CN105801813B - 超细纤维含浸用聚氨酯树脂及其制备方法 - Google Patents

超细纤维含浸用聚氨酯树脂及其制备方法 Download PDF

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CN105801813B
CN105801813B CN201610275579.1A CN201610275579A CN105801813B CN 105801813 B CN105801813 B CN 105801813B CN 201610275579 A CN201610275579 A CN 201610275579A CN 105801813 B CN105801813 B CN 105801813B
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贝文理
赵锡山
叶青
向黎
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ZHEJIANG JOYA POLYMER TECHNOLOGY Co Ltd
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Abstract

本发明涉及一种聚氨酯树脂，特别涉及一种超细纤维含浸用聚氨酯树脂及其制备方法。本发明的一种超细纤维含浸用聚氨酯树脂，由如下组分制备得到：MDI:8%‑15%、聚醚多元醇PTMEG‑1000:3%‑8%、己内酯PCL‑2000:5%‑7%、聚酯多元醇PEG‑2000:3%‑8%、乙二醇EG:2%‑5%、DMF:65‑70%；本发明利用聚酯多元醇和聚醚多元醇的特性，合成的聚氨酯树脂用于含浸超细纤维，该超细纤维在浓度为10%‑15%的氢氧化钠作用下，进行碱减量时树脂脱落率高，会产生良好的表面触感，能够提高超细纤维可染色性能，产品质量优秀。

