CN111876123B - 阻燃型聚氨酯胶黏剂及其制备方法 - Google Patents
阻燃型聚氨酯胶黏剂及其制备方法 Download PDFInfo
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- CN111876123B CN111876123B CN202010621763.3A CN202010621763A CN111876123B CN 111876123 B CN111876123 B CN 111876123B CN 202010621763 A CN202010621763 A CN 202010621763A CN 111876123 B CN111876123 B CN 111876123B
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Classifications
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
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- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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Abstract
本发明属于胶粘材料技术领域,公开了一种耐酸防腐蚀阻燃型聚氨酯胶黏剂及其制备方法,制备方法是:将端羟基液体橡胶与部分耐腐蚀填料混合,再加入抗氧剂、扩链剂、聚烯烃、阻燃剂混合均匀,得到预混料;将剩余的耐腐蚀填料与聚酯多元醇混合升温,抽真空条件下与预混料混合,加入吸水剂,密封出料,得到A组分;将多异氰酸酯固化剂分装即可得到B组分。本发明的胶黏剂固化后具有良好的力学性能和耐酸腐蚀性能、阻燃性能,且产品制备方法简单。
Description
技术领域
本发明涉及一种胶粘材料,尤其是一种用于防腐尤其是烟囱防腐的阻燃型聚氨酯胶黏剂及其制备方法。
背景技术
目前国内电厂烟囱多采用废玻璃泡沫玻璃砖进行的湿烟囱防腐,但大约80%会在1年内出现渗漏,主要原因在于玻璃砖和胶粘剂质量不能满足技术要求。湿烟囱防腐条件苛刻,包括:酸液的浓度大,实际提取的酸液样品PH值接近1;在容易积液的地方,随着酸液中水分的挥发,浓度越来越大;酸液的组成复杂,含有硫酸,还含有微量的硝酸、盐酸和氢氟酸,对材料的腐蚀性都非常强。泡沫玻璃砖防腐隔热系统由泡沫玻璃砖和胶粘剂组成,应用中要求胶粘剂具有很好的弹性、抗酸腐蚀性能和耐高温、抗疲劳、抗老化性能,其对泡沫玻璃砖防腐系统运行的稳定性起到主导作用。
发明内容
为了解决上述现有技术存在的问题,本发明提供一种阻燃型聚氨酯胶黏剂及其制备方法,该材料用于防腐尤其是烟囱防腐,具有优异的阻燃和抗酸腐蚀性能,用于烟囱防腐可以有效提高防腐可靠性及安全性,且制备方法简单。
本发明采用的技术方案是:
一种阻燃型聚氨酯胶黏剂,由A、B组分组成,其中A组分包括以下按重量份数计的组分:
A组分的总重量份数为100份;
B组分为多异氰酸酯固化剂。
所述端羟基液体橡胶是具有活性端羟基、主链为聚丁二烯、聚苯乙烯等的液体橡胶,其与聚酯多元醇等经固化交联形成耐腐蚀层,共同发挥耐腐蚀的作用。优选的,所述端羟基液体橡胶为端羟基液体丁腈橡胶、端羟基聚异丁烯液体橡胶、端羟基液体聚丁二烯、端羟基丁苯液体橡胶中的一种或几种。优选的,所述端羟基液体橡胶的数均分子量为500-6000,羟值为(10-120)mgKOH/g。进一步优选的所述端羟基液体橡胶的数均分子量为1000-5000,羟值为30-100mgKOH/g。
