CN106243911B - 用于制备纤维防火隔热涂层的树脂组合物的制备和应用 - Google Patents

用于制备纤维防火隔热涂层的树脂组合物的制备和应用 Download PDF

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CN106243911B
CN106243911B CN201610616147.2A CN201610616147A CN106243911B CN 106243911 B CN106243911 B CN 106243911B CN 201610616147 A CN201610616147 A CN 201610616147A CN 106243911 B CN106243911 B CN 106243911B
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杨京学
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Jiangxi Hesheng Antai New Materials Co.,Ltd.
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Abstract

本发明提出一种用于制备纤维防火隔热涂层的树脂组合物的制备方法，包括步骤：1)将甲醛加入反应釜中，升温至40～50℃，加入三聚氰胺，在60～70℃温度下反应0.5～3小时；2)加入固含量调节剂，然后将反应釜升温至90～98℃，控制反应完的产物的固含量为25～35％；3)在用于制备纤维防火隔热涂层之前，按照防火隔热树脂总质量，加入1～2％的渗透剂，2～4％的酒精，6～9％的三(2‑羧乙基)膦常温下进行压渗。本各类织物防火隔热层胶由于采用了高蛋白原料合成MF胶，并在MF胶中添加了柔和剂，因此本产品不存在缩水、水洗后防火性能下降等问题，达到了织物高级别的防火性能。

Description

用于制备纤维防火隔热涂层的树脂组合物的制备和应用
技术领域
本发明属于有机材料组合物领域，具体涉及一种含有三聚氰胺树脂的耐高温材料。
背景技术
隔热衣物是工业中一些高温、冶炼、消防等场合使用的特种衣物，其是由阻燃纤维织物与真空镀铝膜的复合材料混合在一起而制作成的，需要衣物比重轻、强度高、阻燃、耐高温、抗热辐射，对人体无害。
现有的隔热衣物产品，仍存在穿着不够舒适的问题。另一方面，衣物的颜色大多是灰色，不能有鲜艳的颜色，限制了隔热衣物的市场发展。
发明内容
针对本领域存在的不足之处，本发明的目的是提出一种用于制备纤维防火隔热涂层的树脂组合物的制备方法。
本发明的第二个目的是提出所述制备方法制得的树脂组合物。
本发明的第三个目的是提出所述树脂组合物的应用。
为实现本发明上述目的的技术方案为：
一种用于制备纤维防火隔热涂层的树脂组合物的制备方法，其包括步骤：
1)将甲醛加入反应釜中，升温至40～50℃，加入三聚氰胺，在60～70℃温度下反应0.5～3小时；
2)加入固含量调节剂，然后将反应釜升温至90～98℃，控制反应完的产物的固含量为25～35％；所述固含量调节剂为无机酸，得到防火隔热树脂；
3)在用于制备纤维防火隔热涂层之前，按照防火隔热树脂总质量，加入1～2％的渗透剂，2～4％的酒精，6～9％的三(2-羧乙基)膦(TCEP)常温下进行压渗；所述纤维为造纸纤维或织物纤维。
其中，所述步骤1)中，所述甲醛以质量含量35～40％的甲醛溶液形式加入，同时加入pH值调节剂，甲醛溶液和三聚氰胺的质量比为150～250：100。
加入pH值调节剂使甲醛溶液的pH值为9～11；所述pH值调节剂为氢氧化钠、碳酸钠、碳酸氢钠、氢氧化钾中的一种或多种。
其中，所述步骤1)中，和三聚氰胺同时加入碳酰胺、增塑剂石蜡、清洁剂硼砂，三聚氰胺和碳酰胺、增塑剂、清洁剂的质量比为100:5～8：2～4：0.1～0.3。
其中，所述增塑剂为石蜡、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯或氯化石蜡，所述清洁剂为硼砂、三聚磷酸钠、二甲苯磺酸钠中的一种或多种。
进一步地，所述步骤2)中，所述固含量调节剂为磷酸、盐酸、硼酸中的一种，将固含量调节剂分2-5批加入。
其中，所述步骤3)中，所述渗透剂为食盐，所述酒精为乙醇质量含量90～99.9％的食用酒精。
本发明所述制备方法制得的树脂组合物。
本发明所述树脂组合物在织物纤维或造纸纤维整理中的应用，其是将织物纤维或造纸纤维浸在所述树脂组合物中，常温进行压渗。
本发明的有益效果在于：
本发明提出的树脂组合物是一种各类织物均可使用的防火隔热层胶，可广泛应用于纺织、造纸行业。
本各类织物防火隔热层胶由于采用了高蛋白原料合成MF胶，并在MF胶中添加了柔和剂，因此本产品不存在缩水、水洗后防火性能下降等问题，达到了织物高级别的防火性能。
本发明各类织物防火隔热层胶由高蛋白原料MF胶合成，无毒无味无烟，耐酸耐碱，防腐性强，遇高温不燃，低温不硬化，本发明MF胶添加了添加剂、碳酸铵、增塑剂、石蜡、DEP、DBP后使织物更加柔和，舒适。本发明添加了硼砂、渗透剂、TCEP或食用酒精，水洗后不掉色，使颜色更加鲜亮明洁。
综上所述，并经实验证明本各类织物防火隔热层胶耐火耐水、不收不缩、抗酸碱腐蚀，提高了织物的安全性能指标。
具体实施方式
以下实施例用于说明本发明，但不应用来限制本发明的范围。实施例中，如无特别说明，所用手段均为本领域常规技术手段。
本发明所述的质量份为本领域技术人员常用的质量单位，例如可以是克，千克，吨，或为了操作方便自定的质量单位。在同一个配方中，“份”表示的质量相同。
实施例1：
原料配比如下：
项目 原料名称 质量份数
原料 甲醛(37％) 300
原料 三聚氰胺(99.9％) 150
pH调节剂 氢氧化钠(40％) 10
添加剂 碳酰胺 9
增塑剂 石蜡 3
清洁剂 硼砂 0.3
增稠剂 磷酸(64％) 23.6
将甲醛、氢氧化钠加入反应釜中，得到的混合物pH值为10；将升温至45℃，加入三聚氰胺、碳酰胺、石蜡、硼砂，搅拌，再升温至65℃反应1小时。然后将磷酸分为等量的三批加入反应釜中，升温至95℃，此时反应釜内粘稠的体系逐变稀，完全反应完，产物的固含量为30％。磷酸按体积称取，23.6g相当于16mL。
在配织物防火渗透液时，按反应后得到的产物总质量计，加入2％渗透剂食盐，食用酒精3％TCEP 8％，在常温下对聚丙烯睛化纤维织物进行压渗(将重物压在织物上，不让织物浮起，保持1小时)。将织物取出织物晾干后，进行耐火试验，结果见表1。晾干后的织物手感柔软舒适，没有掉色现象。
实施例2：
树脂组合物的原料配比如下：
项目 原料名称 质量份数
原料 甲醛(37％) 300
原料 三聚氰胺(99.9％) 150
pH调节剂 氢氧化钠(40％) 10
添加剂 碳酰胺 9
增塑剂 石蜡 5
清洁剂 硼砂 0.3
增稠剂 磷酸(64％) 23
制备方法同实施例1。
按照和实施例1同样的方法处理织物。
实施例2：
树脂组合物的原料配比如下：
项目 原料名称 质量份数
原料 甲醛(37％) 300
原料 三聚氰胺(99.9％) 150
pH调节剂 氢氧化钠(40％) 10
添加剂 碳酰胺 9
增塑剂 石蜡 6
清洁剂 硼砂 0.3
增稠剂 磷酸(64％) 24
制备方法同实施例1。
按照和实施例1同样的方法处理织物。
试验例
实施例1、实施例2、实施例3树脂组合物压渗过的织物100×50mm，共三个样品，依据国家标准“GB/T20285-2006材料产烟毒性危险分级进行测试，测试结果为：产烟毒性t0级。
表1：阻燃性能测试结果
虽然，上文中已经本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (5)

