CN102925002B - 一种纺织品喷墨印花用白色涂料墨水的制备方法 - Google Patents
一种纺织品喷墨印花用白色涂料墨水的制备方法 Download PDFInfo
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Abstract
一种纺织品喷墨印花用白色涂料墨水的制备方法,属于精细化工和材料科学技术领域。本发明的喷墨印花白色涂料墨水是由氧化物/聚合物纳米复合粒子分散体为白色着色剂,通过与水溶性共溶剂、表面活性剂和去离子水混合搅拌,过滤而成,该法制备的白色涂料墨水具有良好的分散稳定和储存稳定性,本发明所述的白色颜料墨水制备方法具有设备投资小,生产工艺简单,产品质量稳定且适合大规模生产等特点。
Description
技术领域
本发明属精细化工和材料科学技术领域,具体涉及一种纺织品喷墨印花用白色涂料墨水的制备方法。
技术背景
喷墨印花是集计算机、信息、新材料和精细化工等多学科领域为一体的纺织品印染加工新技术,具有印花精细度高、批量灵活、无染料和助剂浪费等优点。然而,以往纺织品喷墨印花主要针对白色织物,近年来随着非白色织物印花量的增加,白色涂料墨水的需求量也越来越大,成为纺织品喷墨印花中重要的颜色之一。
氧化硅和氧化钛是纺织品喷墨印花用白色涂料墨水的主要着色剂,然而,由于这些颜料的比重大,在低粘度喷墨印花墨水介质中长期存放时,容易发生颗粒沉降和堵塞喷头等现象,导致喷墨印花无法进行。虽然减小颜料的粒径,或者增大墨水的粘度可在一定程度上提高墨水的稳定性,但仍然距离喷墨墨水实际要求有很大的差距。因此,目前市场上白色涂料墨水还是主要依赖于杜邦、爱普生等跨国企业。资料检索发现中国专利CN101652437A和CN201210180490.9分别公开了溶剂型白色涂料墨水的制备方法,其做法是将白色颜料在分散剂协助下,通过研磨加工而成。美国US2010/0190922A1公开了采用氧化硅、分散剂和乳胶粒为主要组分制备稳定喷墨打印墨水的方法;US2010/0039463A1公开了通过提高墨水中氧化钛含量的方法来改善白色涂料墨水稳定性的方法;US2009/0087627A1和US2006/0155005A1分别公开了以白色涂料、分散剂和光引发剂、可聚合单体组成紫外光固化涂料墨水的方法。
尽管关于白色涂料墨水制备方法很多,然而,总结相关的专利发现,这些方法中所采用的颜料仍然是将氧化硅或者氧化钛在特殊结构分散剂的协助下,通过高速分散制备而成。关于本专利公开的以聚合物包覆氧化物纳米复合粒子为着色剂组成纺织品喷墨印花用白色涂料墨水的报道较少。
发明内容
本发明目的在于提供一种纺织品喷墨印花用白色涂料墨水的制备方法,具体做法是先采用硅烷偶联剂对纳米氧化物进行接枝改性,然后利用硅烷偶联剂的可聚合基团与其它单体共聚,在氧化硅表面引入具有分散和稳定双重作用的聚合物,制备聚合物包覆氧化物纳米复合粒子,并以此为着色剂,加入多种水溶性共溶剂和相关助剂,搅拌均匀后,过滤,制备纺织品喷墨印花用白色涂料墨水。
本发明的技术方案:一种纺织品喷墨印花用白色涂料墨水的制备方法,将聚合物包覆氧化物纳米复合粒子分散体、水溶性共溶剂和表面活性剂按一定比例加入到去离子水中,搅拌混合均匀后,调节墨水的pH,最后用500nm的滤膜过滤,制备白色涂料墨水。具体制备过程是将质量分数1~5%的表面活性剂加到质量分数为15~80%去离子水中,然后加入质量分数10~30%聚合物包覆氧化物纳米复合粒子分散体和质量分数为10~50%水溶性共溶剂,0.05~0.5%的抗菌剂,用搅拌机以500~1000转/分钟的速度搅拌20~50分钟,调节pH为7-9,然后用500nm的滤膜过滤,制备白色涂料墨水;实验测试表明所配制的墨水的粘度5~8cP,表面张力28~35mN/m,粒径50-150nm。