所述聚酯多元醇为脂肪族聚酯多元醇、芳香族聚酯多元醇、聚碳酸酯聚酯多元醇及聚己内酯多元醇中的一种或几种,用于制备所述脂肪族聚酯多元醇的多元醇优选为乙二醇、丙二醇、丁二醇、新戊二醇、二甘醇中的一种或几种,所述脂肪族聚酯多元醇优选为己二酸聚酯二醇或丁二酸聚酯二醇,更优选其数均分子量为500-5000,羟值为10-250mgKOH/g;所述芳香族聚酯多元醇优选为邻苯二甲酸聚酯二醇、对苯二甲酸聚酯二醇或间苯二甲酸聚酯二醇,更优选其数均分子量为1000-5000,羟值为10-120mgKOH/g;所述聚己内酯多元醇优选其数均分子量为800-3000,羟值为(10-400)mgKOH/g。
优选的,所述聚酯多元醇包括聚己内酯多元醇,进一步优选的聚酯多元醇中聚己内酯多元醇的质量百分数为20-100%,聚己内酯多元醇在本发明的方案中能够有效提高胶黏剂的耐酸腐蚀和耐温性能。
所述聚烯烃利于提高胶黏剂固化后胶层的力学性能,选自聚丙烯、聚丁烯、三元乙丙橡胶、聚异丁烯中的一种或几种,优选的,所述聚烯烃包括聚异丁烯,更优选聚烯烃中聚异丁烯的质量百分数为20-100%。优选的,所述聚烯烃25℃条件下为粘稠液态,其粘度为50000-300000cps。
所述扩链剂为山梨糖醇酸酯和/或二元醇,用于调节胶黏剂固化后的力学性能,所述山梨糖醇酸酯为山梨糖醇酐单油酸酯、山梨醇酐单月桂酸酯、山梨糖醇酐单棕榈酸酯中的一种或几种,所述二元醇为1,4丁二醇、1,6己二醇、1,3丙二醇、对苯二酚二(2羟乙基)醚、1,4环己二醇中的一种或几种。
优选的,所述扩链剂为山梨糖醇酸酯和二元醇的混合物,所述山梨糖醇酸酯与二元醇的质量比为1:(1-3)。
所述吸水剂用于清除反应体系中的水分,没有特殊限制,优选为恶唑烷类水分清除剂或分子筛。
所述抗氧剂具体为四(3,5-二叔丁基-4-羟基)苯丙酸季戊四醇酯(1010)、N,N'-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰]肼(1024)、硫代二乙撑双[3-(3,5-二叔丁基-4-羟基苯基)丙酸酯](1035)、N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺(1098)、双(2,4-二叔丁基苯基)季戊四醇二亚磷酸酯(626)、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯(1076)、二亚磷酸季戊四醇二硬脂醇酯(618)、三乙二醇醚-二(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯(245)、亚磷酸三(2,4-二叔丁基苯基)酯(168)、3,5-二叔丁基-4-羟基苯丙酸异辛酯(1135)中的至少一种或几种的混合物。
所述耐腐蚀填料为云母、滑石粉、硫酸钡、玻璃微珠、玻璃片、硅微粉、短切玻璃纤维、短切碳纤维、石墨中的一种或几种。优选的,所述耐腐蚀填料的平均粒径≤60μm。
所述阻燃剂没有特殊限制,优选为氢氧化镁、氢氧化铝、三氧化二锑、三羟甲基氧化膦、三羟丙基氧化膦、十溴二苯乙烷中的一种或多种,优选的为三羟甲基氧化膦、三氧化二锑与十溴二苯乙烷的混合物。
所述多异氰酸酯固化剂为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯甲烷-4,4′-二异氰酸酯或多亚甲基多苯基多异氰酸酯,其用量以能够使A组分完全固化即可。
优选的,所述A组分的37℃动力粘度为2000-150000mPa.s。
本发明所述阻燃型聚氨酯胶黏剂的制备方法,包括以下步骤:
将端羟基液体橡胶与部分耐腐蚀填料混合,再加入抗氧剂、扩链剂、聚烯烃、阻燃剂混合,得到预混料;将剩余的耐腐蚀填料与聚酯多元醇混合升温,抽真空条件下与预混料混合,加入吸水剂,密封出料,得到A组分;将多异氰酸酯固化剂分装即可得到B组分。
本发明阻燃型聚氨酯胶黏剂的制备方法中,优选的,所述部分耐腐蚀填料的质量为耐腐蚀填料总质量的15-70%。
优选的,所述将剩余的耐腐蚀填料与聚酯多元醇混合升温是升温至80-100℃。
