CN105949432B - 一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料 - Google Patents
一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料 Download PDFInfo
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- CN105949432B CN105949432B CN201610321821.4A CN201610321821A CN105949432B CN 105949432 B CN105949432 B CN 105949432B CN 201610321821 A CN201610321821 A CN 201610321821A CN 105949432 B CN105949432 B CN 105949432B
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- insulating material
- polyurethane foam
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Abstract
本发明提供的一种改性煤矸石‑硬质聚氨酯泡沫塑料复合保温材料,由以下重量份的组份制成:改性煤矸石、4,4'‑二环己基甲烷二异氰酸酯、聚酯多元醇、聚醚多元醇、含羟基的低分子量化合物、改性纳米氢氧化铝、发泡剂、有机硅泡沫稳定剂、微晶纤维素、复合催化剂、发泡剂、阻燃剂、水。本发明提供的复合保温材料制备工艺简单、成本低廉,阻燃性能好、保温效果好。
Description
技术领域
本发明涉及一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,属于材料科学领域。
背景技术
近几年来,利用墙体保温实现建筑节能已越来越被重视,国家也已经开始强制施行建筑节能措施,现在市场上大规模使用的保温材料主要有EPS(聚苯乙烯泡沫)、PS(挤塑聚苯乙烯泡沫)和PU(聚氨酯泡沫)。此类有机保温材料最大的优点是质轻、隔热、保温,但最大的缺陷是易燃烧、易老化、防火安全性差,在没有经过阻燃处理时都存在严重的火灾隐患,导致建筑火灾事故。聚氨酯硬泡是一种易燃的有机保温材料,在燃烧时释放出大量的有毒气体和烟雾,对人们的生命财产安全造成严重的威胁,因此,如果不能有效、切实的解决其易燃的防火安全性问题,那么硬质聚氨酯泡沫塑料就无法在我国建筑节能中获得大规模的推广应用。
硬质聚氨酯泡沫塑料的耐热、防火阻燃等问题成为迫切需要解决的重要课题,是关系到硬质聚氨酯泡沫塑料能否继续发展的关键因素之一。如何提高现有聚氨酯硬泡的耐热性并改善其阻燃性的研究以及大规模的推广应用已成为现阶段亟需解决的重要问题。
发明内容
发明目的:本发明的目的是提供一种阻燃性能好、保温效果好的改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料及其制备方法。
技术方案:本发明提供的一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,由以下重量份的组份制成:
作为优选,所述改性煤矸石采用以下方法制得:
(1)煤矸石的预处理:将煤矸石加入物质的量浓度为0.008~0.012mol/L的盐酸中浸泡8-12h,过滤后加入物质的量浓度为0.008~0.012mol/L的氢氧化钠中浸泡4-6h;
(2)将过量的癸二胺溶解于配制好的物质的量浓度为0.008~0.012mol/L的盐酸中,进行部分质子化后,癸二胺被部分质子化成一端仍带有活性-NH2基团的氨盐;
(3)将煤矸石加入部分质子化的癸二胺溶液中,置于50~60℃油浴里,用电动搅拌机搅拌2~4小时,转速为1500~2500r/min;煤矸石和部分质子化的癸二胺溶液的用量比为10g:100ml;
(4)抽滤,滤饼用蒸馏水清洗3~4次,烘干,研磨,过筛,即得改性煤矸石。
作为另一种优选,所述聚酯多元醇为分子量400-5000的聚碳酸酯二元醇或分子量为600-2000的芳烃聚酯多元醇。
作为另一种优选,所述聚醚多元醇为分子量为500-2000的芳香胺类聚醚多元醇或分子量为500-2000的山梨醇类聚醚多元醇。
作为另一种优选,所述含羟基的低分子量化合物为乙二醇。
作为另一种优选,所述复合催化剂为质量比3:2:1的三亚乙基二胺、2,4,6-三(二甲氨基甲基)苯酚和二丁基锡二月桂酸酯的混合物;所述阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲基-4-羟基苯甲醇。
作为另一种优选,所述改性纳米氢氧化镁是由纳米氢氧化镁经硅烷偶联剂KH-550湿法改性制得。
本发明还提供了上述一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料的制备方法,包括以下步骤:
(1)改性煤矸石的制备:
将过量的癸二胺溶解于配制好的物质的量浓度为0.008~0.012mol/L的盐酸中,进行部分质子化后,癸二胺被部分质子化成一端仍带有活性-NH2基团的氨盐;
将煤矸石加入部分质子化的癸二胺溶液中,置于50~60℃油浴里,用电动搅拌机搅拌2~4小时,转速为1500~2500r/min;煤矸石和部分质子化的癸二胺溶液的用量比为10g:100ml;
