CN115073973A - 喷墨记录用油墨组合物及色料分散液 - Google Patents
喷墨记录用油墨组合物及色料分散液 Download PDFInfo
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- CN115073973A CN115073973A CN202210230000.5A CN202210230000A CN115073973A CN 115073973 A CN115073973 A CN 115073973A CN 202210230000 A CN202210230000 A CN 202210230000A CN 115073973 A CN115073973 A CN 115073973A
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Abstract
提供了一种储存稳定性优异、提高了涂膜的柔软性的喷墨记录用油墨组合物及色料分散液。喷墨记录用油墨组合物包含用分散染料着色的尿烷树脂的树脂颗粒,所述尿烷树脂的酸值为1KOHmg/g以上且小于100KOHmg/g。
Description
技术领域
本发明涉及喷墨记录用油墨组合物及色料分散液。
背景技术
以往,使用包含具有升华性的升华染料或分散染料的喷墨用油墨,通过喷墨方法对聚酯布帛进行印刷。
这种印染方法中,有直接打印法,将油墨附于应染色的记录介质后,通过蒸汽处理等热处理使染料上染;或热转印打印法,将染料油墨附于中间转印介质后,通过热使染料从中间转印介质侧向应染色的记录介质升华转印。
专利文献1中,作为省略上述染色工序中的上染工序、转印工序的手段,公开了如下方法:使用在聚酯微粒中包含分散染料的喷墨记录用油墨,通过喷墨方法向聚酯布帛或棉布等记录介质进行印刷。
现有技术文献
专利文献
专利文献1:日本特开平10-114865号公报
专利文献2:WO2016/027835号公报
但是,在专利文献1所述的油墨中,由于用分散剂分散染料,所以油墨的储存稳定性存在问题。另外,在专利文献1和专利文献2所述的记录方法中,由于仅使用聚酯树脂颗粒,所以涂膜容易缺乏柔软性。因此,在对具有柔软性的记录介质进行印刷并弯折的情况下,存在容易产生涂膜裂纹的问题。即,需要一种储存稳定性优异、提高了涂膜的柔软性的喷墨记录用油墨组合物及色料分散液。
发明内容
喷墨记录用油墨组合物包含用分散染料着色的尿烷树脂的树脂颗粒,所述尿烷树脂的酸值为1KOHmg/g以上且小于100KOHmg/g。
色料分散液包含用分散染料着色的尿烷树脂的树脂颗粒,所述尿烷树脂的酸值为1KOHmg/g以上且小于100KOHmg/g。
具体实施方式
1.色料分散液
本实施方式所涉及的色料分散液包含用分散染料着色的尿烷树脂的树脂颗粒、水和其它成分。色料分散液由树脂颗粒等成分分散于水等介质中而成。色料分散液适用于后述的喷墨记录用油墨组合物的制造。该喷墨记录用油墨使用喷墨方法,不仅能够适用于在棉或聚酯的布帛上的记录,还能够适用于在纸等多种记录介质上的记录。下面,对色料分散液中所含的各种成分进行说明。需要说明的是,在以后的说明中,也将喷墨记录用油墨组合物简称为油墨。
1.1.树脂颗粒
树脂颗粒包含尿烷树脂和分散染料。树脂颗粒是分散染料的分子分散在以尿烷树脂为基材的树脂颗粒中的物质。
树脂颗粒的平均粒径优选为30nm以上,更优选为40nm以上,进一步优选为50nm以上。另外,优选为500nm以下,更优选为400nm以下,进一步优选为300nm以下。
由于树脂颗粒的平均粒径在上述范围,使得树脂颗粒不易沉降,因此储存稳定性提高。由此,在通过喷墨方法由油墨形成的涂膜中,形成涂膜的树脂颗粒的致密性提高。其中,在以后的说明中,也将由喷墨记录用油墨组合物形成的涂膜简称为涂膜。
需要说明的是,在本说明书中,平均粒径是指以散射光强度为基准的粒度分布(50%)。平均粒径由散射强度分布求出。平均粒径的测定例如可以适用ELSZ-1000(大冢电子公司制造)。
1.1.1.尿烷树脂
尿烷树脂包含聚酯多元醇、异氰酸酯和其它多元醇作为原料,能够使它们聚合而得到。这里所说的尿烷树脂是指具有酸值的阴离子型树脂。
其中,尤其优选包含聚酯多元醇。据此,使用通常容易被分散染料染色的聚酯多元醇,使得涂膜的发色性提高。另外,在聚酯布帛或纸上印刷时的定影性提高,进而不易产生涂膜裂纹。
尿烷树脂的酸值优选为1KOHmg/g以上,更优选为3KOHmg/g以上,进一步优选为5KOHmg/g以上。另外,优选小于100KOHmg/g,更优选小于80KOHmg/g,进一步优选小于60KOHmg/g。
由于尿烷树脂的酸值在上述范围内,可以得到平均粒径分布窄的树脂颗粒,因此储存稳定性提高。
1.1.1.1.聚酯多元醇
