CN106049049B - 涤纶织物耐久型阻燃、拒水、防水透湿整理方法 - Google Patents

涤纶织物耐久型阻燃、拒水、防水透湿整理方法 Download PDF

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CN106049049B
CN106049049B CN201610622119.1A CN201610622119A CN106049049B CN 106049049 B CN106049049 B CN 106049049B CN 201610622119 A CN201610622119 A CN 201610622119A CN 106049049 B CN106049049 B CN 106049049B
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陈丽颖
李金华
张悦
赵颖
葛川
任亚坤
王芳
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Dandong Unik Textile Ltd
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Abstract

本发明涤纶织物耐久型阻燃、拒水、防水透湿整理方法，由环状磷酸酯阻燃剂20‑30份、水60‑70份、异氰酸酯交联剂1‑1.5份、氟碳化合物共聚物防水剂3‑5份、质量浓度10%NaOH2‑5份制得的阻燃拒水整理剂，由聚醚型聚氨酯聚合物底涂胶100份、甲苯5‑10份、丁酮5‑10份异氰酸酯交联剂2份、促进剂1份、有机磷氮系阻燃剂25‑35份制得的底层涂层胶，由聚醚型聚氨酯聚合物面涂胶100份、甲苯35‑45份制得的面层涂层胶，对织物进行阻燃拒水剂浸轧、轧光、底涂、面涂完成整理。

Description

涤纶织物耐久型阻燃、拒水、防水透湿整理方法
技术领域
本发明涉及的是一种纺织品面料后整理技术。特别适用于涤纶长丝牛津布。具体涉及的是涤纶织物耐久型阻燃、拒水、防水透湿涂层整理方法。
背景技术
涤纶是世界产量最大，应用最广泛的合成纤维品种，占世界合成纤维产量的60%以上，大量用于衣料、床上用品、各种装饰布料、国防军工特殊织物等纺织品以及其他工业用纤维制品。由于涤纶织物合成材料的特性，具有非常易燃的特点，因而涤纶阻燃织物的开发显得极为重要。
专利CN103469603A《一种涤纶面料阻燃整理方法》公开了一种涤纶面料阻燃整理工艺方法；面料碱处理—阻燃浸轧—水洗—焙烘。该工艺整理的涤纶织物不具备除阻燃功能以外的其他功能，且操作工艺复杂。
专利CN103046316A《一种环保阻燃防水涂层织物的整理方法》公开了一种涤纶阻燃防水织物工艺：前拒水—涂层—后拒水，整理后涤纶织物阻燃达国家标准B1级别，但该方法未提及织物具备耐洗的阻燃、拒水性能。
专利CN103276598A《一种阻燃防水透气透湿涂层及其制备方法》公开了一种聚氨酯树脂防水透湿涂层底胶与聚氨酯树脂防水透湿涂层面胶的合成方法。该方法整理面料具有良好的阻燃性能、拒水性能，但未提及拒水能达到的等级。
发明内容
本发明的目的是提供一种生产简单方便，耐水洗性强，具有阻燃、拒水、透湿功能兼备的涤纶织物耐久型阻燃、拒水、防水透湿整理方法。整理后织物变色程度小、手感柔软、拒水≥4级，5次水洗后织物拒水≥2级，阻燃级别达到国家标准B1级别。
本发明涤纶织物耐久型阻燃、拒水、防水透湿涂层整理方法：
A. 阻燃拒水整理剂制备，原料重量配比：
环状磷酸酯阻燃剂 20-30份
水 60-70份
异氰酸酯交联剂 1-1.5 份
氟碳化合物共聚物防水剂 3-5份
质量浓度10% NaOH 2-5份
上述原料按照以上顺序混合搅拌均匀，调节整理液的pH值在5.5-6.5之间。
B.底层涂层胶的制备,原料重量配比：
聚醚型聚氨酯聚合物底涂胶 100份
甲苯 5-10份
