CN113372558A - 可同浴染色的阴离子嵌段硅油的制备方法及其应用工艺 - Google Patents
可同浴染色的阴离子嵌段硅油的制备方法及其应用工艺 Download PDFInfo
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
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Abstract
本发明公开了可同浴染色的阴离子嵌段硅油的制备方法及其应用工艺,步骤如下:将双端环氧硅油,在有机溶剂中与聚醚胺和多乙烯多胺进行缩合反应,得到氨基封端的三元嵌段硅油;将二元羧酸酐加入上述氨基封端的三元嵌段硅油中,搅拌反应,加入醇胺类化合物得到阴离子改性的三元嵌段硅油柔软剂。本发明的优点有:对嵌段硅油进行阴离子改性,使得有机硅柔软剂可以自乳化分散于水中,并且与前处理和染色工艺中的原料离子性相同,因而避免了阴阳离子相互吸附导致物料沉淀的问题,实现了染色和柔软同浴工艺,因而缩减了后整理工艺,大大提高了生产的效率,也避免了后整理工艺中经常出现的色渍色斑问题。
Description
技术领域
本发明涉及织物印染技术领域,尤其涉及一种染色用柔软剂。
背景技术
印染生产工艺主要由前处理,染色和后整理三个工艺组成。现有技术方案通常都是在前处理和染色后,清洗干净织物,再进行柔软整理工艺,工艺耗时长,工作效率低,之所以要分开处理,主要因为前处理和染色的工艺中主要物料都是阴离子结构,而柔软剂大多是阳离子或弱阳离子结构,因此不能同浴使用。这导致生产工序不能减少,水消耗高,能源消耗高,产能低等生产成本高的问题,还导致环境污染严重。因此,研发一种能够在染色同时进行柔软整理的柔软剂是非常具有前景的。
中国专利公开号为“CN 105949468 A”,名为《一种阴离子型线性共聚有机硅柔软整理剂的制备方法》,其公开的制备方法包含:本发明包括1,1,3,3-四甲基二硅氧烷的有机硅高分子扩链反应、甲代烯丙基氯与端含氢硅油的加成反应、端含氯侧含氢硅油的制备、烯酸与侧含氢的加成反应、有机硅高分子链段的氨解、端环氧聚醚的制备和有机硅高分子链段与聚醚链段的缩聚反应。本发明对有机硅链段进行了阴离子改性,提高了乳液对阴离子的配伍性,阴离子的引入还对乳液的耐高温、耐盐、耐碱性能大幅度提高,使得产品可以适用于染色同浴加工。但是该工艺制备步骤复杂,研发一种工序简单的柔软剂制备方法是有前景的。
发明内容
本发明的目的在于提供一种可同浴染色的阴离子嵌段硅油的制备方法,以解决现有技中没有能在染色工序中使用柔软剂,导致生产工序不能缩减的问题。
为了达到上述目的本发明采用如下技术方案:
一种可同浴染色的阴离子嵌段硅油的制备方法,步骤如下:
(1)将51-58份双端环氧硅油,在35-45份有机溶剂中与2-8份聚醚胺和0.2-1份多乙烯多胺进行缩合反应,得到氨基封端的三元嵌段硅油;
(2)将2.5-4.5份二元羧酸酐加入90-95份所述氨基封端的三元嵌段硅油中,搅拌,加入3-5份醇胺类化合物,搅拌,得到阴离子改性的三元嵌段硅油柔软剂。
进一步地,
所述双端环氧硅油选自双端环氧聚醚硅油,分子量为3000-25000。
进一步地,
所述有机溶剂选自乙醇,异丙醇,异辛醇,丙二醇,乙二醇单丁醚,二乙二醇单丁醚,丙二醇单丁醚,二丙二醇单丁醚。
进一步地,
所述聚醚胺的分子结构式为NH2[CH2(CH3)CH2O]m[CH2CH2O]nCH2(CH3)CH2NH2。
进一步地,
所述多乙烯多胺选自二乙烯三胺、三乙烯四胺、四乙烯五胺、五乙烯六胺、哌嗪、胺乙基哌嗪、三乙烯二胺、六乙烯四胺。
进一步地,