优选的,所述抽真空条件下是通过抽真空除去水分,具体是在80-100℃抽真空并保持真空度为-0.08~-0.1MPa,同时保持搅拌状态,时间为2-4h。所述加入吸水剂是降温至60℃以下,再加入吸水剂。
本发明的技术方案具有以下有益效果:
本发明采用特殊组成的基础聚合物及耐腐蚀填料制备得到胶黏剂,具有良好的力学性能、阻燃性能和耐酸腐蚀性能,产品固化后经80℃混酸浸泡15d×24h(混酸为H2SO4质量百分数为2%、HCl质量百分数为0.1%、HNO3质量百分数为0.1%和H3PO4质量百分数为0.1%的水溶液)拉伸强度保持率大于80%、断裂伸长率保持率大于60%,用于烟囱防腐可以有效提高防腐耐久性以及安全性,且产品制备方法简单。
具体实施方式
以下所述是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和演变,这些改进和演变也视为本发明的保护范围。
实施例1
阻燃型聚氨酯胶黏剂包括A组分和B组分,制备方法如下:
将30kg端羟基聚丁二烯(HTPBШ型,黎明化工研究院,羟值38mgKOH/g,分子量1800-3500)与10kg石英粉(604,矽比科矿业有限公司,平均粒径(D50)为15μm)投入搅拌装置混合15分钟,加入3kg三羟甲基氧化膦、10kg三氧化二锑与10kg十溴二苯乙烷,2kg抗氧剂Irganox 1010、2kg扩链剂Span80(广东润华化工有限公司,羟值200mgKOH/g)、10kg聚异丁烯(PB4000,韩国大林,分子量4000)再混合15分钟,得到预混料;将7kg耐腐蚀填料硫酸钡(XLT-3,贵州新力拓矿业有限责任公司,600目)与15kg聚己内酯二醇(L330AL,日本化学工业株式会社大赛璐,3000分子量,羟值56mgKOH/g)混合升温至90℃,再与预混料混合,高速搅拌并在90℃抽真空至-0.09mpa,持续搅拌2h;降温至60℃条件下加入1kg吸水剂(ALT-202,安乡艾利特化工有限公司产品),混合均匀后密封出料,得到A组分;环境湿度在60%以下条件下取10kg多亚甲基多苯基多异氰酸酯固化剂(PM-200,烟台万华集团产品)密封包装,得到B组分。
实施例2
阻燃型聚氨酯胶黏剂包括A组分和B组分,制备方法如下:
将10kg端羟基聚丁二烯(HTPBШ型,黎明化工研究院,羟值38mgKOH/g,分子量1800-3500)与15kg硅微粉(604,矽比科矿业有限公司,粒径(D50)为15μm)投入搅拌装置混合15分钟,加入阻燃剂5kg三羟甲基氧化膦、6kg三氧化二锑与14kg十溴二苯乙烷、2kg抗氧剂Irganox 1010、2kg Span80(广东润华化工有限公司,羟值200mgKOH/g)、3kg 1,4-丁二醇(巴斯夫)、5kg三元乙丙橡胶(EV-30,东莞骏松塑胶,分子量45000,25℃动力粘度值为200000cps)、10kg聚异丁烯(吉林石化,分子量3000)再混合15分钟,得到预混料;将20kg硅微粉(604,矽比科矿业有限公司)与5kg聚己内酯二醇(CAPA2200,瑞典Perstorp集团公司,分子量2000,羟值56mgKOH/g)混合升温至100℃,再与预混料混合,高速搅拌并在100℃抽真空至-0.09mpa,持续搅拌2h;降温至60℃及抽真空条件下加入3kg吸水剂(ALT-202,安乡艾利特化工有限公司),混合均匀后密封出料,得到A组分;环境湿度在60%以下条件下取10kg多亚甲基多苯基多异氰酸酯(PM-200,烟台万华集团产品)固化剂密封包装,得到B组分。
实施例3
阻燃型聚氨酯胶黏剂包括A组分和B组分,制备方法如下:
将25kg端羟基聚丁二烯(HTPB Poly bd R-45HT,日本出光兴产株式会社,分子量2800,羟值46mgKOH/g)与15kg硅微粉(604,矽比科矿业有限公司,粒径(D50)为15μm)投入搅拌装置混合15分钟,加入阻燃剂7kg三氧化二锑与13kg十溴二苯乙烷、3kg抗氧剂Irganox1010、1kg扩链剂1,4-丁二醇(天津中和盛泰化工有限公司)、2kgSpan80(广东润华化工有限公司,羟值200mgKOH/g)、5kg三元乙丙橡胶(EV-30,东莞骏松塑胶,分子量45000,25℃粘度值200000cps)、5kg聚异丁烯(PB2400,韩国大林产,分子量2400,100℃粘度4500cps)再混合15分钟,得到预混料;将10kg耐腐蚀填料硫酸钡(XLT-3,贵州新力拓矿业有限责任公司,600目)与8kg聚己内酯二醇(CAPA2200,瑞典Perstorp集团公司,分子量2000,羟值56mgKOH/g),3kg聚己二酸丁二醇酯XCP-1044(旭川化学,分子量1000,羟值110mgKOH/g)混合升温至80℃,再与预混料混合,高速搅拌并在80℃抽真空至-0.09mpa,持续搅拌2h;降温至60℃及抽真空条件下加入3kg吸水剂(MS-PLUS,陶氏化学产品),混合均匀后密封出料,得到A组分;环境湿度在60%以下条件下取10kg多亚甲基多苯基多异氰酸酯固化剂(PM-200,烟台万华集团产品)密封包装,得到B组分。
实施例4
阻燃型聚氨酯胶黏剂包括A组分和B组分,制备方法如下:
将15kg端羟基聚丁二烯(HTPB Poly bd R-45HT,日本出光兴产株式会社,分子量2800,羟值46mgKOH/g)与15kg硅微粉(606,矽比科矿业有限公司,粒径(D50)为6μm)投入搅拌装置混合15分钟,加入阻燃剂15kg三羟甲基氧化膦、3kg抗氧剂Irganox 1010、2kg扩链剂1,4-丁二醇(天津中和盛泰化工有限公司)、5kg三元乙丙橡胶(CP-1100,日本住友,分子量12000,40℃粘度为22500cst)、12kg聚异丁烯(吉林石化,分子量3000)再混合15分钟,得到预混料;将15kg耐腐蚀填料硫酸钡XLT-3(贵州新力拓矿业有限责任公司,600目)与12kg聚己内酯二醇(L330AL,日本化学工业株式会社大赛璐,3000分子量,羟值56mgKOH/g),4kg聚己二酸丁二醇酯XCP-1044(旭川化学,分子量1000,羟值110mgKOH/g)混合升温至90℃,再与预混料混合,高速搅拌并在90℃抽真空至-0.09mpa,真空度-0.09mpa条件下持续搅拌2h;降温至60℃及真空度-0.09mpa条件下加入2kg吸水剂(MS-PLUS,陶氏化学产品),混合均匀后密封出料,得到A组分;环境湿度在60%以下条件下取10kg多亚甲基多苯基多异氰酸酯固化剂(Desmodur VK 5,德国Bayer公司)密封包装,得到B组分.
实施例5
阻燃型聚氨酯胶黏剂包括A组分和B组分,制备方法如下:
将5kg端羟基丁腈液体橡胶(羟值20mgKOH/g,分子量5200)、20kg端羟基聚丁二烯(HTPBШ型,黎明化工研究院,羟值38mgKOH/g,分子量1800-3500)与10kg石英粉(604,矽比科矿业有限公司,平均粒径(D50)为15μm)投入搅拌装置混合15分钟,加入阻燃剂10kg三氧化二锑与20kg十溴二苯乙烷、3kg抗氧剂Irganox 1010、1kg扩链剂Span80(广东润华化工有限公司,羟值200mgKOH/g)、10kg聚异丁烯(PB4000,韩国大林,分子量4000)再混合15分钟,得到预混料;将5kg耐腐蚀填料硫酸钡(XLT-3,贵州新力拓矿业有限责任公司,600目)与20kg聚己内酯二醇(L330AL,日本化学工业株式会社大赛璐,3000分子量,羟值56mgKOH/g)混合升温至90℃,再与预混料混合,高速搅拌并在90℃抽真空至-0.09mpa,持续搅拌2h;抽真空及降温至60℃条件下加入1kg吸水剂(ALT-202,安乡艾利特化工有限公司产品),混合均匀后密封出料,得到A组分;环境湿度在60%以下条件下取10kg多亚甲基多苯基多异氰酸酯固化剂(PM-200,烟台万华集团产品)密封包装,得到B组分.