丁酮 5-10份
异氰酸酯交联剂 2份
促进剂 1份
有机磷氮系阻燃剂 25-35份
上述原料搅拌分散均匀，得到底涂涂层胶，粘度15000-20000mPa.s。
C.面层涂层胶制备，原料重量配比：
聚醚型聚氨酯聚合物面涂胶 100份
甲苯 35-45份
上述原料搅拌分散均匀，得到面层涂层胶，粘度6500-8000mPa.s。
D.整理工艺过程：
(1)阻燃拒水整理：涤纶织物用A制备的整理剂二浸二轧，110-130℃预烘1-2min、185-195℃焙烘1-2min；
(2)轧光整理：压力9MPa，温度100℃，车速25m/min；
(3)底涂：将步骤（2）轧光后的织物采用B制备的涂层胶进行涂层，130-150℃烘干2-3min，干增重20-25g/m²；
(4)面涂：将步骤（3）底涂后的织物采用C制备的涂层胶进行面涂， 160-170℃烘干1-2min，干增重10-15g/m²。
所述环状磷酸酯阻燃剂，选自江苏利思德化工FR-CU产品；
所述异氰酸酯交联剂，选自辽宁恒星精细化工DF-897产品；
所述氟碳化合物共聚物防水剂，可选自日本大金TG-580产品；
所述聚醚型聚氨酯聚合物底涂胶，选自辽宁恒星精细化工FS-5600产品；
所述促进剂，选自辽宁恒星精细化工DF-899产品；
所述有机磷氮系阻燃剂，选自科莱恩Pekoflam HFC p产品；
所述聚醚型聚氨酯聚合物面涂胶，选自辽宁恒星精细化工FS-5811A产品。
本发明浸轧过程中，加入的异氰酸酯交联剂，其释放异氰酸基-NCO，可与环状磷酸酯中活泼氢反应；可与氟碳化合物共聚物防水剂中的活泼氢反应，使防水剂中氟原子有效聚集在聚合物表面，同时不影响环状磷酸酯阻燃性能的发挥；同时其也可与涤纶织物中含有的羟基反应；异氰酸酯交联剂起到桥梁作用，将氟碳防水剂、有机磷酸酯阻燃剂、涤纶织物有效结合，使织物具备耐久的拒水、阻燃两种功能效果。
此外，异氰酸酯交联剂可使涤纶织物纤维蓬化、空穴增加、比表面增加，增加阻燃剂分子进入纤维内部的通道，进一步增加织物阻燃性能。
底涂涂层胶采用聚醚型聚氨酯聚合物，该聚合物材料中含有一定量的亲水基团，这些基团以氢键形式“捕获”人体散发的水蒸气分子，由于聚氨酯大分子链的热运动，在分子链之间形成瞬间的空隙，加上胶膜内外两侧水蒸气压差的推动，水蒸气分子沿密集的分子链间空隙从蒸气压高的一面“传递”到另一面，即从接触皮肤的一面传到周围环境，达到透湿目的。
底涂涂层胶中添加有机磷氮系阻燃剂，有机磷氮系阻燃剂以物理分散状态与聚醚型聚氨酯聚合物进行共混。使涂层后的织物在高温燃烧过程中促使纤维素物质分解形成焦炭和水，并增加焦炭残留物的生产量，进一步提升织物的阻燃效果。
底涂涂层胶在高温130-150℃焙烘过程中，使浸轧后织物表面未反应完全的异氰酸酯活性基团被进一步释放，该基团可与底涂涂层胶聚醚型聚氨酯含有的活泼氢反应，增强底涂层层胶与浸轧后基布的结合牢度。此外，底涂涂层胶中含有异氰酸酯交联剂，其释放的活性-NCO基团可与涤纶织物的羟基反应，进一步增强底涂涂层胶与织物的结合牢度。
面层涂层胶采用聚醚型聚氨酯聚合物，该聚合物中含有微孔木质纤维素，木质纤维素的微孔结构增加聚醚型聚氨酯中水分子的吸附-脱附的透湿通道，进一步提升织物透湿性能。此外，微孔木质纤维素可赋予织物滑爽性能及柔软的手感。
面涂涂层胶160-170℃高温焙烘过程中，底涂涂层胶中的异氰酸酯交联剂高温条件下可进一步释放出游离的活性-NCO基团，该基团可与面涂涂层胶中聚醚型聚氨酯中的活泼氢进一步反应，增强底涂涂层胶与面涂涂层胶的结合牢度、增加耐洗牢度，使织物具备耐久的阻燃、拒水性能。经本发明方法整理的面料具有耐久的拒水、阻燃、高透湿性能，并且面料手感柔软滑爽、变色程度小。
具体实施方式
：阻燃拒水整理剂制备，原料重量配比：
实施例1
环状磷酸酯阻燃剂 20份
水 60份
异氰酸酯交联剂 1 份
氟碳化合物共聚物防水剂 3份
质量浓度10% NaOH 2份
上述原料按照以上顺序混合搅拌均匀，调节整理液的pH值5.5。