所述二元羧酸酐选自1,4-丁二酸酐,顺丁烯二酸酐,戊二酸酐、己二酸酐、邻苯二甲酸酐。
进一步地,
所述醇胺类化合物选自二乙醇胺、三乙醇胺。
进一步地,
所述步骤(1)的反应温度为80-150℃,反应时间为5-24小时;
所述步骤(2)的反应温度为30-150℃,反应时间为2-12小时。
进一步地,
按摩尔比计,所述双端环氧硅油:聚醚胺和多乙烯多胺的总和为0.6-1.5;
按摩尔比计,所述二元羧酸:聚醚胺和多乙烯多胺的总和为1:1-2。
进一步地,
在常温染色缸中,浴比控制为1:5-10,染料,6.25g/l;氯化钠,60g/l;纯碱,25g/l;阴离子嵌段硅油,5g/l;温度为50-80℃保温90分钟;然后皂洗,冷水清洗干净;出缸烘干定型,得成品棉布。
本发明的优点包括:对嵌段硅油进行阴离子改性,使得有机硅柔软剂可以自乳化分散于水中,并且与前处理和染色工艺中的原料离子性相同,因而避免了阴阳离子相互吸附导致物料沉淀的问题,实现了染色和柔软同浴工艺,因而缩减了后整理工艺,大大提高了生产的效率,也避免了后整理工艺中经常出现的色渍色斑问题。
具体实施方式
下面将结合具体实施例来详细说明本发明,在此以本发明的示意性实施例及说明用来解释本发明,但并不作为对本发明的限定。
实施例1
1.制备氨基封端的嵌段硅油:在反应容器中加入51.4份双端环氧硅油(分子量为3000),7.7份聚醚胺ED-900(NH2[CH2(CH3)CH2O]m[CH2CH2O]nCH2(CH3)CH2NH2),0.9份二乙烯三胺,40份二丙二醇单丁醚,120℃保温反应10小时制得;
2.阴离子改性:在反应容器中加入91份上述氨基封端的嵌段硅油,再加入4.3份1,4-丁二酸酐,在50℃保温反应2小时之后,加入4.7份二乙醇胺,搅拌均匀,降温得到所述阴离子改性的嵌段硅油A。
3.所述硅油A的应用工艺:染色设备为常温染色缸,平纹针织棉布染黑色,浴比为1:8,棉布质量,100kg;活性黑染料,5kg;工业盐,72kg;纯碱,20kg;硅油A,4kg;60℃保温90分钟;然后皂洗,冷水清洗干净;出缸烘干定型,得成品棉布A;
实施例2
1.制备氨基封端的嵌段硅油:在反应容器中加入57.6份双端环氧硅油(分子量为12000),2.2份聚醚胺ED-900,0.2份四乙烯五胺,40份异丙醇,80℃保温反应12小时制得;
2.阴离子改性:在反应容器中加入94份上述氨基封端的嵌段硅油,再加入2.7份戊二酸酐,在50℃保温反应2小时之后,加入3.3份三乙醇胺,搅拌均匀,降温得到所述阴离子改性的嵌段硅油B;
3.应用工艺同实施例1,得棉布B。
实施例3
1.制备氨基封端的嵌段硅油:在反应容器中加入57.3份端环氧聚醚硅油(分子量为9000),2.4份聚醚胺ED-600,0.3份四乙烯五胺,40份乙二醇单丁醚,120℃保温反应8小时制得;
2.阴离子改性:在反应容器中加入93份上述氨基封端的嵌段硅油,再加入3份顺丁烯二酸酐,在40℃保温反应5小时之后,加入4份三乙醇胺,搅拌均匀,降温得到所述阴离子改性的嵌段硅油C;
3.应用工艺同实施例2,得棉布C。
对照试验
染色设备为常温染色缸,平纹针织棉布染黑色,浴比为1:8,棉布质量,25kg;活性黑染料,1.25kg;工业盐,36kg;纯碱,5kg;未改性的嵌段硅油,1kg;60℃保温90分钟;然后皂洗,冷水清洗干净;出缸烘干定型,得成品棉布D。
对比测试
测试几种棉织物的染色均匀度,手感,结果见下表:
染色均匀度采用目测;
柔软度测试:将样品编号,10名专业应用人员手摸评估,综合得到最终结论,评估标准:0-5表示柔软度等级,0最差,5最好;
硅油种类 | 棉布A | 棉布B | 棉布C | 棉布D |
