装置80-100℃搅拌物料3-5小时，获得预聚体；
b：回流：步骤a预聚体中加入质量份80-110份的乙酸乙酯，20-40份的丙酮，50-70℃的条件下回流反应3-5小时；
c：中和反应：之后测异氰酸根含量达3-5％时，降温到50°C以下，加入质量份8-12份的三乙胺中和；
d：分散乳化、扩链反应：中和后，保持50℃以下低温环境，15-30min内加质量份900-1100份的去离子水乳化，使预聚体在剪切力作用下分散于水中，再用质量份8-12份的乙二胺、在水中进行扩链，快速促进链增长反应，生成高分子量的水性聚氨酯，当聚合物粘度达到2000-3000mPa·s时，加质量份18-22份得异丙醇终止链增长；
e：成品包装：扩链反应结束后，向反应釡夹套中通入冷却水冷却物料到35-45℃，开启氮气控制阀向反应釡内通入氮气，将物料压入包装桶内包装即成成品聚氨酯树脂；包装时将物料通过不锈钢滤网过滤杂质。
本发明制备工艺过程简单，原料利用率高，产品转化率高达99％以上，未转化部分99％以上均回收利用，生产对环境和社会无负影响；制备工艺以去离子水为溶剂，采用节能设备，能耗减少，生产成本降低；最终制备产品绿色环保，具有无毒、节能、成本低、安全、不污染环境等优点；其中制备过程中分散乳化保持在低温环境进行，是为了降低-NCO与水反应活性。
进一步的，所述反应釡上设置冷凝器，冷凝器设置连接排放管和接收桶。保证废气收集处理。
进一步地，所述水性聚氨酯树脂制备扩链反应后多余溶剂采用真空泵抽取。回收多余溶剂，并采用冷凝器冷凝后重新利用，提高原料利用率。
本发明的有益效果：
本发明制备工艺以去离子水代替有机溶剂，采用节能设备，能耗减少，生产成本降低；生产工艺简单，原料利用率高，产品转化率高达99％以上，未转化部分99％以上均回收利用，生产对环境和社会无负影响；产品绿色环保，具有无毒、节能、成本低、安全、不污染环境等优点。
具体实施方式：
下面结合实施例对本发明做进一步说明。
实施例1
一种水性聚氨酯树脂制备工艺，其特征在于，由以下步骤实现：
a：预聚：常温常压下将质量份聚酯760份的多元醇，160份的二苯基甲烷二异氰酸酯和18份的二羟甲基丁酸用泵送入聚氨酯树脂反应釡，开启搅拌装置80-100℃搅拌物料3小时，获得预聚体；
b：回流：步骤a预聚体中加入质量份80份的乙酸乙酯，20份的丙酮，在50-70℃的条件下回流反应3小时；
c：中和反应：之后测异氰酸根含量达3-5％时，降温到50°C以下，加入质量份8份的三乙胺中和；
d：分散乳化、扩链反应：中和后，保持50℃以下低温环境，快速加质量份的900份去离子水乳化，使预聚体在剪切力作用下分散于水，再用质量份8份的乙二胺、在水中进行扩链，快速促进链增长反应，生成高分子量的水性聚氨酯，当聚合物粘度达到2000-3000mPa·s后，加质量份18份的异丙醇终止链增长；
e：成品包装：扩链反应结束后，向反应釡夹套中通入冷却水冷却物料到35-45℃，开启氮气控制阀向反应釡内通入氮气，将物料压入包装桶内包装即成成品聚氨酯树脂；包装时将物料通过不锈钢滤网过滤杂质。
其中反应釡上设置冷凝器，冷凝器上设置连接排放管和接收桶，保证废气收集处理；水性聚氨酯树脂制备扩链反应结束后去离子水等多余溶剂采用真空泵抽取；最终水性聚氨酯树脂产品的质量份为1860份。
实施例2
一种水性聚氨酯树脂制备工艺，其特征在于，由以下步骤实现：
a：预聚：常温常压下将质量份780份的聚酯多元醇，180份的二苯基甲烷二异氰酸酯和20份的二羟甲基丁酸用泵送入聚氨酯树脂反应釡，开启搅拌装置80-100℃搅拌物料4小时，获得预聚体；
b：回流：步骤a预聚体中加入质量份90份的乙酸乙酯，30份的丙酮，在50-70℃的条件下回流反应4小时；
c：中和反应：之后测异氰酸根含量达3-5％时，降温到50°C以下，加入质量份10份的三乙胺中和；