本发明所述的聚合物包覆氧化物纳米复合粒子分散体的制备方法:将质量分数为5~30%纳米氧化物分散到质量分数为40~90%乙醇和水所组成的混合溶剂中(乙醇和水的质量比为1∶1),加入质量分数为1~6%的硅烷偶联剂,用氨水调节pH至8~9,在20-60℃条件下反应2-3小时后,加入质量分数为5~20%的共聚单体和质量分数为0.5-2%的乳化剂,高速分散至纳米级,转移置水浴锅中,通氮气30分钟后,在搅拌速度为250-600转/分钟下升温至60-80℃,开始滴加对单体质量分数为0.5~3%的引发剂。反应2-8小时后高速离心,即可得到聚合物包覆氧化物纳米复合粒子。将质量分数为1~10%分散剂溶解到70~90%去离子水中,调节pH为7~9,添加10~20%聚合物包覆氧化物纳米复合粒子,使用超声波进行分散处理10~40分钟。所选用的分散剂为分子量在3000~10000丙烯酸类单体的聚合物。所述制备纺织品喷墨印花用白色涂料墨水的氧化物为纳米氧化硅或纳米氧化钛。所述的共聚单体为丙烯酸、甲基丙烯酸、丙烯酰胺、衣康酸、对苯乙烯磺酸钠中的一种或两种;所选用的引发剂是过硫酸铵、过硫酸钾、过硫酸钠、偶氮二异丁基脒盐酸盐、偶氮二异丙基咪唑啉盐酸盐中的一种;所选用的乳化剂是十二烷基硫酸钠、十二烷基苯磺酸钠、十二烷基磺酸钠、烷基萘磺酸钠中的一种或两种。
所选用的水溶性共溶剂是乙醇、正丙醇、异丙醇、正丁醇、乙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、一缩二乙二醇、二缩三乙二醇、三缩四乙二醇、聚乙烯醇200、聚乙烯醇400、聚乙二醇600、丙三醇、三乙醇胺、季戊四醇、2-吡咯烷酮、N-甲基-2-吡咯烷酮中的两种或几种。
所选用的表面活性剂是阴离子型、非离子型或者两者复配;阴离子型表面活性剂为十二烷基硫酸钠、十二烷基苯磺酸钠、油酸钾、烷基萘磺酸钠、松香酸钠中的一种;所述的非离子型如聚氧乙烯烷基酚缩合物:OP-7、OP-10或OP-15;聚氧乙烯脂肪醇缩合物:平平加O-10、平平加O-20、平平加O-25或平平加A-20;聚氧乙烯多元醇醚脂肪酸酯:如Tween40、Tween60、Tween65、Tween80;脂肪酸的聚氧乙烯酯类:如SG-10、SE-10、OE-15。
所述的pH调节剂为氢氧化钠、碳酸钠、氨水、三乙醇胺中的一种。
所述的抗菌剂是香草醛或乙基香草醛类化合物、酰基苯胺类、咪唑类、噻唑类、异噻唑酮衍生物、季铵盐类、双呱类、酚类中的一种。
本发明的有益效果:本发明制备的白色涂料墨水平均粒径小于180nm,采用聚合物包覆氧化物纳米复合粒子为着色剂,具有分散稳定性好,遮盖力高等优点。该墨水可长期贮存,并可直接用于纺织品的喷墨印花。
具体实施方式
下面通过实施例子,进一步阐述本发明的突出优点和显著特点,但本发明决不局限于实施例子。
实例1
纳米二氧化硅复合粒子的制备:称取纳米二氧化硅15g,水29.5g,乙醇29.5g,混合均匀后加入5g KH-570,用氨水溶液调节pH至8~9,在40℃条件下反应2小时后再加入10g对苯乙烯磺酸钠和1g十二烷基硫酸钠,充分搅拌后将溶液转移到功率为1100w的超声粉碎仪下超声15分钟。然后再转移至水浴锅中,通氮气30分钟后在500转/分钟的搅拌速度下升温至65℃,滴加10g质量分数为10%的过硫酸铵溶液,反应4h。高速离心沉淀,即可得到二氧化硅/聚对苯乙烯磺酸钠纳米复合粒子。
