CN106758205A - 一种无甲醛耐久阻燃剂的制备方法 - Google Patents
一种无甲醛耐久阻燃剂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种无甲醛耐久阻燃剂的制备方法,包括以下制备步骤:取二羟甲基膦酸酯、二元醇、亚膦酸三苯酯、辛酸亚锡;备用;本发明所述阻燃剂,产物澄清、黄色的粘性液体。密度为1570g/L,粘度为26Pa·s,酸度值为l.8。该阻燃剂与多元羧酸及酸性催化剂构成阻燃整理体系,在织物上形成网状交联,使阻燃效果具有耐洗性,从而得到无甲醛耐久阻燃棉织物。该阻燃剂可大大降低棉织物的热裂解温度,应用时不需要特殊工艺和设备,阻燃效果具有耐久性,可满足多领域对纺织品的阻燃要求。
Description
技术领域
本发明涉及一种无甲醛耐久阻燃剂的制备。
背景技术
围绕棉织物的阻燃技术,国内外已开发了一些适用于纺织品整理的阻燃剂及相应的工艺。如棉织物耐久阻燃剂以英国的THPc、瑞士ciba公司的Pvrovalex cP为代表。THPC为四羟甲基氯化磷,在合成过程中有可能产生双氯甲醚,有致癌的危险性,且含有游离甲醛,现已禁用。Pvrovalex cP属羟甲基酰胺的磷酸酯类化合物,含有大量游离甲醛,为了使其与纤维化学交联以获得耐洗性,整理时还要使用含甲醛的多羟甲基三聚氰胺类(如HMM)交联剂,致使整理后织物上的游离甲醛含量很高,大于O 3%,且有后续甲醛释放问题。
国产阻燃剂cFR一20l、FRc一2、nD一512等均属此类。Pvrovalex cP阻燃剂的主要成分为N一羟甲基.3.二甲氧磷酰基丙酰胺,它含有活性基团,在150℃以上能与纤维素交联或借助于交联剂与纤维素交联形成共价键,使织物产生耐久的阻燃性能。Pvrovalex cP类阻燃剂作为棉织物阻燃整理剂,阻燃效果及耐久性好,对织物的强力损失少,手感良好,但因含有大量游离甲醛限制了其发展。随着世界各国对生产场所和纺织品上游离甲醛含量限制法规的实施,无甲醛耐久阻燃剂的研究开发成为研究工作者的重要课题。
发明内容
本发明提出一种无甲醛耐久阻燃剂的制备方法。
一种无甲醛耐久阻燃剂的制备方法,其特征在于包括以下制备步骤:
(1)取二羟甲基膦酸酯、二元醇、亚膦酸三苯酯、辛酸亚锡;备用;
(2)在装有搅拌器、温度计、滴液漏斗、冷凝器的四口烧瓶中,加入甲基膦酸酯284g,亚膦酸三苯酯13g,加热至50℃;
(3)加入含磷氧化物284g,隔绝水气;
(4)将反应物加热至70-100℃,直到无反应现象发生,时长为1-5h;
(5)将反应混合物冷却到50℃,再加入亚膦酸三苯酯13g,直到无反应现象发生时长为1h;
(6)将反应混合物加热至一定温度,缓慢滴加二元醇142g,在冰水浴环境下剧烈放热反应,直到滴加完毕,时长为3h;
(7)在反应物中加入辛酸亚锡lg,保持反应温度为60-120℃,持续到无反应现象为止,时长为1-5h;即得产物。
优选地,所述步骤(4)反应物加热至90℃,直到无反应现象发生,时长为3h。
优选地,所述步骤(7)反应温度为80℃,持续到无反应现象为止,时长为3h。
本发明所述阻燃剂,产物澄清、黄色的粘性液体。密度为1570g/L,粘度为26Pa·s,酸度值为l.8。该阻燃剂与多元羧酸及酸性催化剂构成阻燃整理体系,在织物上形成网状交联,使阻燃效果具有耐洗性,从而得到无甲醛耐久阻燃棉织物。该阻燃剂可大大降低棉织物的热裂解温度,应用时不需要特殊工艺和设备,阻燃效果具有耐久性,可满足多领域对纺织品的阻燃要求。
具体实施方式
实施例1。
一种无甲醛耐久阻燃剂的制备方法,其特征在于包括以下制备步骤:
(1)取二羟甲基膦酸酯、二元醇、亚膦酸三苯酯、辛酸亚锡;备用;
(2)在装有搅拌器、温度计、滴液漏斗、冷凝器的四口烧瓶中,加入甲基膦酸酯284g,亚膦酸三苯酯13g,加热至50℃;
(3)加入含磷氧化物284g,隔绝水气;
(4)将反应物加热至70-100℃,直到无反应现象发生,时长为1-5h;
(5)将反应混合物冷却到50℃,再加入亚膦酸三苯酯13g,直到无反应现象发生时长为1h;