d：分散乳化、扩链反应：中和后，保持50℃以下低温环境，快速加质量份1000份的去离子水乳化，使预聚体在剪切力作用下分散于水，再用质量份10份的乙二胺、在水中进行扩链，快速促进链增长反应，生成高分子量的水性聚氨酯，当聚合物粘度达到2000-3000mPa·s后，加质量份20份的异丙醇终止链增长；
e：成品包装：扩链反应结束后，向反应釡夹套中通入冷却水冷却物料到35-45℃，开启氮气控制阀向反应釡内通入氮气，将物料压入包装桶内包装即成成品聚氨酯树脂；包装时将物料通过不锈钢滤网过滤杂质。
其中反应釡上设置冷凝器，冷凝器上设置连接排放管和接收桶，保证废气收集处理；水性聚氨酯树脂制备扩链反应结束后去离子水等多余溶剂采用真空泵抽取；最终水性聚氨酯树脂产品的质量份为2000份。
实施例3
一种水性聚氨酯树脂制备工艺，其特征在于，由以下步骤实现：
a：预聚：常温常压下将质量份800份的聚酯多元醇，200份的二苯基甲烷二异氰酸酯和22份的二羟甲基丁酸用泵送入聚氨酯树脂反应釡，开启搅拌装置80-100℃搅拌物料5小时，获得预聚体；
b：回流：步骤a预聚体中加入质量份110份的乙酸乙酯，40份的丙酮，在50-70℃的条件下回流反应5小时；
c：中和反应：之后测异氰酸根含量达3-5％时，降温到50°C以下，加入质量份12份的三乙胺中和；
d：分散乳化、扩链反应：中和后，保持50℃以下低温环境，快速加质量份1100份的去离子水乳化，使预聚体在剪切力作用下分散于水，再用质量份12份的乙二胺、在水中进行扩链，快速促进链增长反应，生成高分子量的水性聚氨酯，当聚合物粘度达到2000-3000mPa·s后，加质量份22份的异丙醇终止链增长；
e：成品包装：扩链反应结束后，向反应釡夹套中通入冷却水冷却物料到35-45℃，开启氮气控制阀向反应釡内通入氮气，将物料压入包装桶内包装即成成品聚氨酯树脂；包装时将物料通过不锈钢滤网过滤杂质。
其中反应釡上设置冷凝器，冷凝器上设置连接排放管和接收桶，保证废气收集处理；水性聚氨酯树脂制备扩链反应结束后去离子水等多余溶剂采用真空泵抽取；最终水性聚氨酯树脂产品的质量份为2150份。
以上列举的仅是本发明的具体实施例。显然，本发明不限于以上实施例，还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。
Claims (3)
1.一种水性聚氨酯树脂的制备工艺，其特征在于，由以下步骤实现：
a：预聚：常温常压下将质量份760-800份的聚酯多元醇，160-200份的二苯基甲烷二异氰酸酯和18-22份的二羟甲基丁酸用泵送入聚氨酯树脂反应釡，开启搅拌装置于80-100℃搅拌物料3-5小时，获得预聚体；
b：稀释回流：步骤a预聚体中加入质量份80-110份的乙酸乙酯，20-40份的丙酮，于50-70℃的条件下回流反应3-5小时；
c：中和反应：回流反应中检测异氰酸根含量，当其含量达到3-5％时，反应体系降温到50°C以下，加入质量份8-12份的三乙胺中和；
d：分散乳化、扩链反应：中和后，保持50℃以下低温环境，在20-30min的时间内加入质量份900-1100份的去离子水乳化，使预聚体在剪切力作用下分散于水中，再用质量份8-12份的乙二胺、在水中进行扩链，快速促进链增长反应，生成高分子量的水性聚氨酯，当聚合物粘度达到2000-3000 mPa·s时，加质量份18-22份的异丙醇终止链增长；
e：成品包装：扩链反应结束后，向反应釡夹套中通入冷却水冷却物料到35-45℃，开启氮气控制阀向反应釡内通入氮气，将物料压入包装桶内包装即成成品聚氨酯树脂；包装时将物料通过不锈钢滤网过滤杂质。
2.根据权利要求1 所述的一种水性聚氨酯树脂的制备工艺，其特征在于，所述反应釡上设置冷凝器，冷凝器设置排放管和接收桶。
3.根据权利要求1 所述的一种水性聚氨酯树脂的制备工艺，其特征在于，所述水性聚氨酯树脂制备扩链反应结束后多余溶剂采用真空泵抽取。
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