取2g马来酸酐-甲基丙烯酸甲酯共聚物(Mn=8000,马来酸酐:甲基丙烯酸甲酯=1∶1),加入0.20g氢氧化钠,去离子水85.8g,搅拌至完全溶解,然后加入二氧化硅/聚对苯乙烯磺酸钠纳米复合粒子12g,使用超声波超声分散30分钟制得二氧化硅/聚苯乙烯磺酸钠纳米复合粒子分散体。
取十二烷基硫酸钠1.2g和OP-10乳化剂1g溶于41.7g去离子水,依次加入纳米复合粒子分散体30g,1,6-己二醇10g,三缩四乙二醇12g,正丁醇4g,酰基苯胺抗菌剂0.1g用搅拌机500r/min搅拌30min,再氢氧化钠溶液调节pH值至9,最后用500nm的微孔滤膜过滤得到水性白色颜料墨水。物墨水指标如下:表面张力σ=34.6mN/m,粘度η=7.67cP,Z均粒径d=154.2nm。
实例2
纳米复合粒子分散体制备同实例1,取十六烷基苯磺酸钠1.5g,0.5g吐温80溶于42.7g去离子水中,加入纳米硅复合粒子分散体25g,正丙醇10g、一缩二乙二醇10g、季戊四醇10g和噻唑类抗菌剂0.3g,用搅拌机1000r/min搅拌50min,再用氢氧化钠调节pH值至8,最后用500nm的微孔滤膜过滤得到水性白色颜料墨水,墨水指标如下:表面张力σ=31.2mN/m,粘度η=8.91cP,Z均粒径d=158.6nm。
实例3
纳米二氧化钛复合粒子的制备:称取纳米二氧化钛30g,水11g,乙醇11g,混合均匀后,加入6g KH-570,用氨水溶液调节pH至8~9,反应3h后再加入20g甲基丙烯酸和2g十二烷基磺酸钠,充分搅拌后将其转移到高速乳化机中乳化15分钟。转移至水浴中,通氮气30分钟后在250转/分钟的搅拌速度下升温至75℃,开始滴加20g质量分数为10%的过硫酸钠溶液,反应5h。高速离心沉淀,即可得到二氧化钛/聚甲基丙烯酸纳米复合粒子。
取3g苯乙烯-丙烯酸丁酯共聚物(Mn=5000,苯乙烯∶丙烯酸丁酯=3∶1),加入20%氨水6g,去离子水71g,搅拌至完全溶解,然后加入纳米复合粒子20g,使用超声波超声分散10分钟制得二氧化钛/聚甲基丙烯酸纳米复合粒子分散体。
取平平加O-251g溶于48.5g去离子水中,加入纳米二氧化钛复合粒子分散体20g,异丙醇5g、聚乙烯醇20010g、1,4-丁二醇15g和异噻唑酮0.5g,用搅拌机700转/分搅拌40分钟,再用20%氨水调节pH值至8,最后用500nm的微孔滤膜过滤得到水性白色颜料墨水,物性指标如下:表面张力σ=28.4mN/m,粘度η=6.15cP,Z均粒径d=162.2nm。
实例4
纳米复合粒子分散体制备同实例2,取SE-10 1g溶解到45.7g去离子水中,加入纳米硅复合粒子分散体25g,异丙醇6g、二缩二乙二醇10g、2-吡咯烷酮12g和双呱类抗菌剂0.3g用搅拌机1000r/min搅拌30min,再用三乙醇胺调节pH值至9,最后用500nm的微孔滤膜过滤得到水性白色颜料墨水,物性指标如下:表面张力σ=30.5mN/m,粘度η=6.97cP,Z均粒径d=152.4nm。
Claims (3)