聚酯多元醇是作为尿烷树脂的前驱体而制造的。聚酯多元醇包含以下所述的多元醇、二元酸和三元酸作为原料,使它们聚合而得到。
多元醇是具有两个以上作为官能团的羟基的单体成分。作为多元醇,可列举:乙二醇、二乙二醇、三乙二醇、新戊二醇、丙二醇、二丙二醇、丁二醇、聚乙二醇、1,3-丙二醇、1,4-丁二醇、3-甲基-1,5-戊二醇、1,4-环己烷二甲醇、异山梨醇、四氢呋喃二醇、双酚A、氢化双酚A、双酚A环氧烷加成物等。
其中,从涂膜的柔软性、发色性的观点出发,尤其优选乙二醇、二乙二醇、双酚A、3-甲基-1,5-戊二醇、新戊二醇。
多元醇可以分别单独使用一种或将两种以上组合使用。
二元酸是指具有两个作为官能团的羧基的单体成分。另外,也可以使用它们的酸酐和它们的碳数为1以上且4以下的烷基酯等。
作为二元酸,可列举:邻苯二甲酸、间苯二甲酸、对苯二甲酸、富马酸、马来酸、己二酸、癸二酸、琥珀酸、环己烷二甲酸以及它们的酸酐,还有它们的碳数为1以上且4以下的烷基酯等。
其中,从涂膜的柔软性、发色性的观点出发,尤其优选己二酸二甲酯、对苯二甲酸二甲酯、间苯二甲酸二甲酯。
二元酸可以单独使用一种,也可以将两种以上组合。
三元酸是指具有三个作为官能团的羧基的单体成分。另外,也可以使用它们的酸酐和它们的碳数为1以上且4以下的烷基酯等。
三元酸例如有:偏苯三酸、均苯三酸以及它们的酸酐等。
其中,尤其优选偏苯三酸、均苯三酸。据此,能够使尿烷树脂具有适度的亲水性,因此能够得到平均粒径的分布更窄的树脂颗粒,有助于提高储存稳定性。
三元酸可以单独使用一种,也可以将两种以上组合。
本实施方式的聚酯多元醇能够通过使多元醇、二元酸和三元酸共聚而得到。聚合反应例如可采用缩聚、加聚,没有特别限制。
1.1.1.2.异氰酸酯
异氰酸酯是具有一个以上作为官能团的异氰酸基的成分。作为异氰酸酯,可列举:2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、4,4'-二苯基甲烷二异氰酸酯、间苯二异氰酸酯、对苯二异氰酸酯、3,3'-二甲基-4,4'-联苯二异氰酸酯、1,3-苯二甲基二异氰酸酯、1,4-苯二甲基二异氰酸酯、1,5-萘二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、4-甲基-1,3-环己基二异氰酸酯、1,2-双(异氰酸根合甲基)环己烷、1,3-双(异氰酸根合甲基)环己烷、1,4-双(异氰酸根合甲基)环己烷、二环己基甲烷-4,4'-二异氰酸酯等。
异氰酸酯尤其优选具有两个以上的异氰酸酯基。由此,尿烷树脂中的尿烷键的比例增加,涂膜的强度提高。
上述异氰酸酯中,尤其优选使用六亚甲基二异氰酸酯、1,3-双(异氰酸根合甲基)环己烷、二环己基甲烷-4,4'-二异氰酸酯、异佛尔酮二异氰酸酯中的一种以上。据此,尿烷树脂中的分子运动的自由度增加,能够使得尿烷树脂更柔软,涂膜的柔软性提高。
1.1.1.3.其它多元醇
其他多元醇是在合成尿烷树脂时与聚酯多元醇一起使用的成分。作为其他多元醇,可列举:聚丁二醇、二羟甲基丙酸等。也可以使用作为聚酯多元醇的原料列举出的上述多元醇,并不限于这些。
其中,作为其他多元醇,特别优选二羟甲基丙酸。据此,能够使尿烷树脂具有适度的亲水性,因此能够得到平均粒径的分布更窄的树脂颗粒,有助于提高储存稳定性。
1.1.1.4.尿烷树脂的制造方法
本实施方式的尿烷树脂能够通过使聚酯多元醇、异氰酸酯和其它多元醇共聚而得到。聚合反应例如可采用加聚,没有特别限制。
1.1.2.分散染料
本实施方式的油墨及色料分散液包含以尿烷树脂为基材的树脂颗粒,该树脂颗粒中包含分散染料。
分散染料只要包含在尿烷树脂的树脂颗粒中即可,但优选分散在树脂颗粒中。需要说明的是,树脂颗粒可以以分散状态包含分散染料,也可以分散染料的一部分露出于树脂颗粒的表面。
据此,通过使用富于柔软性的尿烷树脂,对涂膜也赋予了柔软性。因此,在具有柔软性的记录介质上记录时,即使弯折记录介质,涂膜的追随性提高,结果,不易产生涂膜裂纹。
树脂颗粒中的尿烷树脂的质量相对于分散染料的质量优选为4倍以上且30倍以下。据此,尿烷树脂的质量相对于分散染料的质量为4倍以上,则分散染料分散在尿烷树脂中时剩余的分散染料减少,因此能够提高涂膜的发色性,另外,尿烷树脂的质量相对于分散染料的质量为30倍以下,则相对于尿烷树脂包含足够量的分散染料,因此能够提高涂膜的发色性。