Description

超细纤维含浸用聚氨酯树脂及其制备方法
技术领域
本发明涉及一种聚氨酯树脂，特别涉及一种超细纤维含浸用聚氨酯树脂及其制备方法。
背景技术
用超细纤维制成的纺织品在其后整理工艺中需要用聚氨酯树脂进行浸渍、涂覆等工序处理。目前，超细纤维含浸产品存在手感硬，染色性不均匀等特点，常用的方法是用氢氧化钠进行减量，这种方法表面触摸感好，可染色，有鲜明的色彩。
现有技术中聚氨酯树脂的原料配方通常由聚酯多元醇、聚醚多元醇、扩链剂、异氰酸酯、有机溶剂、链终止剂和抗氧剂以及其他助剂组成，主要采用两步法(预聚体法)合成。由于在超细纤维制品的制备过程中需要用强碱减量，对聚氨酯树脂浆料就要求其在强碱中不能被溶解或造成性能下降。但是现有技术中的聚氨酯树脂整体来说，耐溶剂和耐酸碱性较差，达不到超细纤维浸渍用的要求。
发明内容
本发明的目的在于克服现有技术的不足，提供一种超细纤维含浸用聚氨酯树脂，浸渍该聚氨酯树脂后的超细纤维制品经碱减量处理后，触摸感好，染色性能佳。
为了达到上述目的，本发明的一种超细纤维含浸用聚氨酯树脂，以重量百分比计由如下组分制备得到：
MDI(4，4`-二苯基甲烷二异氰酸酯):8％-15％
聚醚多元醇PTMEG-1000:3％-8％
聚己内酯PCL-2000:5％-7％
聚酯多元醇PEG-2000:3％-8％
乙二醇EG:2％-5％
DMF(N,N-二甲基甲酰胺):65-70％
作为优选，所述一种超细纤维含浸用聚氨酯树脂，以重量百分比计由如下组分制备得到：
MDI(4，4`-二苯基甲烷二异氰酸酯)：10.55％
聚醚多元醇PTMEG-1000:5.55％
聚己内酯PCL-2000:6.66％
聚酯多元醇PEG-2000:4.44％
乙二醇EG:2.8％
DMF(N,N-二甲基甲酰胺)：70％
本发明的另一目的是提供一种超细纤维含浸用聚氨酯树脂的制备方法，包括如下步骤：所有原料的用量以重量百分比计
步骤一：将3％-8％的聚醚多元醇PTMEG-1000、5％-7％的聚己内酯PCL-2000和3％-8％的聚酯多元醇PEG-2000投料到反应釜，加热使其熔化成液体后投入2％-5％的扩链剂乙二醇EG，然后投入42％的DMF合成反应；
步骤二：将步骤一中的反应物料搅拌一个小时之后，将8％-15％的MDI分两次进行投料；在60℃温度下，第一次投入一半用量的MDI,投入MDI后会发生温度急速上升情况，控制MDI添加速度，保持60℃温度下反应20分钟；第二次在保持80℃温度下，投入剩余量的MDI，控制MDI添加速度，达到预聚粘度后搅拌20分钟，投入剩余23-28％的DMF稀释，若粘度过低则再加少量MDI补正提粘；
步骤三、确认是否残留NCO，如有NCO残留，继续充分搅拌，达到无NCO之后投入苹果酸来稳定粘度，合成反应终止之后投入各种添加剂，如：抗紫外线吸收剂，分散剂等。
作为优选，所述一种超细纤维含浸用聚氨酯树脂的制备方法，包括如下步骤：所有原料的用量以重量百分比计
步骤一：将5.55％的聚醚多元醇PTMEG-1000、6.66％的聚己内酯PCL-2000和4.44％的聚酯多元醇PEG-2000投料到反应釜，加热使其熔化成液体后投入2.8％的扩链剂乙二醇EG，然后投入42％的DMF合成反应；
步骤二：将步骤一中的反应物料搅拌一个小时之后，将10.55％的MDI分两次进行投料；在60℃温度下，第一次投入一半用量的MDI,投入MDI后会发生温度急速上升情况，控制MDI添加速度，保持60℃温度下反应20分钟；第二次在保持80℃温度下，投入剩余量的MDI，控制MDI添加速度，达到预聚粘度后搅拌20分钟，投入剩余28％的DMF稀释，若粘度过低则再加少量MDI补正提粘；
步骤三、确认是否残留NCO，如有NCO残留，继续充分搅拌，达到无NCO之后投入苹果酸来稳定粘度，合成反应终止之后投入各种添加剂，如：抗紫外线吸收剂，分散剂等。
本发明的有益效果：通过研究发现聚氨酯树脂中的聚酯多元醇在氢氧化钠作用下容易水解，但聚醚多元醇则防碍水解。本发明利用聚酯多元醇和聚醚多元醇的特性，合成的聚氨酯树脂用于含浸超细纤维，该超细纤维在浓度为10％-15％的氢氧化钠作用下，进行碱减量时树脂脱落率高，会产生良好的表面触感，能够提高超细纤维可染色性能，产品质量优秀。
具体实施方式
实施例1：
一种超细纤维含浸用聚氨酯树脂，由如下组分制备得到：
MDI:105.5g
PTMEG-1000:55.5g
PCL-2000：66.6g
PEG-2000:44.4g
乙二醇:28g
DMF:700g
其制备方法如下：
步骤一：将55.5gPTMEG-1000、66.6gPCL-2000和44.4gPEG-2000投料到反应釜，加热使其熔化成液体后投入28g扩链剂乙二醇，然后投入420gDMF合成反应；
步骤二：将步骤一中的反应物料搅拌一个小时之后，将105.5gMDI分两次进行投料；在60℃下，第一次投入一半用量的MDI,投入MDI后会发生温度急速上升情况，控制MDI添加速度，保持60℃温度下反应20分钟；第二次在保持80℃温度下，投入剩余量的MDI，控制MDI添加速度，达到预聚粘度后搅拌20分钟，投入剩余280g的DMF稀释，若粘度过低则再加少量MDI补正提粘；
步骤三、确认是否残留NCO，如有NCO残留，继续充分搅拌，达到无NCO之后投入苹果酸来稳定粘度，合成反应终止之后投入各种添加剂，如：抗紫外线吸收剂，分散剂等。
检测制备得到的聚氯酯树脂的流动性，使用该聚氯酯树脂浸渍超细纤维，将浸渍聚氯酯树脂后的超细纤维用浓度为10％的氢氧化钠溶液，在100℃下浸泡40min，进行碱减量处理，检测树脂脱落率和表面触感；将碱减量后的超细纤维在105℃下进行染色处理2小时，检测超细纤维的可染色性。检测结果如下：
项目 树脂流动性 树脂脱落率 表面触感 可染色性
结果 好 13％ 好 好
实施例2：
一种超细纤维含浸用聚氯酯树脂，由如下组分制备得到：
MDI：95g
PTMEG-1000：50g
PCL-2000：60g
PEG-2000：40g
乙二醇：25.2g
DMF：630.9g
其制备方法如下：
步骤一：将50gPTMEG-1000、60gPCL-2000和40gPEG-2000投料到反应釜，加热使其熔化成液体后投入25.2g扩链剂乙二醇，然后投入378.42gDMF合成反应；
步骤二：将步骤一中的反应物料搅拌一个小时之后，将95gMDI分两次进行投料；在60℃下，第一次投入一半用量的MDI，投入MDI后会发生温度急速上升情况，控制MDI添加速度，保持60℃温度下反应20分钟；第二次在保持80℃温度下，投入剩余量的MDI，控制MDI添加速度，达到预聚粘度后搅拌20分钟，投入剩余252.48g的DMF稀释，若粘度过低则再加少量MDI补正提粘；
步骤三、确认是否残留NCO，如有NCO残留，继续充分搅拌，达到无NCO之后投入苹果酸来稳定粘度，合成反应终止之后投入各种添加剂，如：抗紫外线吸收剂，分散剂等。
检测制备得到的聚氯酯树脂的流动性，使用该聚氯酯树脂浸渍超细纤维，将浸渍聚氯酯树脂后的超细纤维用浓度为10％的氢氧化钠溶液，在100℃下浸泡40min，进行碱减量处理，检测树脂脱落率和表面触感；将碱减量后的超细纤维在105℃下进行染色处理2小时，检测超细纤维的可染色性。检测结果如下：
项目 树脂流动性 树脂脱落率 表面触感 可染色性
结果 较好 17％ 好 优秀
实施例3：
一种超细纤维含浸用聚氯酯树脂，由如下组分制备得到：
MDI：80g
PTMEG-1000：30g
PCL-2000：70g
PEG-2000：80g
乙二醇：50g
DMF：690g
其制备方法如下：
步骤一：将30gPTMEG-1000、70gPCL-2000和80gPEG-2000投料到反应釜，加热使其熔化成液体后投入50g扩链剂乙二醇，然后投入420gDMF合成反应；
步骤二：将步骤一中的反应物料搅拌一个小时之后，将80gMDI分两次进行投料；在60℃下，第一次投入一半用量的MDI，投入MDI后会发生温度急速上升情况，控制MDI添加速度，保持60℃温度下反应20分钟；第二次在保持80℃温度下，投入剩余量的MDI，控制MDI添加速度，达到预聚粘度后搅拌20分钟，投入剩余270g的DMF稀释，若粘度过低则再加少量MDI补正提粘；
步骤三、确认是否残留NCO，如有NCO残留，继续充分搅拌，达到无NCO之后投入苹果酸来稳定粘度，合成反应终止之后投入各种添加剂，如：抗紫外线吸收剂，分散剂等。
检测制备得到的聚氯酯树脂的流动性，使用该聚氯酯树脂浸渍超细纤维，将浸渍聚氯酯树脂后的超细纤维用浓度为10％的氢氧化钠溶液，在100℃下浸泡40min，进行碱减量处理，检测树脂脱落率和表面触感；将碱减量后的超细纤维在105℃下进行染色处理2小时，检测超细纤维的可染色性。检测结果如下：
项目 树脂流动性 树脂脱落率 表面触感 可染色性
结果 较好 12％ 好 较好
实施例4：
一种超细纤维含浸用聚氯酯树脂，由如下组分制备得到：
MDI：150g
PTMEG-1000：80g
PCL-2000：50g
PEG-2000：30g
乙二醇：20g
DMF：670g
其制备方法如下：
步骤一：将80gPTMEG-1000、50gPCL-2000和30gPEG-2000投料到反应釜，加热使其熔化成液体后投入20g扩链剂乙二醇，然后投入420gDMF合成反应；
步骤二：将步骤一中的反应物料搅拌一个小时之后，将150gMDI分两次进行投料；在60℃下，第一次投入一半用量的MDI，投入MDI后会发生温度急速上升情况，控制MDI添加速度，保持60℃温度下反应20分钟；第二次在保持80℃温度下，投入剩余量的MDI，控制MDI添加速度，达到预聚粘度后搅拌20分钟，投入剩余250g的DMF稀释，若粘度过低则再加少量MDI补正提粘；
步骤三、确认是否残留NCO，如有NCO残留，继续充分搅拌，达到无NCO之后投入苹果酸来稳定粘度，合成反应终止之后投入各种添加剂，如：抗紫外线吸收剂，分散剂等。
检测制备得到的聚氯酯树脂的流动性，使用该聚氯酯树脂浸渍超细纤维，将浸渍聚氯酯树脂后的超细纤维用浓度为10％的氢氧化钠溶液，在100℃下浸泡40min，进行碱减量处理，检测树脂脱落率和表面触感；将碱减量后的超细纤维在105℃下进行染色处理2小时，检测超细纤维的可染色性。检测结果如下：
项目 树脂流动性 树脂脱落率 表面触感 可染色性
结果 较好 11％ 较好 好

