CN109666177A - 一种含有酯化改性ac发泡剂的发泡材料及其制备方法 - Google Patents

一种含有酯化改性ac发泡剂的发泡材料及其制备方法 Download PDF

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CN109666177A
CN109666177A CN201811500938.4A CN201811500938A CN109666177A CN 109666177 A CN109666177 A CN 109666177A CN 201811500938 A CN201811500938 A CN 201811500938A CN 109666177 A CN109666177 A CN 109666177A
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foaming agent
esterification modification
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葛铁军
唐昊洋
赵越
毛洪雨
吴美珊
刘晓洋
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Shenyang University of Chemical Technology
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Abstract

一种含有酯化改性AC发泡剂的发泡材料及其制备方法,涉及一种发泡材料及其制备方法,酯化改性的AC发泡剂,偶氮二甲酰胺在氢氧化钠的水溶液中水解生成偶氮二甲酸钠盐,在相转移催化剂等作用下偶氮二甲酸钠盐在水溶液中与硫酸二甲酯反应,生成酯化改性AC发泡剂,该发泡剂的结构式如下:

Description

一种含有酯化改性AC发泡剂的发泡材料及其制备方法
技术领域
本发明涉及一种发泡材料及其制备方法,特别是涉及一种含有酯化改性AC发泡剂的发泡材料及其制备方法。
背景技术
发泡材料质量轻,具备缓冲、吸音、吸震、保温、过滤等功能,广泛应用于电子、家电、汽车、体育休闲等行业。由于用途广泛,与国民经济的基础行业息息相关,多年来一直保持20%左右的稳定持续的增长。
偶氮二甲酰胺是一种通用型发气量大的发泡剂。广泛用于聚氯乙烯、聚乙烯、乙烯-乙酸乙烯共聚物、聚丙烯、聚苯乙烯、ABS、尼龙-6和氯丁橡胶等多种合成材料,至今还没有能与竞争的产品出现。然而偶氮二甲酰胺(AC)分解温度在200~210℃,许多材料加工温度低于AC的分解温度,因此需要对其进行改性。本发明从偶氮二甲酰胺结构上引入烷氧基取代氨基,降低了N—C键电子云密度,重叠程度减小,导致N—C键易断裂,故所制得的发泡剂活性提高,分解温度降低,且发泡量提高,使得分解温度在加工范围内并提高发泡材料的发泡度。
发明内容
本发明的目的在于提供一种含有酯化改性AC发泡剂的发泡材料及其制备方法,本发明在偶氮二甲酰胺结构中引入烷氧基,降低了N—C键电子云密度,重叠程度减小,导致N—C键易断裂,故所制得的发泡剂活性提高,发泡量提高,使得其分解温度在加工范围内并提高发泡材料发泡度。
本发明的目的是通过以下技术方案实现的:
一种含有酯化改性AC发泡剂的发泡材料,酯化改性的AC发泡剂,偶氮二甲酰胺在氢氧化钠的水溶液中水解生成偶氮二甲酸钠盐,在相转移催化剂等作用下偶氮二甲酸钠盐在水溶液中与硫酸二甲酯反应, 生成酯化改性AC发泡剂,该发泡剂的结构式如下:
所述的一种含有酯化改性AC发泡剂的发泡材料,按质量重量份计,包括有:基体材料 100份;发泡剂 1~3份;其他助剂 1~5份。
所述的一种含有酯化改性AC发泡剂的发泡材料,所述的基体材料为PP或ABS。
所述的一种含有酯化改性AC发泡剂的发泡材料,所述发泡剂为酯化改性AC发泡剂。