测试实施例
对实施例1-5制备的阻燃型聚氨酯胶黏剂的A组分进行粘度测试:参考标准:GB/T2794-1995,取A组分调节其温度为37℃,用博勒飞粘度计测试A组分在37℃的粘度。
对实施例1~5制备得到的阻燃型聚氨酯胶黏剂以及对比的防腐蚀胶黏剂(宾高德内衬胶黏剂,以下简称对比胶黏剂)做以下性能测试:
1、将A、B组分混合均匀后抽真空排泡,倒入磨具内室温固化7×24h,固化块厚度大于6mm,固化后用邵A硬度计测试邵氏硬度,测试方法为:GB/T531-1999。
2、将A、B组分混合均匀后均匀涂布在脱脂处理过的铝板表面,将涂布了胶黏剂的铝板表面平行搭接,搭接面积25×15mm,室温放置固化7×24h,用万能拉力测试仪测试剪切强度(Mpa),测试方法参考GB/T 50212。
3、将A、B组分混合均匀,倒入磨具内室温固化7×24h,裁切成规定规格测试条,测试拉伸强度(Mpa),参考ASTM D412。
4、将A、B组分混合均匀,倒入磨具内室温固化7×24h,裁切成规定规格测试条,测试断裂伸长率,参考ASTM D412。
5、耐热性能:将A、B组分混合均匀,倒入磨具内室温固化7×24h后进行热老化实验,热老化条件为120℃×24h,测试老化前后的拉伸强度、断裂伸长率保持率,拉伸强度、断裂伸长率测试方法参照4、5.
6、耐酸腐蚀性能:将A、B组分混合均匀,倒入磨具内室温固化7×24h后,裁切成拉伸强度、断裂伸长率测试方法规定规格的测试条,进行耐酸腐蚀处理后测试,具体是将测试条放入80℃混酸浸泡15d×24h(混酸为H2SO4质量百分数为2%、HCl质量百分数为0.1%、HNO3质量百分数为0.1%和H3PO4质量百分数为0.1%的水溶液)后取出,参照4、5分别测试拉伸强度、断裂伸长率,与未进行耐酸腐蚀处理时的性能对比,计算得到拉伸强度、断裂伸长率的保持率。
7、阻燃测试:根据标准ANSI/UL 94-1985制备样品,按照UL94垂直燃烧测试标准测试阻燃等级。
测试数据列于表1。
表1
由表1数据可见,本发明的胶黏剂产品具有优异的阻燃及耐酸腐蚀性能,用于烟囱防腐中性能水平与进口产品相当,应用前景良好。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单推演或替换,都应当视为属于本发明的保护范围。
Claims (7)
2.如权利要求1所述的阻燃型聚氨酯胶黏剂,其特征在于,所述聚酯多元醇为脂肪族聚酯多元醇、芳香族聚酯多元醇、聚碳酸酯聚酯多元醇及聚己内酯多元醇中的一种或几种。
3.如权利要求2所述的阻燃型聚氨酯胶黏剂,其特征在于,所述聚酯多元醇包括聚己内酯多元醇,所述聚酯多元醇中聚己内酯多元醇的质量百分数为20-100%。
4.如权利要求1所述的阻燃型聚氨酯胶黏剂,其特征在于,所述聚烯烃包括聚异丁烯,所述聚烯烃中聚异丁烯的质量百分数为20-100%。
5.如权利要求1-3任一项所述的阻燃型聚氨酯胶黏剂,其特征在于,所述阻燃剂为三羟甲基氧化膦、三氧化二锑与十溴二苯乙烷的混合物。
6.如权利要求1-3任一项所述的阻燃型聚氨酯胶黏剂的制备方法,包括以下步骤:
将端羟基液体橡胶与部分耐腐蚀填料混合,再加入抗氧剂、扩链剂、聚烯烃、阻燃剂混合,得到预混料;将剩余的耐腐蚀填料与聚酯多元醇混合升温,抽真空条件下与预混料混合,加入吸水剂,密封出料,得到A组分;将多异氰酸酯固化剂分装即可得到B组分。
7.如权利要求6所述的阻燃型聚氨酯胶黏剂的制备方法,其特征在于,所述部分耐腐蚀填料的质量为耐腐蚀填料总质量的15-70%。
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