CN111335050B - 一种印花用梳型分散染料分散剂及其制备方法 - Google Patents
一种印花用梳型分散染料分散剂及其制备方法 Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/5214—Polymers of unsaturated compounds containing no COOH groups or functional derivatives thereof
- D06P1/5221—Polymers of unsaturated hydrocarbons, e.g. polystyrene polyalkylene
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- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
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- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
- D06P1/5292—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds containing Si-atoms
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- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/60—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
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- D06P1/64—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
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Abstract
本发明提供一种印花用梳型分散染料分散剂及其制备方法,该印花用梳型分散染料分散剂包括苯乙烯马来酸酐共聚物、聚乙二醇醚单胺、含环状结构的烷基胺、长链烷基胺、胺基封端聚二甲基硅氧烷和催化剂。制备方法包括:在氮气保护下,加入聚乙二醇醚单胺、含环状结构的烷基胺、长链烷基胺,加热完全溶解后,加入苯乙烯马来酸酐共聚物,升温至140~160℃,溶解完全;加入催化剂,保温反应;降温至100~120℃,加入胺基封端聚二甲基硅氧烷,保温反应;加入水,稀释至固含量为40~60%,调节pH至5~7,即得。本发明以苯乙烯马来酸酐为基础树脂进行梳型改性,通过聚乙二醇醚单胺、含环状结构的烷基胺的改性,构建了锚固、空间位阻、电荷排斥的三重分散结构。
Description
技术领域
本发明属于分散染料技术领域,具体涉及一种印花用梳型分散染料分散剂及其制备方法。
背景技术
分散染料是一类分子比较小,结构上不带水溶性基团,是一类水溶性低、染色时在水中主要以微细颗粒呈分散状态存在的非离子染料。它在染色时必须借助于分散剂,将染料均匀地分散在染液中,才能对聚酯之类的纤维进行染色。分散染料是随着水性纤维的发展而发展起来的一类染料。20世纪20年代醋酯纤维出现后,用水溶性的染料很难染色,因此人们合成了疏水性较强的一类染料,分散染料。随着聚酰胺纤维、丙烯腈纤维,特别是聚酯纤维的迅速发展,分散染料有了飞速的发展。经分散染料印染加工的化纤纺织产品,色泽艳丽,耐洗牢度优良,用途广泛。
分散染料主要有染色和印花两种印染方式,其中印花是使用染料,通过一定的实施方式,能够在纺织品上得到可复制图案的加工过程。印花工艺流程主要包含图案设计、制版、色浆调制、印制花纹、后护理等工艺,其中后处理工艺包含蒸化、退浆、水洗等步骤,是影响花纹质量最重要的步骤。蒸化,也称汽蒸,在较高温度下实现染料从色浆向纤维中转移的过程,大规模的生产车间大都采用高温蒸化机,在160~180℃下,连续蒸发5~20分钟。