抽滤,滤饼用蒸馏水清洗3~4次,烘干,研磨,过筛,即得改性煤矸石;
(2)复合保温材料的制备:将聚酯多元醇和聚醚多元醇加热至100-120℃,混匀,冷却至70-80℃,得初混料;将含羟基的低分子量化合物、改性纳米氢氧化铝、发泡剂、有机硅泡沫稳定剂、微晶纤维素、复合催化剂、发泡剂、阻燃剂加入水中混合后,加入至初混料中,混匀;再加入改性煤矸石搅拌10-20min,最后加入4,4'-二环己基甲烷二异氰酸酯,搅拌1-3h;冷却,即得。
有益效果:本发明提供的复合保温材料制备工艺简单、成本低廉,阻燃性能好、保温效果好。
具体实施方式
根据下述实施例,可以更好地理解本发明。然而,本领域的技术人员容易理解,实施例所描述的具体的物料配比、工艺条件及其结果仅用于说明本发明,而不应当也不会限制权利要求书中所详细描述的本发明。
实施例1
改性煤矸石的制备,采用以下方法:
(1)煤矸石的预处理:将煤矸石加入物质的量浓度为0.010mol/L的盐酸中浸泡10h,过滤后加入物质的量浓度为0.010mol/L的氢氧化钠中浸泡5h;
(2)将过量的癸二胺溶解于配制好的物质的量浓度为0.010mol/L的盐酸中,进行部分质子化后,癸二胺被部分质子化成一端仍带有活性-NH2基团的氨盐;
(3)将煤矸石加入部分质子化的癸二胺溶液中,置于55℃油浴里,用电动搅拌机搅拌3小时,转速为2000r/min;煤矸石和部分质子化的癸二胺溶液的用量比为10g:100ml;(4)抽滤,滤饼用蒸馏水清洗3~4次,烘干,研磨,过筛,即得改性煤矸石。
实施例2
改性煤矸石的制备,采用以下方法:
(1)煤矸石的预处理:将煤矸石加入物质的量浓度为0.008mol/L的盐酸中浸泡12h,过滤后加入物质的量浓度为0.012mol/L的氢氧化钠中浸泡4h;
(2)将过量的癸二胺溶解于配制好的物质的量浓度为0.008mol/L的盐酸中,进行部分质子化后,癸二胺被部分质子化成一端仍带有活性-NH2基团的氨盐;
(3)将煤矸石加入部分质子化的癸二胺溶液中,置于50℃油浴里,用电动搅拌机搅拌4小时,转速为1500r/min;煤矸石和部分质子化的癸二胺溶液的用量比为10g:100ml;
(4)抽滤,滤饼用蒸馏水清洗3~4次,烘干,研磨,过筛,即得改性煤矸石。
实施例3
改性煤矸石的制备,采用以下方法:
(1)煤矸石的预处理:将煤矸石加入物质的量浓度为0.012mol/L的盐酸中浸泡8h,过滤后加入物质的量浓度为0.008mol/L的氢氧化钠中浸泡6h;
(2)将过量的癸二胺溶解于配制好的物质的量浓度为0.012mol/L的盐酸中,进行部分质子化后,癸二胺被部分质子化成一端仍带有活性-NH2基团的氨盐;
(3)将煤矸石加入部分质子化的癸二胺溶液中,置于60℃油浴里,用电动搅拌机搅拌2小时,转速为2500r/min;煤矸石和部分质子化的癸二胺溶液的用量比为10g:100ml;(4)抽滤,滤饼用蒸馏水清洗3~4次,烘干,研磨,过筛,即得改性煤矸石。
实施例4
改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,由以下重量份的组份制成:
其中,分子量400的聚碳酸酯二元醇;分子量为2000的芳香胺类聚醚多元醇;所述复合催化剂为质量比3:2:1的三亚乙基二胺、2,4,6-三(二甲氨基甲基)苯酚和二丁基锡二月桂酸酯的混合物;所述阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲基-4-羟基苯甲醇;所述改性纳米氢氧化镁是由纳米氢氧化镁经硅烷偶联剂KH-550湿法改性制得。
上述改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料的制备,包括以下步骤:
将聚酯多元醇和聚醚多元醇加热至110℃,混匀,冷却至75℃,得初混料;将含羟基的低分子量化合物、改性纳米氢氧化铝、发泡剂、有机硅泡沫稳定剂、微晶纤维素、复合催化剂、发泡剂、阻燃剂加入水中混合后,加入至初混料中,混匀;再加入改性煤矸石搅拌15min,最后加入4,4'-二环己基甲烷二异氰酸酯,搅拌2h;冷却,即得。
实施例5
改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,由以下重量份的组份制成:
其中,分子量5000的聚碳酸酯二元醇;分子量为2000的芳香胺类聚醚多元醇;所述复合催化剂为质量比3:2:1的三亚乙基二胺、2,4,6-三(二甲氨基甲基)苯酚和二丁基锡二月桂酸酯的混合物;所述阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲基-4-羟基苯甲醇;所述改性纳米氢氧化镁是由纳米氢氧化镁经硅烷偶联剂KH-550湿法改性制得。
上述改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料的制备,包括以下步骤:
将聚酯多元醇和聚醚多元醇加热至100℃,混匀,冷却至70℃,得初混料;将含羟基的低分子量化合物、改性纳米氢氧化铝、发泡剂、有机硅泡沫稳定剂、微晶纤维素、复合催化剂、发泡剂、阻燃剂加入水中混合后,加入至初混料中,混匀;再加入改性煤矸石搅拌10min,最后加入4,4'-二环己基甲烷二异氰酸酯,搅拌3h;冷却,即得。
实施例6
改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,由以下重量份的组份制成:
其中,分子量为600的芳烃聚酯多元醇;分子量为2000的山梨醇类聚醚多元醇;所述复合催化剂为质量比3:2:1的三亚乙基二胺、2,4,6-三(二甲氨基甲基)苯酚和二丁基锡二月桂酸酯的混合物;所述阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲基-4-羟基苯甲醇;所述改性纳米氢氧化镁是由纳米氢氧化镁经硅烷偶联剂KH-550湿法改性制得。
上述改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料的制备,包括以下步骤:
将聚酯多元醇和聚醚多元醇加热至120℃,混匀,冷却至80℃,得初混料;将含羟基的低分子量化合物、改性纳米氢氧化铝、发泡剂、有机硅泡沫稳定剂、微晶纤维素、复合催化剂、发泡剂、阻燃剂加入水中混合后,加入至初混料中,混匀;再加入改性煤矸石搅拌20min,最后加入4,4'-二环己基甲烷二异氰酸酯,搅拌1h;冷却,即得。
实施例7
改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,由以下重量份的组份制成:
其中,分子量为2000的芳烃聚酯多元醇;分子量为500的山梨醇类聚醚多元醇;所述复合催化剂为质量比3:2:1的三亚乙基二胺、2,4,6-三(二甲氨基甲基)苯酚和二丁基锡二月桂酸酯的混合物;所述阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲基-4-羟基苯甲醇;所述改性纳米氢氧化镁是由纳米氢氧化镁经硅烷偶联剂KH-550湿法改性制得。
上述改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料的制备,包括以下步骤:
将聚酯多元醇和聚醚多元醇加热至115℃,混匀,冷却至75℃,得初混料;将含羟基的低分子量化合物、改性纳米氢氧化铝、发泡剂、有机硅泡沫稳定剂、微晶纤维素、复合催化剂、发泡剂、阻燃剂加入水中混合后,加入至初混料中,混匀;再加入改性煤矸石搅拌15min,最后加入4,4'-二环己基甲烷二异氰酸酯,搅拌2h;冷却,即得。
测试实施例4至7的性能。
表1
其中,对比例为市售硬质聚氨酯泡沫塑料。
由上表可知,本发明产品具有较高的的压缩强度、泡孔细腻、具有较低的导热系数、泡沫的阻燃性能好。
Claims (6)
1.一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,其特征在于:由以下重量份的组份制成:
改性煤矸石 5-10份;
4,4'-二环己基甲烷二异氰酸酯 40-50份;
聚酯多元醇 20-30份;
聚醚多元醇 10-20份;
含羟基的低分子量化合物 5-10份;
改性纳米氢氧化铝 5-10份;
发泡剂 10-20份;
有机硅泡沫稳定剂 1-3份;
微晶纤维素 1-3份;
复合催化剂 1-3份;
发泡剂 1-3份;
阻燃剂 1-3份;
水 5-15份。
2.根据权利要求1所述的一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,其特征在于:所述改性煤矸石采用以下方法制得:
(1) 煤矸石的预处理:将煤矸石加入物质的量浓度为0.008~0.012mol/L的盐酸中浸泡8-12h,过滤后加入物质的量浓度为0.008~0.012mol/L的氢氧化钠中浸泡4-6h;
(2) 将过量的癸二胺溶解于配制好的物质的量浓度为0.008~0.012mol/L的盐酸中,进行部分质子化后,癸二胺被部分质子化成一端仍带有活性-NH2基团的氨盐;
(3) 将步骤(1)预处理后的煤矸石加入部分质子化的癸二胺溶液中,置于50~60℃油浴里,用电动搅拌机搅拌2~4小时,转速为1500~2500r/min;煤矸石和部分质子化的癸二胺溶液的用量比为10g:100ml;
(4) 抽滤,滤饼用蒸馏水清洗 3~4次,烘干,研磨,过筛,即得改性煤矸石。
3.根据权利要求1所述的一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,其特征在于:所述聚酯多元醇为分子量400-5000的聚碳酸酯二元醇或分子量为600-2000的芳烃聚酯多元醇。
4.根据权利要求1所述的一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,其特征在于:所述聚醚多元醇为分子量为500-2000的芳香胺类聚醚多元醇或分子量为500-2000的山梨醇类聚醚多元醇。
5.根据权利要求1所述的一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,其特征在于:所述含羟基的低分子量化合物为乙二醇。
6.根据权利要求1所述的一种改性煤矸石-硬质聚氨酯泡沫塑料复合保温材料,其特征在于:所述复合催化剂为质量比3:2:1的三亚乙基二胺、2,4,6-三(二甲氨基甲基)苯酚和二丁基锡二月桂酸酯的混合物;所述阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲基-4- 羟基苯甲醇。
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CN108610721B (zh) * | 2018-05-17 | 2020-12-01 | 东莞市大兴化工有限公司 | 阻燃改性聚氨酯固化剂及制备方法和双组份聚氨酯涂料 |
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