实施例2
环状磷酸酯阻燃剂 23份
水 62份
异氰酸酯交联剂 1.2 份
氟碳化合物共聚物防水剂 3.5份
质量浓度10% NaOH 3份
上述原料按照以上顺序混合搅拌均匀，调节整理液的pH值6.0。
实施例3
环状磷酸酯阻燃剂 25份
水 64份
异氰酸酯交联剂 1.3 份
氟碳化合物共聚物防水剂 4份
质量浓度10% NaOH 4份
上述原料按照以上顺序混合搅拌均匀，调节整理液的pH值6.0。
实施例4
环状磷酸酯阻燃剂 28份
水 68份
异氰酸酯交联剂 1.4份
氟碳化合物共聚物防水剂 4.3份
质量浓度10% NaOH 4.5份
上述原料按照以上顺序混合搅拌均匀，调节整理液的pH值6.5。
实施例5
环状磷酸酯阻燃剂 30份
水 70份
异氰酸酯交联剂 1.5份
氟碳化合物共聚物防水剂 5份
质量浓度10% NaOH 5份
上述原料按照以上顺序混合搅拌均匀，调节整理液的pH值6.5。
：底层涂层胶的制备,原料重量配比：
实施例1
聚醚型聚氨酯聚合物底涂胶 100份
甲苯 5份
丁酮 5份
异氰酸酯交联剂 2份
促进剂 1份
有机磷氮系阻燃剂 25份
上述原料搅拌分散均匀，得到底涂涂层胶，粘度20000mPa.s。
实施例2
聚醚型聚氨酯聚合物底涂胶 100份
甲苯 7份
丁酮 5份
异氰酸酯交联剂 2份
促进剂 1份
有机磷氮系阻燃剂 28份
上述原料搅拌分散均匀，得到底涂涂层胶，粘度18000mPa.s。
实施例3
聚醚型聚氨酯聚合物底涂胶 100份
甲苯 8份
丁酮 6份
异氰酸酯交联剂 2份
促进剂 1份
有机磷氮系阻燃剂 30份
上述原料搅拌分散均匀，得到底涂涂层胶，粘度17000mPa.s。
实施例4
聚醚型聚氨酯聚合物底涂胶 100份
甲苯 10份
丁酮 8份
异氰酸酯交联剂 2份
促进剂 1份
有机磷氮系阻燃剂 33份
上述原料搅拌分散均匀，得到底涂涂层胶，粘度15000mPa.s。
实施例5
聚醚型聚氨酯聚合物底涂胶 100份
甲苯 5份
丁酮 10份
异氰酸酯交联剂 2份
促进剂 1份
有机磷氮系阻燃剂 35份
上述原料搅拌分散均匀，得到底涂涂层胶，粘度17000mPa.s。
：面层涂层胶制备，原料重量配比：
实施例1
聚醚型聚氨酯聚合物面涂胶 100份
甲苯 35份
上述原料搅拌分散均匀，得到面层涂层胶，粘度8000mPa.s。
实施例2
聚醚型聚氨酯聚合物面涂胶 100份
甲苯 38份
上述原料搅拌分散均匀，得到面层涂层胶，粘度7700mPa.s。
实施例3
聚醚型聚氨酯聚合物面涂胶 100份
甲苯 40份
上述原料搅拌分散均匀，得到面层涂层胶，粘度7200mPa.s。
实施例4
聚醚型聚氨酯聚合物面涂胶 100份
甲苯 43份
上述原料搅拌分散均匀，得到面层涂层胶，粘度6800mPa.s。
实施例5
聚醚型聚氨酯聚合物面涂胶 100份
甲苯 45份
上述原料搅拌分散均匀，得到面层涂层胶，粘度6500mPa.s。
上述实施例中环状磷酸酯阻燃剂，选自江苏利思德化工FR-CU产品；
上述实施例中氟碳化合物共聚物防水剂，选自日本大金TG-580产品；
上述实施例中有机磷氮系阻燃剂，选自科莱恩Pekoflam HFC p产品；
上述实施例中聚醚型聚氨酯聚合物底涂胶，选自辽宁恒星精细化工FS-5600产品；
上述实施例中聚醚型聚氨酯聚合物面涂胶，选自辽宁恒星精细化工FS-5811A产品；
所述异氰酸酯交联剂，选自辽宁恒星精细化工DF-897产品；
所述促进剂，选自辽宁恒星精细化工DF-899产品。
：具体整理工艺过程：
实施例1
（1）阻燃拒水整理：用A阻燃拒水整理剂制备实施例1制备的阻燃拒水整理剂对涤纶织物进行二浸二轧，110-130℃预烘2min、185-195℃焙烘1min；
（2）轧光整理：压力9MPa，温度100℃，车速25m/min；
（3）底涂：将步骤（2）轧光后的涤纶织物采用B底层涂层胶的制备实施例2制备的底涂涂层胶进行涂层，烘干温度130-150℃，时间2min，增重20g/m²；