高温高压下的纤维分子链段的剧烈运动,产生瞬时空隙,染料分子扩散进入,完成染色、固色的过程。高温高压下尽管有效提高了分散染料的染色、固色效果,但也给分散染料的分散剂带来的更大更高的需求,由于高温高压条件下,染料的自我分散性降低,染料颗粒更容易团聚,凝结成粗大颗粒,尽管现有的木质素、萘盐类分散剂都能一定程度上满足上述需求,但是其也存在加入量多,不环保,分散效率差的问题,而同时现有的大多数高分子超分散剂在高温高压体系下由于分子运动的加剧以及高温高压下的水化作用加剧,使得分散剂会容易从水溶剂体系中脱出,大大降低对染料颗粒的分散保护作用,更进一步加剧了染料颗粒的团聚凝结,导致印花过程中发生浮色、色点等问题。
另外,印花是在织物上局部地方获得有色发纹的加工着色过程,为了获得清晰的团,印花色浆中需要加入适当的糊料来防止染料的渗化,现有工艺中使用的糊料以海藻酸钠与丙烯酸盐为主。现有的应用于分散染料的分散剂多为羧酸盐类,聚电解质类高分子表面活性剂,在印花工艺中使用时会极大的影响染料与耐盐性较差的印花糊料的相容性,带来色浆黏度下降,产生渗化、花纹不清晰等问题,大大影响印花质量。
发明内容
本发明针对现有技术存在的不足,提供一种印花用梳型分散染料分散剂及其制备方法,具有良好的耐高温高压效果,可有效保证分散染料在高温印花过程中的染料颗粒稳定性,大大减少染料颗粒的团聚凝结,获得更好的染色效果,同时具有良好的印花糊料相容性,有效保证印花过程中的产品花纹质量,抑制渗化、色点,减少白底沾污。
本发明解决上述技术问题的技术方案如下:一种印花用梳型分散染料分散剂,按照重量份包括以下成分:苯乙烯马来酸酐共聚物10~40份、聚乙二醇醚单胺60~80份、含环状结构的烷基胺5~10份、长链烷基胺3~6份、胺基封端聚二甲基硅氧烷0.1~0.25份、催化剂1~5份。
本发明进一步设置为,所述苯乙烯马来酸酐共聚物中,马来酸酐(MA)的占比为20~35%,分子量(Mn)在2000~7500。
本发明进一步设置为,所述聚乙二醇醚单胺中,烷基为C1~C6的烷基,乙氧基(EO)数为40~70。
优选的,所述聚乙二醇醚单胺中,烷基为C4~C6的支链结构。
本发明进一步设置为,所述含环状结构的烷基胺中的环状结构为5~8烷基环;所述含环状结构的烷基胺中的烷基为碳链数为0~4的直链结构。
本发明进一步设置为,所述长链烷基胺为碳链数为8~12的直链或异构链。
本发明进一步设置为,所述胺基封端聚二甲基硅氧烷为双胺基封端的二甲基硅氧烷,其中硅氧烷聚合度为3~6。
本发明进一步设置为,所述催化剂为有机强酸。
优选的,所述催化剂为4-甲苯磺酸、胺基磺酸和丙酸中的一种或多种。
本发明还提供了上述印花用梳型分散染料分散剂的制备方法,包括以下步骤:
(1)在氮气保护下,加入聚乙二醇醚单胺、含环状结构的烷基胺、长链烷基胺,加热至80~100℃,完全溶解后,加入苯乙烯马来酸酐共聚物,升温至140~160℃,溶解完全;
(2)加入催化剂,保温反应5~10小时;
(3)降温至100~120℃,加入胺基封端聚二甲基硅氧烷,保温反应2~3小时;
(4)加入水,稀释至固含量为40~60%,使用氢氧化钠溶液调节pH至5~7,即得所述印花用梳型分散染料分散剂。
相比现有技术,本发明有以下有益效果:
本发明印花用梳型分散染料分散剂以苯乙烯马来酸酐为基础树脂进行梳型改性,通过聚乙二醇醚单胺、含环状结构的烷基胺的改性,构建了锚固、空间位阻、电荷排斥的三重分散结构。
1、含环状结构的烷基胺的结构引入,有效解决了单一苯乙烯结构硬链段,空间位阻大,对染料颗粒包覆锚固不完全的问题,通过软性环形链段的引入,双锚固基团更进一步的对染料颗粒进行各位置的锚固,协同作用,有效提升了锚固稳定作用。同时环形结构,相比常规链状结构在空间位阻方面也有进一步的改善,从锚固吸附、空间位阻两个方面对染料颗粒达到了更进一步的稳定分散效果。
2、长链烷基胺的引入可以进一步提升分散剂的降低表面张力效果,改善润湿性,一方面提升了分散剂对染料的润湿分散能力,另一方面可以有效提升分散剂与印花糊料等组分的相容性,提高应用范围。