染色均匀度 | 均匀 | 均匀 | 均匀 | 严重色花 |
柔软度 | 4-5 | 3-4 | 4-5 | 2-3 |
平滑度 | 3-4 | 5 | 4-5 | 2-3 |
。
以上对本发明实施例所提供的技术方案进行了详细介绍,本文中应用了具体个例对本发明实施例的原理以及实施方式进行了阐述,以上实施例的说明只适用于帮助理解本发明实施例的原理;同时,对于本领域的一般技术人员,依据本发明实施例,在具体实施方式以及应用范围上均会有改变之处,综上所述,本说明书内容不应理解为对本发明的限制。
Claims (10)
1.可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
步骤如下:
(1)将51-58份双端环氧硅油,在35-45份有机溶剂中与2-8份聚醚胺和0.2-1份多乙烯多胺进行缩合反应,得到氨基封端的三元嵌段硅油;
(2)将2.5-4.5份二元羧酸酐加入90-95份所述氨基封端的三元嵌段硅油中,搅拌,加入3-5份醇胺类化合物,搅拌,得到阴离子改性的三元嵌段硅油柔软剂。
2.根据权利要求1所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
所述双端环氧硅油选自双端环氧聚醚硅油,分子量为3000-25000。
3.根据权利要求1或2所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
所述有机溶剂选自乙醇,异丙醇,异辛醇,丙二醇,乙二醇单丁醚,二乙二醇单丁醚,丙二醇单丁醚,二丙二醇单丁醚。
4.根据权利要求1所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
所述聚醚胺的分子结构式为NH2[CH2(CH3)CH2O]m[CH2CH2O]nCH2(CH3)CH2NH2。
5.根据权利要求1所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
所述多乙烯多胺选自二乙烯三胺、三乙烯四胺、四乙烯五胺、五乙烯六胺、哌嗪、胺乙基哌嗪、三乙烯二胺、六乙烯四胺。
6.根据权利要求1或5所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
所述二元羧酸酐选自1,4-丁二酸酐,顺丁烯二酸酐,戊二酸酐、己二酸酐、邻苯二甲酸酐。
7.根据权利要求1所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
所述醇胺类化合物选自二乙醇胺、三乙醇胺。
8.根据权利要求1所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
所述步骤(1)的反应温度为80-150℃,反应时间为5-24小时;
所述步骤(2)的反应温度为30-150℃,反应时间为2-12小时。
9.根据权利要求5所述的可同浴染色的阴离子嵌段硅油的制备方法,其特征在于:
按摩尔比计,所述双端环氧硅油:聚醚胺和多乙烯多胺的总和为0.6-1.5;
按摩尔比计,所述二元羧酸:聚醚胺和多乙烯多胺的总和为1:1-2。
10.一种应用如权利要求1所述的可同浴染色的阴离子嵌段硅油的工艺,其特征在于:
在常温染色缸中,浴比控制为1:5-10,染料,6.25g/l;氯化钠,60g/l;纯碱,25g/l;阴离子嵌段硅油,5g/l;温度为50-80℃保温90分钟;然后皂洗,冷水清洗干净;出缸烘干定型,得成品棉布。
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