1.一种用于制备纤维防火隔热涂层的树脂组合物的制备方法，其特征在于，包括步骤：
1)将甲醛加入反应釜中，升温至40～50℃，加入三聚氰胺，同时加入碳酰胺、增塑剂石蜡、清洁剂硼砂，三聚氰胺和碳酰胺、增塑剂、清洁剂的质量比为100:5～8：2～4：0.1～0.3，在60～70℃温度下反应0.5～3小时；
所述甲醛以质量含量35～40％的甲醛溶液形式加入，同时加入pH值调节剂，甲醛溶液和三聚氰胺的质量比为150～250：100；加入pH值调节剂使甲醛溶液的pH值为9～11；所述pH值调节剂为氢氧化钠、碳酸钠、碳酸氢钠、氢氧化钾中的一种或多种；
2)加入固含量调节剂，然后将反应釜升温至90～98℃，控制反应完的产物的固含量为25～35％；所述固含量调节剂为无机酸，得到防火隔热树脂；
3)在用于制备纤维防火隔热涂层之前，按照防火隔热树脂总质量，加入1～2％的渗透剂，2～4％的酒精，6～9％的三(2-羧乙基)膦常温下进行压渗；所述纤维为造纸纤维或织物纤维。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤2)中，所述固含量调节剂为磷酸、盐酸、硼酸中的一种，将固含量调节剂分2-5批加入。
3.根据权利要求1或2所述的制备方法，其特征在于，所述步骤3)中，所述渗透剂为食盐，所述酒精为乙醇质量含量90～99.9％的食用酒精。
4.权利要求1～3任一所述制备方法制得的树脂组合物。
5.权利要求4所述树脂组合物在织物纤维整理中的应用，其特征在于，将织物纤维浸在所述树脂组合物中，常温进行压渗。
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