(6)将反应混合物加热至一定温度,缓慢滴加二元醇142g,在冰水浴环境下剧烈放热反应,直到滴加完毕,时长为3h;
(7)在反应物中加入辛酸亚锡lg,保持反应温度为60-120℃,持续到无反应现象为止,时长为1-5h;即得产物。
实施例2。
一种无甲醛耐久阻燃剂的制备方法,其特征在于包括以下制备步骤:
(1)取二羟甲基膦酸酯、二元醇、亚膦酸三苯酯、辛酸亚锡;备用;
(2)在装有搅拌器、温度计、滴液漏斗、冷凝器的四口烧瓶中,加入甲基膦酸酯284g,亚膦酸三苯酯13g,加热至50℃;
(3)加入含磷氧化物284g,隔绝水气;
(4)将反应物加热至90℃,直到无反应现象发生,时长为3h;
(5)将反应混合物冷却到50℃,再加入亚膦酸三苯酯13g,直到无反应现象发生时长为1h;
(6)将反应混合物加热至一定温度,缓慢滴加二元醇142g,在冰水浴环境下剧烈放热反应,直到滴加完毕,时长为3h;
(7)在反应物中加入辛酸亚锡lg,保持反应温度为60-120℃,持续到无反应现象为止,时长为1-5h;即得产物。
优选地,所述步骤(4)反应物加热至90℃,直到无反应现象发生,时长为3h。
实施例3。
一种无甲醛耐久阻燃剂的制备方法,其特征在于包括以下制备步骤:
(1)取二羟甲基膦酸酯、二元醇、亚膦酸三苯酯、辛酸亚锡;备用;
(2)在装有搅拌器、温度计、滴液漏斗、冷凝器的四口烧瓶中,加入甲基膦酸酯284g,亚膦酸三苯酯13g,加热至50℃;
(3)加入含磷氧化物284g,隔绝水气;
(4)将反应物加热至90℃,直到无反应现象发生,时长为3h;
(5)将反应混合物冷却到50℃,再加入亚膦酸三苯酯13g,直到无反应现象发生时长为1h;
(6)将反应混合物加热至一定温度,缓慢滴加二元醇142g,在冰水浴环境下剧烈放热反应,直到滴加完毕,时长为3h;
(7)在反应物中加入辛酸亚锡lg,保持反应温度为80℃,持续到无反应现象为止,时长为3h;即得产物。
Claims (3)
1.一种无甲醛耐久阻燃剂的制备方法,其特征在于包括以下制备步骤:
(1)取二羟甲基膦酸酯、二元醇、亚膦酸三苯酯、辛酸亚锡;备用;
(2)在装有搅拌器、温度计、滴液漏斗、冷凝器的四口烧瓶中,加入甲基膦酸酯284g,亚膦酸三苯酯13g,加热至50℃;
(3)加入含磷氧化物284g,隔绝水气;
(4)将反应物加热至70-100℃,直到无反应现象发生,时长为1-5h;
(5)将反应混合物冷却到50℃,再加入亚膦酸三苯酯13g,直到无反应现象发生时长为1h;
(6)将反应混合物加热至一定温度,缓慢滴加二元醇142g,在冰水浴环境下剧烈放热反应,直到滴加完毕,时长为3h;
(7)在反应物中加入辛酸亚锡lg,保持反应温度为60-120℃,持续到无反应现象为止,时长为1-5h;即得产物。
2.如权利要求1所述一种无甲醛耐久阻燃剂的制备方法,其特征在于所述步骤(4)反应物加热至90℃,直到无反应现象发生,时长为3h。
3.如权利要求1所述一种无甲醛耐久阻燃剂的制备方法,其特征在于所述步骤(7)反应温度为80℃,持续到无反应现象为止,时长为3h。
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CN107761377A (zh) * | 2017-10-17 | 2018-03-06 | 江苏尼美达科技有限公司 | 无卤无甲醛释放的棉用氮磷协同体系的耐久阻燃剂的合成与应用 |
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CN107761377A (zh) * | 2017-10-17 | 2018-03-06 | 江苏尼美达科技有限公司 | 无卤无甲醛释放的棉用氮磷协同体系的耐久阻燃剂的合成与应用 |
CN107761377B (zh) * | 2017-10-17 | 2019-10-11 | 江苏尼美达科技有限公司 | 无卤无甲醛释放的棉用氮磷协同体系的耐久阻燃剂的合成与应用 |
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