作为分散染料,例如可列举:C.I.(Colour Index Generic Name,颜料索引通用名称)分散黄1、3、4、5、7、9、13、23、24、30、33、34、42、43、44、49、50、51、54、56、58、60、61、63、64、66、68、71、74、76、79、82、83、85、86、88、90、91、93、98、99、100、104、108、114、116、118、119、122、124、126、135、140、141、149、154、160、162、163、164、165、179、180、182、183、184、186、192、198、199、201、202、204、210、211、215、216、218、224、227、231、232;C.I.分散橙1、3、5、7、11、13、17、20、21、25、29、30、31、32、33、37、38、42、43、44、45、46、47、48、49、50、53、54、55、56、57、58、59、61、66、71、73、76、78、80、89、90、91、93、96、97、119、127、130、139、142;C.I.分散红1、4、5、7、11、12、13、15、17、27、43、44、50、52、53、54、55、56、58、59、60、65、72、73、74、75、76、78、81、82、86、88、90、91、92、93、96、103、105、106、107、108、110、111、113、117、118、121、122、126、127、128、131、132、134、135、137、143、145、146、151、152、153、154、157、159、164、167、169、177、179、181、183、184、185、188、189、190、191、192、200、201、202、203、205、206、207、210、221、224、225、227、229、239、240、257、258、、277、278、279、281、288、298、302、303、310、311、312、320、324、328、362、364;C.I.还原红41;C.I.分散紫1、4、8、23、26、27、28、31、33、35、36、38、40、43、46、48、50、51、52、56、57、59、61、63、69、77;C.I.分散绿9;C.I.分散棕1、2、4、9、13、19;C.I.分散蓝3、7、9、14、16、19、20、24、26、27、35、43、44、54、55、56、58、60、62、64、71、72、73、75、79、81、82、83、87、91、92、93、94、95、96、102、106、108、112、113、115、118、120、122、125、128、130、139、141、142、143、146、148、149、153、154、158、165、167、171、173、174、176、181、183、185、186、187、189、197、198、200、201、205、207、211、214、224、225、257、259、267、268、270、284、285、287、288、291、293、295、297、301、315、330、333、359、360;C.I.分散黑1、3、10、24等。
分散染料可以单独使用一种,也可以将两种以上组合使用。
1.2.水
水作为树脂颗粒的分散介质发挥功能。作为水,例如可以使用RO(ReverseOsmosis,反渗透水)水、蒸馏水、离子交换水等纯水。
1.3.其他成分
除上述成分以外,色料分散液还可包含其它成分。作为其他成分,例如可列举:分散染料以外的着色剂、尿烷树脂以外的树脂材料、各种分散剂、乳化剂或表面活性剂、水溶性有机溶剂、渗透剂、干燥抑制剂、pH调节剂、乙二胺四乙酸盐等螯合剂、防腐剂·防霉剂、防锈剂等。作为防腐剂·防霉剂,例如可以优选使用分子内具有异噻唑啉环结构的化合物。需要说明的是,也可以使色料分散液中不包含上述其他成分,而在由色料分散液制备油墨时添加。
1.3.1.pH调节剂
作为pH调节剂,没有特别限制,例如可列举:硫酸、盐酸、硝酸等无机酸;氢氧化锂、氢氧化钠、氢氧化钾、氨等无机碱;己二酸、柠檬酸、琥珀酸等有机酸;以及三乙醇胺、二乙醇胺、单乙醇胺、三丙醇胺等有机碱等。pH调节剂可以单独使用一种,也可以混合两种以上使用。
1.3.2.表面活性剂
作为表面活性剂,没有特别限制,例如可列举:阴离子型表面活性剂、阳离子型表面活性剂、非离子型表面活性剂等。
作为阴离子型表面活性剂,例如可列举:月桂酸钠、硬脂酸钠、油酸钠等高级脂肪酸盐类;十二烷基硫酸钠、月桂基硫酸钠、十六烷基硫酸钠、硬脂基硫酸钠、油基硫酸钠等烷基硫酸酯盐类;辛醇硫酸酯钠、月桂醇硫酸酯钠、月桂醇硫酸酯铵等高级醇硫酸酯盐类;乙酰基醇硫酸酯钠等脂肪族醇硫酸酯盐类;十二烷基苯磺酸钠、月桂基苯磺酸钠、十六烷基苯磺酸钠、硬脂基苯磺酸钠、油基苯磺酸钠等烷基苯磺酸盐类;异丙基萘磺酸钠等烷基萘磺酸盐类;烷基二苯基醚二磺酸钠等烷基二苯基醚二磺酸盐类;月桂基磷酸钠、硬脂基磷酸钠等烷基磷酸酯盐类;月桂基醚硫酸钠的聚环氧乙烷加成物、月桂基醚硫酸铵的聚环氧乙烷加成物、月桂基醚硫酸三乙醇胺的聚环氧乙烷加成物等烷基醚硫酸盐的聚环氧乙烷加成物类;壬基苯基醚硫酸钠的聚环氧乙烷加成物等烷基苯基醚硫酸盐的聚环氧乙烷加成物类;月桂基醚磷酸钠的聚环氧乙烷加成物等烷基醚磷酸盐的聚环氧乙烷加成物类;壬基苯基醚磷酸钠的聚环氧乙烷加成物等烷基苯基醚磷酸盐的聚环氧乙烷加成物类;全氟烷基磺酸盐,全氟烷基羧酸盐,全氟烷基磷酸酯等。