Claims (1)

1.一种超细纤维含浸用聚氨酯树脂，其特征在于：以重量百分比计由如下组分制备得到：
MDI(4，4`-二苯基甲烷二异氰酸酯)：10.55％
聚醚多元醇PTMEG-1000:5.55％
聚己内酯PCL-2000:6.66％
PEG-2000:4.44％
乙二醇EG:2.8％
DMF(N,N-二甲基甲酰胺)：70％；
包括如下步骤：所有原料的用量以重量百分比计：
步骤一：将5.55％的聚醚多元醇PTMEG-1000、6.66％的聚己内酯PCL-2000和4.44％的PEG-2000投料到反应釜，加热使其熔化成液体后投入2.8％的扩链剂乙二醇EG，然后投入42％的DMF合成反应；
步骤二：将步骤一中的反应物料搅拌一个小时之后，将10.55％的MDI分两次进行投料；在60℃温度下，第一次投入一半用量的MDI,投入MDI后会发生温度急速上升情况，控制MDI添加速度，保持60℃温度下反应20分钟；第二次在保持80℃温度下，投入剩余量的MDI，控制MDI添加速度，达到预聚粘度后搅拌20分钟，投入剩余28％的DMF稀释，若粘度过低则再加少量MDI补正提粘；
步骤三、确认是否残留NCO，如有NCO残留，继续充分搅拌，达到无NCO之后投入苹果酸来稳定粘度，合成反应终止之后投入各种添加剂，所述添加剂为抗紫外线吸收剂、分散剂。
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