3、高乙氧基数(EO值)聚乙二醇醚单胺,为梳型分散剂提供了足够的亲水性基团,调整整体分散剂亲水亲油性的同时,高EO值醇醚可以有效提升分散剂在高温高压下的耐受性,尤其是常规聚醚性表活在高温下的浊点问题,通过对醇醚EO值的控制,本发明分散剂的耐受温度远远大于高温高压的常规使用温度130℃。
4、胺基封端聚二甲基硅氧烷的引入,通过聚二甲基硅烷的柔性链段,在梳型分散剂间建立微交联结构,更好的通过交联网状构型结构提升梳型分散剂的耐高分散及耐高压效果的同时,链段的柔性效果可以更好的包覆保护染料颗粒,保证在高温高压期间随着环境的改变,分散剂可以始终随着染料颗粒理化性质的改变进行相对应的链段变化,保证稳定效果的高效性。
胺基端基的改性,在140℃以上反应,与马来酸酐形成酰亚胺结构,一方面进一步提升了分散剂的耐高温效果,同时大大减少了体系的羧酸盐含量,有效改善了分散剂与印花糊料的相容性,显著提高了印花效果质量。
通过上述工艺的引入,本发明分散剂相比常规木质素或超分散剂在对分散染料的分散效果,尤其是高温高压下的稳定效果有了显著性的提升,可以有效保证分散染料的染色期间的分散稳定性,同时与印花糊料有良好的相容性,大大提升印染效果及染料利用率,对提高分散染料的印染效率及环保问题有着重要意义。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例一
1、在氮气保护下,加入聚乙二醇醚单甲胺(EO=40)70份、环戊胺5份、辛胺3份,加热至80℃,完全溶解后,加入苯乙烯马来酸酐共聚物10份,Mn=2000,MA占比35%,升温至140℃,溶解完全。
2、加入催化剂丙酸1份,保温反应5小时。
3、降温至100℃,加入交联剂胺基封端聚六甲基三硅氧烷0.1份,保温反应2小时。
4、加入水,稀释至固含量为40%,氢氧化南调节pH值5.0,即得所述梳型分散剂。
实施例二
1、在氮气保护下,加入聚乙二醇醚单丁胺(EO=70)60份、乙基环己胺10份、月桂胺6份,加热至90℃,完全溶解后,加入苯乙烯马来酸酐共聚物20份,Mn=7500,MA占比20%,升温至150℃,溶解完全。
2、加入催化剂胺基磺酸3份,保温反应10小时。
3、降温至110℃,加入交联剂胺基封端聚八甲基四硅氧烷0.25份,保温反应2小时。
4、加入水,稀释至固含量为60%,调节pH至6.0,即得所述梳型分散剂。
实施例三
1、在氮气保护下,加入聚乙二醇醚单己胺(EO=50)80份、丁基环辛胺7.5份、癸胺4.5份,加热至100℃,完全溶解后,加入苯乙烯马来酸酐共聚物40份,Mn=5000,MA占比30%,升温至160℃,溶解完全。
2、加入催化剂4-甲苯磺酸5份,保温反应8.5小时。
3、降温至120℃,加入交联剂胺基封端聚十二甲基六硅氧烷0.2份,保温反应3小时。
4、加入水,稀释至固含量为50%,调节pH至6.0,即得所述梳型分散剂。
实施例四
1、在氮气保护下,加入聚乙二醇醚单戊胺(EO=60)70份、环戊胺9份、2-辛胺5份,加热至90℃,完全溶解后,加入苯乙烯马来酸酐共聚物30份,Mn=5500,MA占比25%,升温至140℃,溶解完全。
2、加入催化剂4-甲苯磺酸3份,保温反应7.5小时。
3、降温至115℃,加入交联剂胺基封端聚十甲基五硅氧烷0.15份,保温反应2小时。
4、加入水,稀释至固含量为55%,调节pH至7.0,即得所述梳型分散剂。
对比例一 工艺参照实施例二,去除步骤3交联剂的加入,得60%固含量的梳型分散剂。
对比例二 以木质素磺酸钠做分散剂。
对比例三 以BYK190做分散剂。
对比例四 工艺参照实施例三,去除步骤1中癸胺的加入,得50%固含量的梳型分散剂。
高温稳定性试验:
(1)色浆研磨:在容器中加入配方用量的水、分散剂,用搅拌机充分搅拌均匀,使分散剂完全溶于水;加入配方用量的分散染料(试验染料类型为分散红FB),用高速剪切搅拌机对物料进行高速剪切搅拌,搅拌时长30分钟;取上述浆液用砂磨机研磨,研磨遍数2~5遍;取砂磨过后的浆液,筛网过滤即可得分散染料色浆成品。