作为阳离子型表面活性剂,例如可列举:月桂基三甲基氯化铵、十六烷基三甲基氯化铵、十六烷基三甲基溴化铵、硬脂基三甲基氯化铵、二十二烷基三甲基氯化铵、二硬脂基二甲基氯化铵、羊毛脂衍生的季铵盐等季铵盐类;氯化月桂基吡啶鎓、溴化月桂基吡啶鎓、氯化十六烷基吡啶鎓等吡啶鎓盐类;2-硬脂基-羟乙基-2-咪唑啉衍生物等咪唑啉鎓盐类;N,N-二乙基-硬脂酰胺-甲胺盐酸盐、聚氧乙烯硬脂胺等胺盐类等。
作为非离子型表面活性剂,例如可列举:聚乙二醇十六烷基醚、聚乙二醇硬脂基醚、聚乙二醇油基醚、聚乙二醇二十二烷基醚等聚乙二醇烷基醚类;聚乙二醇聚丙二醇十六烷基醚、聚乙二醇聚丙二醇癸基十四烷基醚等聚乙二醇聚丙二醇烷基醚、聚乙二醇辛基苯基醚、聚乙二醇壬基苯基醚等聚乙二醇烷基苯基醚类;乙二醇单硬脂酸酯、乙二醇二硬脂酸酯、硬脂酸二乙二醇酯、二硬脂酸聚乙二醇酯、单月桂酸聚乙二醇酯、单硬脂酸聚乙二醇酯、单油酸聚乙二醇酯等聚乙二醇脂肪酸酯类;单肉豆蔻酸甘油酯、单硬脂酸甘油酯、单异硬脂酸甘油酯、二硬脂酸甘油酯、二油酸甘油酯等甘油脂肪酸酯类;脱水山梨糖醇单棕榈酸酯、脱水山梨糖醇单硬脂酸酯、脱水山梨糖醇三硬脂酸酯、脱水山梨糖醇单油酸酯、脱水山梨糖醇三油酸酯等脱水山梨糖醇脂肪酸酯类;单硬脂酸甘油酯的聚环氧乙烷加成物、单油酸甘油酯的聚环氧乙烷加成物等甘油脂肪酸酯的聚环氧乙烷加成物类;脱水山梨糖醇单棕榈酸酯的聚环氧乙烷加成物、脱水山梨糖醇单硬脂酸酯的聚环氧乙烷加成物、脱水山梨糖醇三硬脂酸酯的聚环氧乙烷加成物、脱水山梨糖醇单油酸酯的聚环氧乙烷加成物、脱水山梨糖醇三油酸酯的聚环氧乙烷加成物等脱水山梨糖醇脂肪酸酯的聚环氧乙烷加成物类;山梨糖醇单月桂酸酯的聚环氧乙烷加成物、山梨糖醇四硬脂酸酯的聚环氧乙烷加成物、山梨糖醇六硬脂酸酯的聚环氧乙烷加成物、山梨糖醇四油酸酯的聚环氧乙烷加成物等山梨糖醇脂肪酸酯的聚环氧乙烷加成物类;蓖麻油的聚环氧乙烷加成物类;2,4,7,9-四甲基-5-癸炔-4,7-二醇和2,4,7,9-四甲基-5-癸炔-4,7-二醇的烯化氧加成物以及2,4-二甲基-5-癸炔-4-醇和2,4-二甲基-5-癸炔-4-醇的烯化氧加成物、全氟烷基环氧乙烷加成物、聚硅氧烷系化合物、聚醚改性有机硅氧烷等。
表面活性剂可以单独使用一种,也可以混合两种以上使用。
1.3.3.水溶性有机溶剂
作为水溶性有机溶剂,没有特别限制,例如可列举:甘油;乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、1,3-丙二醇、1,2-丁二醇、1,2-戊二醇、1,2-己二醇、1,4-丁二醇、1,5-戊二醇、3-甲基-1,5-戊二醇、1,6-己二醇等二醇类;乙二醇单甲醚、乙二醇单乙醚、二乙二醇单甲醚、二乙二醇单乙醚、丙二醇单甲醚、丙二醇单乙醚、二丙二醇单甲醚、二丙二醇单乙醚、三乙二醇单甲醚、三乙二醇单丁醚等二醇单醚类;2-吡咯烷酮、N-甲基-2-吡咯烷酮、N-乙基-2-吡咯烷酮等含氮溶剂;甲醇、乙醇、正丙醇、异丙醇、正丁醇、2-丁醇、叔丁醇、异丁醇、正戊醇、2-戊醇、3-戊醇及叔戊醇等醇类。水溶性有机溶剂可以单独使用一种,也可以两种以上并用。
1.3.4.尿烷树脂以外的树脂材料
色料分散液还可以包含尿烷树脂以外的其他树脂。作为其他树脂,没有特别限制,例如可列举:阴离子型树脂、阳离子型树脂或非离子型树脂。包含这样的树脂,能够使树脂颗粒固定于记录介质。
作为阳离子型树脂,没有特别限制,例如可列举:阳离子淀粉等淀粉衍生物、阳离子型的尿烷树脂、阳离子型的烯烃树脂以及阳离子型的烯丙胺树脂。
作为阴离子型树脂的例子,可列举:羧甲基纤维素盐、粘胶等纤维素衍生物、藻酸盐、阿拉伯胶、黄蓍胶、木质素磺酸盐等天然树脂类。
作为非离子型树脂,没有特别限制,例如可列举:丙烯酸树脂、苯乙烯-丙烯酸树脂、尿烷树脂、酯树脂、烯烃树脂以及乙酸乙烯酯树脂。
1.4.色料分散液的制造方法
色料分散液的制造方法具有:乳化悬浮液制备工序,将含有分散染料、尿烷树脂和有机溶剂的第一组合物与包含水的第二组合物混合来制备乳化悬浮液;以及有机溶剂除去工序,从乳化悬浮液中除去有机溶剂的至少一部分。另外,其他成分可以混合在第二组合物中,也可以在有机溶剂除去工序后混合。
首先,准备含有分散染料、尿烷树脂和有机溶剂的第一组合物。第一组合物可以将各成分同时混合来制备,也可以分两个以上的阶段将各成分混合来制备。
例如,可以在制备尿烷树脂与分散染料的混揉物后,将该混揉物与有机溶剂混合,以使尿烷树脂和分散染料溶解或分散。