所述的一种含有酯化改性AC发泡剂的发泡材料,所述其他助剂为白油、抗氧剂、热稳定剂和光稳定剂中的一种或多种。
一种含有酯化改性AC发泡剂的发泡材料制备方法,所述制备方法,包括以下步骤:
A、偶氮二甲酰胺在氢氧化钠的水溶液中水解生成偶氮二甲酸钠盐,在相转移催化剂等作用下偶氮二甲酸钠盐在水溶液中与硫酸二甲酯反应, 生成酯化改性AC发泡剂;
B、按质量分数称取100份基体材料,2份发泡剂,5份其他助剂混合后放入高速混合机中混合6~8min混合均匀;
C、将混合后的物料注塑机注射。
所述的一种含有酯化改性AC发泡剂的发泡材料制备方法,注塑机的注塑温度控制在170℃-190℃之间。
本发明的优点与效果是:
本发明发泡是使材料具备轻量化、缓冲、吸音、吸震、保温、过滤等功能的一种有效途径,偶氮二甲酰胺发泡工艺应用范围广,可实现大批量生产,满足市场的工业化要求和可持续发展,因此,针对现有技术的缺陷本方法通过用含有酯化改性AC发泡剂的制备发泡材料,达到提高偶氮二甲酰胺活性,降低分解温度,提高发气量,从而使得发泡剂分解温度在生产温度范围内并提高材料的发泡度。
本发明发泡剂是酯化的AC发泡剂,偶氮二甲酰胺在氢氧化钠的水溶液中水解生成偶氮二甲酸钠盐,在相转移催化剂等作用下偶氮二甲酸钠盐在水溶液中与硫酸二甲酯反应,生成酯化改性新型发泡剂。本发明从偶氮二甲酰胺结构上引入烷氧基取代氨基,降低了N—C键电子云密度,重叠程度减小,导致N—C键易断裂,故所制得的发泡剂活性提高,分解温度降低,且发泡量提高,使得分解温度在加工范围内并提高发泡材料的发泡度。具体改性方法是:向装有机械搅拌器、回流冷凝管、恒压滴液漏斗、温度计的的四口烧瓶中加入偶氮二甲酰胺,氢氧化钠 ,水。在油浴中加热回流,用稀盐酸水溶液吸收产生的氨气。至氨气不再产生,停止加热,得到澄清无色水溶液。取硫酸二甲酯加人恒压滴液漏斗中在机械搅拌下缓慢滴加,滴加过程中控制反应温度在30℃以下,保持pH值=9~10,待滴加完毕,升温至55℃反应3 h制得新型发泡剂。把各组份按配比称取,于高速搅拌机中混合6~8分钟,出料,将混合料的原料置于注塑机注射,注塑机温度控制在170-190℃之间,制备样条,按相应的标准测试新型发泡剂较AC发泡剂发泡度有明显提高,并且其它力学性能并无明显影响,本发明实现了酯化改性AC发泡剂对可发材料的发泡度效果的提高。
附图说明
图1为本发明发泡剂的方程式。
具体实施方式
下面结合实施例对本发明进行详细说明。
本发明的实施过程:向装有机械搅拌器、回流冷凝管、恒压滴液漏斗、温度计的的四口烧瓶中加入偶氮二甲酰胺,氢氧化钠 ,水。在油浴中加热回流,用稀盐酸水溶液吸收产生的氨气。至氨气不再产生,停止加热,得到澄清无色水溶液。取硫酸二甲酯加人恒压滴液漏斗中在机械搅拌下缓慢滴加,滴加过程中控制反应温度在30℃以下,保持pH值=9~10,待滴加完毕,升温至55℃反应3 h制得新型发泡剂。
实施例1-3,各实施例中各组份的重量分配比如表1 所示。把各组份按配比称取,于高速搅拌机中混合6~8分钟,出料,将混合料的原料置于注塑机注射,注塑机温度控制在170-190℃之间,制备样条,按相应的标准测试(见表2),性能结果见表3。
表1 :实施例1-3 的配方组成(份)
表2 :力学性能测试标准
表3 :实施例1 -3 中PP回料的力学性能测试
从表3 实施例1-3 以及对比例1的性能测试结果,我们可知:新型发泡剂较AC发泡剂发泡度有明显提高,并且其它力学性能并无明显影响,这种方法实现了酯化改性AC发泡剂对可发材料的发泡度的提高效果。
以上通过具体实施例对本发明进行了进一步说明,不过这些实施例仅是范例性的,并不对本发明的保护范围构成任何限制。本领域技术人员理解,在不超出本发明的精神和保护范围的情况下,可以对本发明的技术方案及其实施方式进行多种等价替换、修饰或改进,这些均应落入本发明的保护范围内。本发明的保护范围以所附的权利要求为准。