1.一种纺织品喷墨印花用白色涂料墨水的制备方法,其特征在于由下列组分按质量份数组成:聚合物包覆氧化物纳米复合粒子分散体10~30份,水溶性共溶剂10~50份,表面活性剂1~5份,抗菌剂0.05~0.5份,加去离子水至总重量100份,按配方在去离子水中依次加入聚合物包覆氧化物纳米复合粒子分散体、水溶性共溶剂、表面活性剂和抗菌剂,搅拌混合均匀后,调节墨水pH为7~9,最后用500nm的滤膜过滤,制备白色涂料墨水;这里聚合物包覆氧化物纳米复合粒子分散体按如下方法制备:将质量分数为5~30%纳米氧化硅或纳米氧化钛分散到质量分数为40~90%质量比为1∶1乙醇和水的混合溶剂中,然后加入质量分数为1~6%的硅烷偶联剂KH570,用氨水调节pH至8~9,在20-60℃条件下反应2-3小时,加入质量分数为5~20%的共聚单体和质量分数为0.5-2%的乳化剂,高速分散至纳米级,转移置水浴锅中,通氮气30分钟,在搅拌速度为250-600转/分钟下升温至60-80℃,开始滴加对单体质量分数为0.5~5%的引发剂,反应2-8小时后高速离心,得到聚合物包覆氧化物纳米复合粒子,将质量分数为1~10%分子量在3000~10000丙烯酸类聚合物溶解到70~90%去离子水中,调节pH为7~9,添加10~20%聚合物包覆氧化物纳米复合粒子,用超声波进行分散处理10~40分钟;这里采用的共聚单体为丙烯酸、甲基丙烯酸、丙烯酰胺、衣康酸、对苯乙烯磺酸钠中的一种或两种;引发剂是过硫酸铵、过硫酸钾、过硫酸钠、偶氮二异丁基脒盐酸盐、偶氮二异丙基咪唑啉盐酸盐中的一种;乳化剂是十二烷基硫酸钠、十二烷基苯磺酸钠、十二烷基磺酸钠、烷基萘磺酸钠中的一种或两种。
2.如权利要求1所述的制备方法,其特征是所用的水溶性共溶剂是乙醇、正丙醇、异丙醇、正丁醇、乙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、一缩二乙二醇、二缩三乙二醇、三缩四乙二醇、聚乙烯醇200、聚乙烯醇400、聚乙二醇600、丙三醇、三乙醇胺、季戊四醇、2-吡咯烷酮、N-甲基-2-吡咯烷酮中的两种或几种。
3.如权利要求1所述的制备方法,其特征是所用的表面活性剂是阴离子型、非离子型或者两者复配;所述的阴离子型为十二烷基硫酸钠、十二烷基苯磺酸钠、油酸钾、烷基萘磺酸钠、松香酸钠;所述的非离子型为聚氧乙烯烷基酚缩合物:OP-7、OP-10或OP-15,聚氧乙烯脂肪醇缩合物:平平加0-10、平平加O-20、平平加O-25或平平加A-20;聚氧乙烯多元醇醚脂肪酸酯:Tween40、Tween60、Tween65、Tween80;脂肪酸的聚氧乙烯酯类:SG-10、SE-10、OE-1。
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EP4066064A4 (en) | 2019-11-25 | 2024-01-10 | Landa Corp Ltd | INK DRYING IN DIGITAL PRINTING WITH INFRARED RADIATION ABSORBED BY PARTICLES EMBEDDED WITHIN AN ITM |
US11321028B2 (en) | 2019-12-11 | 2022-05-03 | Landa Corporation Ltd. | Correcting registration errors in digital printing |
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JP2008248006A (ja) * | 2007-03-29 | 2008-10-16 | The Inctec Inc | インクジェット記録用油性白色インク及びその製造方法 |
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