作为有机溶剂,例如可以优选使用25℃下相对于水的溶解度为0.1g/100gH2O以上且30g/100gH2O以下的有机溶剂。
作为这种有机溶剂,例如可列举:甲乙酮、甲基异丙基酮等酮类;乙酸乙酯、乙酸丁酯、乙酸异丙酯等酯类等,可以使用选自它们中的一种,或将两种以上组合使用。
另外,有机溶剂优选溶解或分散尿烷树脂,同时在后面的工序中容易脱溶剂的有机溶剂。因此,优选沸点比较低的有机溶剂。
从这样的观点出发,作为有机溶剂,优选甲乙酮、乙酸乙酯,更优选甲乙酮。
1.4.1.乳化悬浮液制备工序
在乳化悬浮液制备工序中,将第一组合物和包含水的第二组合物混合,来制备乳化悬浮液。
这样得到的乳化悬浮液是包含分散染料、尿烷树脂和有机溶剂的分散质分散在水系分散介质中的状态。
第二组合物至少包含水即可,例如可以使用纯水,也可以使用包含水以外的成分的液体。
作为第二组合物中所含的水以外的成分,例如可列举上述pH调节剂中的碱性成分。第二组合物包含碱性成分,能够中和尿烷树脂所具有的羧基,由此,尿烷树脂的亲水性提高。
需要说明的是,在混合第一组合物和第二组合物之前,可以将碱性成分与第一组合物混合。在该情况下,也能够得到与上述同样的效果。
由此,能够更好地使尿烷树脂亲水化,能够使最终得到的树脂颗粒的粒度分布更窄。
作为碱性成分,例如可以使用选自无机碱和有机碱中的一种,或将两种以上组合使用。
第一组合物与第二组合物的混合例如可以通过向第一组合物供给第二组合物来进行,也可以通过向第二组合物供给第一组合物来进行,但优选通过向第一组合物滴加第二组合物来进行。由此,能够更好地得到乳化悬浮液。
另外,第一组合物与第二组合物的混合优选通过边搅拌第一组合物,边向该第一组合物供给第二组合物来进行。由此,能够更好地得到乳化悬浮液。
1.4.2.有机溶剂除去工序
在有机溶剂除去工序中,从乳化悬浮液中除去至少一部分有机溶剂。由此,形成含有与构成色料分散液的树脂颗粒对应的分散染料和尿烷树脂的固体状颗粒。
有机溶剂除去工序例如通过加热乳化悬浮液或将乳化悬浮液置于减压环境下来进行。
水系的分散介质中分散有有机溶剂除去工序中得到的含有分散染料和尿烷树脂的固体状树脂颗粒的色料分散液可以直接作为本实施方式的油墨,也可以将该色料分散液与其他成分混合后作为本实施方式的油墨。
另外,在有机溶剂除去工序之后,可以实施洗涤、干燥等后处理工序。由此,能够除去不需要的成分,能够更可靠地得到组成调整后的油墨。
有机溶剂除去工序中得到的色料分散液中所含的树脂颗粒的洗涤例如能够通过以下方式来进行:使用离心分离机、压滤机、带式过滤器等分离手段,从构成该色料分散液的分散液中分离而得到微粒滤饼后,将该微粒滤饼在水中搅拌、分散,再脱水。
脱水后,可以根据需要进行干燥处理。干燥处理例如可以使用圆锥型螺带式干燥机(大川原制作所公司制造)、NAUTA混合机(细川密克朗公司制造)等混合真空干燥机、流化床干燥机(大川原制作所公司制造)、振动流化床干燥机(中央化工机公司制造)等流化床型干燥机等。
进行脱水处理、干燥处理时,通过将洗涤后的树脂颗粒与至少包含水的其他成分混合,能够得到上述本实施方式的色料分散液。
需要说明的是,在有机溶剂除去工序中,将乳化悬浮液中所含的有机溶剂,特别是乳化悬浮液的分散质中所含的有机溶剂的至少一部分除去即可,无需完全除去。即使在这种情况下,通常也能够通过洗涤、干燥等后处理工序充分除去残留的有机溶剂。另外,在最终制备出的油墨中,有机溶剂少量的话也可以残存。
2.喷墨记录用油墨组合物
本实施方式所涉及的喷墨记录用油墨组合物包含上述色料分散液、水和其他成分。
相对于油墨的总质量,油墨中的树脂颗粒的含量优选为10质量%以上且20质量%以下。
由于油墨中的树脂颗粒的含量为10质量%以上,因此能够在记录时形成涂膜,提高在记录介质上的定影性。由于油墨中的树脂颗粒的含量为20质量%以下,因此涂膜的膜结构整齐,能够维持涂膜的强度。
2.1.水
油墨还可以包含水。作为水,没有特别限制,可列举色料分散液中例示的水。
2.2.其他成分
油墨还可以包含其他成分。作为其他成分,没有特别限制,可列举色料分散液中例示的其他成分。
2.2.1.pH调节剂
油墨还可以包含pH调节剂。作为pH调节剂,没有特别限制,可列举色料分散液中例示的pH调节剂。油墨中的pH调节剂可以是源自色料分散液混合的pH调节剂,也可以是在制备油墨时另外添加的pH调节剂。
2.2.2.表面活性剂
油墨还可以包含表面活性剂。作为表面活性剂,没有特别限制,可列举色料分散液中例示的表面活性剂。油墨中的表面活性剂可以是源自色料分散液混合的表面活性剂,也可以是在制备油墨时另外添加的表面活性剂。
2.2.3.水溶性有机溶剂
油墨还可以包含水溶性有机溶剂。作为水溶性有机溶剂,没有特别限制,可列举色料分散液中例示的水溶性有机溶剂。油墨中的水溶性有机溶剂可以是源自色料分散液混合的水溶性有机溶剂,也可以是在制备油墨时另外添加的水溶性有机溶剂。