（4）面涂：将步骤（3）底涂后的涤纶织物采用C面层涂层胶制备实施例5制备的面层涂层胶进行涂层，烘干温度160-170℃，时间1min，增重10g/m²。
实施例2
（1）阻燃拒水整理：用A阻燃拒水整理剂制备实施例2制备的阻燃拒水整理剂对涤纶织物进行二浸二轧，110-130℃预烘2min、185-195℃焙烘1min；
（2）轧光整理：压力9MPa，温度100℃，车速25m/min；
（3）底涂：将步骤（2）轧光后的涤纶织物采用B底层涂层胶的制备实施例1制备的底涂涂层胶进行涂层，烘干温度130-150℃，时间3min，增重25g/m²；
（4）面涂：将步骤（3）底涂后的涤纶织物采用C面层涂层胶制备实施例4制备的面层涂层胶进行涂层，烘干温度160-170℃，时间1min，增重12g/m²。
实施例3
（1）阻燃拒水整理：用A阻燃拒水整理剂制备实施例3制备的阻燃拒水整理剂对涤纶织物进行二浸二轧，110-130℃预烘1.5min、185-195℃焙烘1.5min；
（2）轧光整理：压力9MPa，温度100℃，车速25m/min；
（3）底涂：将步骤（2）轧光后的涤纶织物采用B底层涂层胶的制备实施例5制备的底涂涂层胶进行涂层，烘干温度130-150℃，时间2min，增重22g/m²；
（4）面涂：将步骤（3）底涂后的涤纶织物采用C面层涂层胶制备实施例3制备的面层涂层胶进行涂层，烘干温度160-170℃，时间1min，增重15g/m²。
实施例4：
（1）阻燃拒水整理：用A阻燃拒水整理剂制备实施例4制备的阻燃拒水整理剂对涤纶织物进行二浸二轧，110-130℃预烘1 min、185-195℃焙烘2min；
（2）轧光整理：压力9MPa，温度100℃，车速25m/min；
（3）底涂：将步骤（2）轧光后的涤纶织物采用B底层涂层胶的制备实施例4制备的底涂涂层胶进行涂层，烘干温度130-150℃，时间2.5min，增重22g/m²；
（4）面涂：将步骤（3）底涂后的涤纶织物采用C面层涂层胶制备实施例2制备的面层涂层胶进行涂层，烘干温度160-170℃，时间1.5min，增重10g/m²。
实施例5：
（1）阻燃拒水整理：用A阻燃拒水整理剂制备实施例5制备的阻燃拒水整理剂对涤纶织物进行二浸二轧，110-130℃预烘1min、185-195℃焙烘2min；
（2）轧光整理：压力9MPa，温度100℃，车速25 m/min；
（3）底涂：将步骤（2）轧光后的涤纶织物采用B底层涂层胶的制备实施例3制备的底涂涂层胶进行涂层，烘干温度130-150℃，时间2.2min，增重22g/m²；
（4）面涂：将步骤（3）底涂后的涤纶织物采用C面层涂层胶制备实施例1制备的面层涂层胶涂层，烘干温度160-170℃，时间2min，增重13g/m²。
：基布选择
实验例1：
上述D具体整理工艺过程中所述涤纶织物选择200D涤纶长丝牛津布，克重130g/m²。
实验例2：
上述D具体整理工艺过程中所述涤纶织物选择150D涤纶长丝牛津布，克重115g/m²。
实验例3：
上述D具体整理工艺过程中所述涤纶织物选择150D涤纶弹丝牛津布，克重 97g/m²。
实验例4：
上述D具体整理工艺过程中所述涤纶织物选择涤纶300D弹丝丝牛津布，克重148g/m²。
按照背景技术中提及的三种现有常用技术方法对涤纶织物进行处理，并与本发明实施实验例产品技术指标进行对比：
对比例1：
（1）采用上述E基布选择所述各种涤纶织物面料进行碱处理:工艺配方NaOH 20g/L,阳离子渗透剂0.3g/L，处理温度95-100℃，20-60min，处理过的织物充分水洗，去除残碱后烘干；
（2）浸轧阻燃剂配制：
阻燃剂(ATP) 150g/L
NaOH 含量 8%
(3)对织物用上述（2）阻燃剂进行二浸二轧，110-130℃预烘1-2min，185-195℃培烘；
（4）水洗 ；
（5）烘干。
对比例2：
（1）采用上述E基布选择所述各种涤纶织物面料进行前拒水整理：