(2)高温稳定性测试:取上述色浆成品按色浆与水1:100的比例进行稀释,用醋酸调节pH值5.0~5.5之间,在170℃,密封保温一段时间后,降温至90℃,真空滤纸抽滤后,滤纸自然晾干,进行检测评级,稳定性观察。其稳定性情况如表1所示:
表1高温稳定性试验
*级别越高,说明残留物越少,染料聚集颗粒少,分散稳定性较好。
(3)分散剂与印花糊料相容性实验
取(1)中研磨好的色浆与合成丙烯酸糊料按1:100进行混合,搅拌均匀后,检测其粒径变化,同时采用100目丝网进行印压过网后,观察丝网上染料残留情况。
表2不同分散剂与印花糊料的相容性
从表2中可以看出本发明分散剂与丙烯酸糊料具有良好的相容性,可以有效保证印花过程中的产品印花质量。
(4)对(1)中研磨好的色浆进行涤纶织物印花效果评价,经色浆调制、印花、烘干、蒸化、水洗、烘干等工艺。
印花色浆处方:染料色浆5%,丙烯酸类糊料60%,六偏磷酸钠0.1%水余量。
蒸化工艺:常压高温法,170℃,汽蒸10min。
表3不同分散剂对织物印花性能影响
表3中,耐皂洗色牢度参照GB/T 3921-2008,干耐摩擦牢度参照GB/T3920-2008。
从上两表中可以看出本发明的印花用梳型分散染料分散剂可以有效提高分散染料在高温印花下的体系颗粒稳定性,相比传统的木质素及高分子分散剂,本发明分散剂具有更高的耐高温高压的能力,通过对锚固及空间位阻结构的调控更好的对染料颗粒进行了包覆分散,锚固更完全,分散更稳定,同时通过柔性微交联组分的引入,可以进一步提升分散剂在水体系中理化稳定性,从而保证对染料颗粒的在不同环境下的稳定分散保护,相比传统分散剂本发明分散剂在染色效果及利用率上有了显著的改善提升,同时通过酰亚胺化等措施有效改善了分散剂与印花糊料的相容性,印花后的布匹效果优良,图案更清晰鲜艳,色牢度更高。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种印花用梳型分散染料分散剂,其特征在于,按照重量份包括以下成分:苯乙烯马来酸酐共聚物10~40份、聚乙二醇醚单胺60~80份、含环状结构的烷基胺5~10份、8~12碳长链烷基胺3~6份、胺基封端聚二甲基硅氧烷0.1~0.25份、催化剂1~5份。
2.根据权利要求1所述的印花用梳型分散染料分散剂,其特征在于,所述苯乙烯马来酸酐共聚物中,马来酸酐的占比为20~35%,分子量在2000~7500。
3.根据权利要求1所述的印花用梳型分散染料分散剂,其特征在于,所述聚乙二醇醚单胺中,烷基为C1~C6的烷基,乙氧基数为40~70。
4.根据权利要求3所述的印花用梳型分散染料分散剂,其特征在于,所述聚乙二醇醚单胺中,烷基为C4~C6的支链结构。
5.根据权利要求1所述的印花用梳型分散染料分散剂,其特征在于,所述含环状结构的烷基胺中的环状结构为5~8烷基环;所述含环状结构的烷基胺中的烷基为碳链数为0~4的直链结构。
6.根据权利要求1所述的印花用梳型分散染料分散剂,其特征在于,所述8~12碳长链烷基胺为直链烷基胺。
7.根据权利要求1所述的印花用梳型分散染料分散剂,其特征在于,所述胺基封端聚二甲基硅氧烷为双胺基封端的二甲基硅氧烷,其中硅氧烷聚合度为3~6。
8.根据权利要求1所述的印花用梳型分散染料分散剂,其特征在于,所述催化剂为有机强酸。
9.根据权利要求8所述的印花用梳型分散染料分散剂,其特征在于,所述催化剂为4-甲苯磺酸和胺基磺酸中的一种或多种。
10.根据权利要求1~9任一项所述的印花用梳型分散染料分散剂的制备方法,其特征在于,包括以下步骤:
(1)在氮气保护下,加入聚乙二醇醚单胺、含环状结构的烷基胺、长链烷基胺,加热至80~100℃,完全溶解后,加入苯乙烯马来酸酐共聚物,升温至140~160℃,溶解完全;
(2)加入催化剂,保温反应5~10小时;
(3)降温至100~120℃,加入胺基封端聚二甲基硅氧烷,保温反应2~3小时;
(4)加入水,稀释至固含量为40~60%,使用氢氧化钠溶液调节pH至5~7,即得所述印花用梳型分散染料分散剂。
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