为了更稳定地进行利用喷墨方法的油墨液滴喷出,作为水溶性有机溶剂,优选甘油、二醇类或二醇单醚类,尤其优选二乙二醇、丙二醇、三乙二醇单丁醚和甘油。
2.3.喷墨记录用油墨组合物的制造方法
喷墨记录用油墨组合物通过混合上述各成分,并充分搅拌以使各成分均匀混合来制造。搅拌后,可以根据需要实施过滤。
3.喷墨记录装置
喷墨记录装置是将油墨喷出并附于记录介质的装置。利用喷墨方式喷出油墨可以使用喷墨打印机等公知的喷墨记录装置来进行。作为喷出机构,可以使用压电方式,或利用加热油墨而产生的泡使油墨喷出的方式等。其中,从喷墨记录用油墨组合物不易变质等观点出发,优选压电方式。
4.记录介质
记录介质根据由油墨和记录介质制成的印刷物的用途等适当选择。作为记录介质的形成材料,没有特别限制,例如可列举:聚氯乙烯(氯乙烯树脂)、聚丙烯、聚乙烯、聚碳酸酯、二乙酸纤维素、三乙酸纤维素、丙酸纤维素、丁酸纤维素、乙酸丁酸纤维素、硝酸纤维素、聚对苯二甲酸乙二醇酯等聚酯类;聚乙烯、聚苯乙烯、聚丙烯、聚碳酸酯、聚乙烯醇缩醛、聚酰胺、尿烷树脂、丙烯酸树脂等树脂材料以及对它们的表面进行了加工处理的材料;玻璃、纸、金属、陶瓷、皮革、木材陶瓷;或由它们中的至少1种构成的纤维、丝绸、羊毛、棉、麻、聚酯、聚酰胺、丙烯酸纤维、聚氨酯、纤维素、棉绒、人造丝、铜氨丝、醋酯纤维等各种天然纤维、合成纤维、半合成纤维等,可以使用选自它们中的一种,或将两种以上组合使用。
作为记录介质的形态,例如可列举:卷状或单张状的片、板及布等,也可以使用具有球状、长方体形状等立体形状的物体。
5.记录方法
记录方法是使用喷墨记录装置喷出油墨,并将油墨附于记录介质的方法。此时,可以并用多种喷墨记录用油墨组合物,也可以并用喷墨记录用油墨组合物以外的油墨。
根据本实施方式,能够得到以下的效果。
在油墨中,能够提高储存稳定性,提高涂膜的柔软性。即,能够提供一种储存稳定性优异、提高了涂膜的柔软性的油墨。
6.实施例和比较例
下面,将示出实施例和比较例,以对本发明的效果进行更具体的描述。需要说明的是,本发明不受以下实施例的任何限制。
与实施例1至实施例12以及比较例1和比较例2相关的组成如表1至表4所示。详细地说,表1是示出尿烷树脂中使用的聚酯多元醇PE1至PE6和PEA的组成的表。表2是示出作为尿烷树脂的树脂1至树脂9和树脂B的组成和酸值的表。表3是示出包含树脂1至树脂9、树脂B和聚酯多元醇PEA作为尿烷树脂的色料分散液1至10,以及色料分散液A、B的组成等的表。表4是示出包含作为色料分散液的分散液1至分散液10以及分散液A、B的实施例1至实施例12以及比较例1、2的油墨的组成等的表。需要说明的是,在表1、2中,没有数值记载、标记-的栏意味着不含有。另外,在表1至表4中,一部分成分的名称使用简称。各简称附注于表后。
6.1.聚酯多元醇的合成
6.1.1.共聚物PE1的合成
在具备搅拌机的300mL的分液瓶中,加入35重量份的己二酸二甲酯、35重量份的对苯二甲酸二甲酯、15重量份的偏苯三酸、17重量份的乙二醇、33重量份的3-甲基-1,5-戊二醇、4.6重量份的四丁氧基钛,在氮气氛围下以180℃加热3小时后,在减压下,边除去挥发成分边缓慢升温至220℃,共计加热5小时,得到共聚物PE1。
6.1.2.共聚物PE2~6和PEA的合成
除改变所用单体的种类和量以得到下述表1的聚酯多元醇以外,通过与共聚物PE1同样的方法合成共聚物PE2~PE6和PEA。需要说明的是,在表1中,以重量份标记各成分的配合量。
表1
AA:己二酸二甲酯
TPA:对苯二甲酸二甲酯
IPA:间苯二甲酸二甲酯
TMA:偏苯三酸
BTC:均苯三甲酸
EG:乙二醇
DEG:二乙二醇
BisA:双酚A
MPD:3-甲基-1,5-戊二醇
NPG:新戊二醇
6.2.尿烷树脂的合成
6.2.1.树脂1的合成
在具备搅拌机和滴液漏斗的500mL的分液瓶中加入100重量份的PE1,在氮气氛围下边加热至80℃,边滴加15重量份的甲苯二异氰酸酯。之后,在120℃下加热5小时,用FT-IR(Fourier Transform Infrared Spectroscopy,傅里叶变换红外光谱)确认来自异氰酸酯的吸收消失,反应结束。由此得到树脂1。通过后述的酸值测定来测定树脂1的酸值,结果为18KOHmg/g。
6.2.2.树脂2~树脂9和树脂B的合成
除改变所用单体的种类和量以得到下述表2的尿烷树脂以外,通过与树脂1同样的方法合成树脂2~树脂9和树脂B。需要说明的是,在表2中,以重量份标记各成分的配合量。
表2
PTMG:聚丁二醇1000
DMPA:二羟甲基丙酸
TDI:甲苯二异氰酸酯
HDI:六亚甲基二异氰酸酯
HXDI:1,3-双(异氰酸根合甲基)环己烷
IPDI:异佛尔酮二异氰酸酯
HMDI:二环己基甲烷-4,4'-二异氰酸酯