将氟系拒水剂与水混合制成拒水整理剂，拒水剂用量20g/L，对织进行二浸二轧，165-185℃焙烘；
（2）轧光整理：压力8-9MPa，温度100-110℃，车速25m/min；
（3）涂层整理：将水性聚氨酯涂层胶100份、异氰酸酯交联剂2份、无机镁铝水滑石阻燃剂10份混合后搅拌均匀，制得阻燃涂层胶，对步骤（2）轧光整理后的织物进行干法涂层，焙烘温度160-180℃，时间2min；
（4）后拒水：将氟系防水剂与水混合制成拒水整理剂，拒水剂用量30g/L，对步骤（3）涂层整理后的织物进行二浸二轧，180-190℃焙烘，时间1min。
对比例3：
（1）采用上述E基布选择所述各种涤纶织物进行底涂：将聚氨酯树脂防水透湿底层涂层胶100份、异氰酸酯交联剂2份、磷酸酯类阻燃剂20份混合搅拌均匀，制得阻燃涂层胶，对织物进行底层干法涂层，焙烘温度110-120℃，时间2min；
（2）面涂：用聚氨酯树脂防水透湿面层涂层胶进行干法面层涂层，焙烘温度150-165℃，时间1min。
产品具体技术指标对比结果：
实验例1对应结果，表1。
实验例2对应结果，表2。
实验例3对应结果，表3。
实验例4对应结果，表4
测试方法：
拒水测试：按GB/T 4745-2012《纺织品 防水性能的检测和评价 沾水法》标准测定；
阻燃测试：按GB/T 5455-1997《纺织品 燃烧性能试验 垂直法》标准测定；
变色级别：按GB 250-2008《纺织品 色牢度试验 评定变色用灰色样卡》标准测定；
克重测试：按照GB/T 4669-1995标准测试；
透湿量测试：按GB/T 12704.2.B -2009标准测试；
耐水洗测试：按照GB/T 8629-2001 5A 程序洗5次；
手感：凭经验评比。
通过上表比较可以看出，由本发明获得的产品其阻燃、拒水耐久效果明显高于普通阻燃拒水面料产品，同时其手感及透湿量等指标也达到较好要求，产品综合性能良好。

Claims (1)

1.涤纶织物耐久型阻燃、拒水、防水透湿整理方法，其特征是：
A. 阻燃拒水整理剂制备，原料按重量配比：
环状磷酸酯阻燃剂 20-30份
水 60-70份
异氰酸酯交联剂 1-1.5 份
氟碳化合物共聚物防水剂 3-5份
质量浓度10% NaOH 2-5份
上述原料按照以上顺序混合搅拌均匀，调节整理液的pH值在5.5-6.5之间；
B.底层涂层胶的制备，原料按重量配比：
聚醚型聚氨酯聚合物底涂胶 100份
甲苯 5-10份
丁酮 5-10份
异氰酸酯交联剂 2份
促进剂 1份
有机磷氮系阻燃剂 25-35份
上述原料搅拌分散均匀，得底涂涂层胶，粘度15000-20000mPa.s；
C.面层涂层胶制备，原料按重量配比：
聚醚型聚氨酯聚合物面涂胶 100份
甲苯 35-45份
上述原料搅拌分散均匀，得面层涂层胶，粘度6500-8000mPa.s；
D.整理工艺：
(1)阻燃拒水整理：涤纶织物用A制备的整理剂二浸二轧，110-130℃预烘1-2min、185-195℃焙烘1-2min；
(2)轧光整理：压力9MPa，温度100℃，车速25m/min；
(3)底涂：将步骤（2）轧光后的织物采用B制备的涂层胶进行涂层，130-150℃烘干2-3min，干增重20-25g/m²；
(4)面涂：将步骤（3）底涂后的织物采用C制备的涂层胶进行面涂， 160-170℃烘干1-2min，干增重10-15g/m²；
所述环状磷酸酯阻燃剂，选自江苏利思德化工FR-CU产品；
所述异氰酸酯交联剂，选自辽宁恒星精细化工DF-897产品；
所述聚醚型聚氨酯聚合物底涂胶，选自辽宁恒星精细化工FS-5600产品；
所述促进剂，选自辽宁恒星精细化工DF-899产品；
所述有机磷氮系阻燃剂，选自科莱恩Pekoflam HFC p产品；
所述聚醚型聚氨酯聚合物面涂胶，选自辽宁恒星精细化工FS-5811A产品。
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