Claims (7)

1.一种含有酯化改性AC发泡剂的发泡材料,其特征在于,酯化改性的AC发泡剂,偶氮二甲酰胺在氢氧化钠的水溶液中水解生成偶氮二甲酸钠盐,在相转移催化剂等作用下偶氮二甲酸钠盐在水溶液中与硫酸二甲酯反应, 生成酯化改性AC发泡剂,该发泡剂的结构式如下:
2.根据权利要求1所述的一种含有酯化改性AC发泡剂的发泡材料,其特征在于,按质量重量份计,包括有:基体材料 100份;发泡剂 1~3份;其他助剂 1~5份。
3.根据权利要求1所述的一种含有酯化改性AC发泡剂的发泡材料,其特征在于,所述的基体材料为PP或ABS。
4.根据权利要求1所述的一种含有酯化改性AC发泡剂的发泡材料,其特征在于,所述发泡剂为酯化改性AC发泡剂。
5.根据权利要求1所述的一种含有酯化改性AC发泡剂的发泡材料,其特征在于,所述其他助剂为白油、抗氧剂、热稳定剂和光稳定剂中的一种或多种。
6.一种含有酯化改性AC发泡剂的发泡材料制备方法,其特征在于,所述制备方法,包括以下步骤:
A、偶氮二甲酰胺在氢氧化钠的水溶液中水解生成偶氮二甲酸钠盐,在相转移催化剂等作用下偶氮二甲酸钠盐在水溶液中与硫酸二甲酯反应, 生成酯化改性AC发泡剂;
B、按质量分数称取100份基体材料,2份发泡剂,5份其他助剂混合后放入高速混合机中混合6~8min混合均匀;
C、将混合后的物料注塑机注射。
7.根据权利要求6所述的一种含有酯化改性AC发泡剂的发泡材料制备方法,其特征在于,注塑机的注塑温度控制在170℃-190℃之间。
CN201811500938.4A 2018-12-10 2018-12-10 一种含有酯化改性ac发泡剂的发泡材料及其制备方法 Pending CN109666177A (zh)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020143061A1 (en) * 2000-04-13 2002-10-03 Pitzele Barnett S. 2-amino-5, 6 heptenoic acid derivatives useful as nitric oxide synthase inhibitors
CN102898327A (zh) * 2012-10-26 2013-01-30 山东师范大学 偶氮二甲酸二甲酯及其中间体的合成方法
CN103012215A (zh) * 2013-01-22 2013-04-03 山东师范大学 偶氮二甲酸二烷基酯的制备方法
CN103193686A (zh) * 2013-04-26 2013-07-10 山东师范大学 酯化法制备偶氮二甲酸二烷基酯

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020143061A1 (en) * 2000-04-13 2002-10-03 Pitzele Barnett S. 2-amino-5, 6 heptenoic acid derivatives useful as nitric oxide synthase inhibitors
CN102898327A (zh) * 2012-10-26 2013-01-30 山东师范大学 偶氮二甲酸二甲酯及其中间体的合成方法
CN103012215A (zh) * 2013-01-22 2013-04-03 山东师范大学 偶氮二甲酸二烷基酯的制备方法
CN103193686A (zh) * 2013-04-26 2013-07-10 山东师范大学 酯化法制备偶氮二甲酸二烷基酯

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Application publication date: 20190423