6.2.3.酸值测定
酸值测定可以通过以下方式测定:在将得到的树脂溶解于四氢呋喃的溶液中滴加乙醇性氢氧化钾,确认相对于供给的树脂的质量的中和所需的氢氧化钾的质量。在酸值的测定中,例如可以适用GT-200(日东精工分析科学公司制造)。
6.3.色料分散液的制备
6.3.1.分散液1的制备
在具备搅拌机的500mL的分液瓶中加入50重量份的树脂1、50重量份的乙酸乙酯、1重量份的分散红60、2.4重量份的三乙醇胺,并搅拌。加入100质量份的纯水混合后,在减压下蒸除乙酸乙酯,得到分散液1。
6.3.2.分散液2的制备
在具备搅拌机的500mL的分液瓶中加入50重量份的树脂1、50重量份的甲乙酮、1重量份的分散红60、2.4重量份的三乙醇胺,并搅拌。加入100质量份的纯水混合后,在减压下蒸除甲乙酮,得到分散液2。
6.3.3.分散液3~10和A、B的制备
除改变所用树脂的种类和量、溶剂和分散染料的量以得到表3的分散液以外,通过与分散液2同样的方法制备分散液3~10和A、B。需要说明的是,在表3中,各成分的使用量的单位为质量份。
表3
MEK:甲乙酮
TEA:三乙醇胺
DR60:C.I.分散红60
6.3.4.固形物浓度的测定
固形物浓度的测定可以称取例如1g等的色料分散液和油墨,根据冷冻干燥后残留的重量占冷冻干燥前的重量的比例来测定。
6.4.喷墨记录用油墨组合物的制备
根据表4制备实施例1~实施例12以及比较例1和比较例2的油墨。需要说明的是,在表4的油墨组成一栏中,各成分的使用量的单位为质量%。
表4
BYK-348:有机硅型表面活性剂,毕克化学公司制造
E1010:OLFINE E1010,炔二醇型表面活性剂,日信化学工业公司制造
PG:丙二醇
BTG:三乙二醇单丁醚
GL:甘油
DEG:二乙二醇
其中,实施例1是使用分散液1制作的油墨,其关系是分散液1使用树脂1,树脂1使用PE1。
实施例2使用分散液2。其关系是分散液2使用树脂1,树脂1使用PE1。分散液2的水准是与分散液1相比小粒径化。
实施例3使用分散液3。其关系是分散液3使用树脂2,树脂2使用PE2。树脂2以后的水准是使用六亚甲基二异氰酸酯、1,3-双(异氰酸根合甲基)环己烷、二环己基甲烷-4,4'-二异氰酸酯以及异佛尔酮二异氰酸酯中的一种。
实施例4使用分散液4。其关系是分散液4使用树脂3,树脂3使用PE3。
实施例5使用分散液3。其关系是分散液3使用树脂2,树脂2使用PE2。以后的水准是使用二羟甲基丙酸。
实施例6使用分散液2。其关系是分散液2使用树脂1,树脂1使用PE1。
实施例7使用分散液5。其关系是分散液5使用树脂4,树脂4使用PE6。
实施例8使用分散液6。其关系是分散液6使用树脂5,树脂5使用PE5。
实施例9使用分散液7。其关系是分散液7使用树脂6,树脂6使用PE3。
实施例10使用分散液8。其关系是分散液8使用树脂7,树脂7使用PE4。
实施例11使用分散液9。其关系是分散液9使用树脂8,树脂8使用PE5。
实施例12使用分散液10。其关系是分散液10使用树脂9,树脂9使用PE2。
比较例1使用分散液A。其关系是分散液A使用聚酯多元醇PEA。比较例1的水准是直接使用聚酯多元醇,而不是尿烷树脂。
比较例2使用分散液B。其关系是分散液B使用树脂B,树脂B使用PE3。比较例2的水准是使用了具有酸值高达128KOHmg/g的酸值的树脂B。
6.5.评价
对各实施例及各比较例的油墨进行如下所述的评价,其评价结果如表5所示。
6.5.1.储存稳定性
对于各实施例及各比较例的油墨,分别将5g放入9mL的样品瓶中,在60℃下放置120小时。之后,使用FPIA-3000(马尔文帕纳科公司制造),根据0.5μm以上的规定颗粒个数,测定粗大颗粒数。评价遵照以下基准。可以说规定颗粒个数越少,储存稳定性越优异。
A:规定颗粒个数小于100000个
B:规定颗粒个数为100000个以上且小于200000个
C:规定颗粒个数为200000个以上
6.5.2.柔软性
对于各实施例及各比较例的油墨,分别使用记录装置M105(精工爱普生公司制造),以预定的图案向作为记录介质的MCPW纸(凸版资讯公司制造)喷出。之后,将作为所得记录物的着色部的涂膜轻轻弯折成倾斜45度,以一定的速度滚动加压辊,使其往复一次,形成折痕。展开记录介质的折痕,将清洁的脱脂棉往复一次拂去。此时观察着色部上的弯曲部,按照以下的基准进行评价。可以说,弯折部因油墨脱落而产生的线越少,涂膜的柔软性越优异。
A:无法确认因油墨脱落而产生的线。
B:能够确认一部分因油墨脱落而产生的线。
C:能够确认因油墨脱落而产生的一连串的线。
6.5.3.发色性
对于各实施例及各比较例的油墨,分别使用记录装置M105(精工爱普生公司制造),以预定的图案向作为记录介质的MCPW纸(凸版资讯公司制造)喷出。之后,对于得到的记录物,使用i1(X-rite公司制造),求出各记录物附有油墨的部位的OD(Optical Density,光密度)值,按照以下基准进行评价。可以说,OD值越大,发色性越优异。
A:OD值为1.2以上。
B:OD值为1.0以上且小于1.2。
C:OD值为0.7以上且小于1.0。
D:OD值为0.5以上且小于0.7。
E:OD值小于0.5。
6.5.4.定影性
对于各实施例及各比较例的油墨,分别使用记录装置PX-M860F(精工爱普生公司制造),以预定的图案向作为记录介质的棉布帛喷出。使用洗涤用洗剂(狮王公司制造,TOPClear Liquid),在家用洗衣机(东芝生活电器公司制造,滚筒式洗涤烘干机TW-Z9500L)的标准模式下,用40℃的温水对该记录物进行洗涤,求出洗涤前后的染色部的OD值下降率,按照以下的基准进行评价。可以说,OD值下降率越低,油墨染色部在记录介质上的定影性越优异。
A:OD值的下降率小于3%。
B:OD值的下降率为3%以上且小于10%。
C:OD值的下降率为10%以上且小于30%。
D:OD值的下降率为30%以上且小于50%。
E:OD值的下降率为50%以上。
表5
6.5.5.评价结果总结
如表5所示,在实施例的油墨的储存稳定性方面,实施例1、2、3、4的评价为B。特别是实施例5、6、7、8、9、11、12的评价为A。另外,在实施例的油墨的涂膜柔软性方面,实施例1、2的评价为B,实施例3~12放热评价为A。由此表明,实施例的油墨储存稳定性及柔软性优异。
实施例的油墨的发色性在实施例3、4、5中评价为C,在实施例9、10、11、12中评价为A。另外,实施例的油墨定影性在实施例7、8、10中评价为B,在实施例9、11、12中评价为A。由此表明,实施例的油墨易于提高发色性及定影性。
另一方面,比较例的油墨储存稳定性的评价均为C,柔软性的评价也为C。由此可知,储存稳定性和柔软性难以提高。
Claims (10)
1.一种喷墨记录用油墨组合物,其特征在于,
包含用分散染料着色的尿烷树脂的树脂颗粒,
所述尿烷树脂的酸值为1KOHmg/g以上且小于100KOHmg/g。
2.根据权利要求1所述的喷墨记录用油墨组合物,其特征在于,
所述尿烷树脂包含聚酯多元醇和异氰酸酯作为原料。
3.根据权利要求2所述的喷墨记录用油墨组合物,其特征在于,
所述异氰酸酯具有两个以上异氰酸酯基作为聚合性的官能团。
4.根据权利要求3所述的喷墨记录用油墨组合物,其特征在于,
所述异氰酸酯包含六亚甲基二异氰酸酯、1,3-双(异氰酸根合甲基)环己烷、二环己基甲烷-4,4'-二异氰酸酯以及异佛尔酮二异氰酸酯中的一种以上。
5.根据权利要求2至4中任一项所述的喷墨记录用油墨组合物,其特征在于,
所述聚酯多元醇包含偏苯三酸及均苯三酸中的一种以上作为原料。
6.根据权利要求2所述的喷墨记录用油墨组合物,其特征在于,
所述尿烷树脂还包含多元醇作为原料,
所述多元醇包含二羟甲基丙酸。
7.根据权利要求1所述的喷墨记录用油墨组合物,其特征在于,
所述树脂颗粒的平均粒径为30nm以上且500nm以下。
8.根据权利要求1所述的喷墨记录用油墨组合物,其特征在于,
相对于总质量,所述树脂颗粒的含量为10质量%以上且20质量%以下。
9.根据权利要求1所述的喷墨记录用油墨组合物,其特征在于,
所述尿烷树脂的质量为所述分散染料的质量的4倍以上且30倍以下。
10.一种色料分散液,其特征在于,
包含用分散染料着色的尿烷树脂的树脂颗粒,
所述尿烷树脂的酸值为1KOHmg/g以上且小于100KOHmg/g。
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JP2017119798A (ja) * | 2015-12-28 | 2017-07-06 | 花王株式会社 | 水系インク |
CN110785468A (zh) * | 2017-06-27 | 2020-02-11 | 富士胶片株式会社 | 印染用喷墨油墨、油墨盒、油墨组及喷墨印染方法 |
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CN102939345A (zh) * | 2010-05-31 | 2013-02-20 | 东海炭素株式会社 | 聚氨酯树脂附着颜料,颜料分散组合物以及喷墨墨组合物 |
JP2017119798A (ja) * | 2015-12-28 | 2017-07-06 | 花王株式会社 | 水系インク |
CN110785468A (zh) * | 2017-06-27 | 2020-02-11 | 富士胶片株式会社 | 印染用喷墨油墨、油墨盒、油墨组及喷墨印染方法 |
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