CN101228236A - 含有水溶性表面活性添加剂和抗氧化剂的固体颜料制剂 - Google Patents
含有水溶性表面活性添加剂和抗氧化剂的固体颜料制剂 Download PDFInfo
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- CN101228236A CN101228236A CNA2006800271702A CN200680027170A CN101228236A CN 101228236 A CN101228236 A CN 101228236A CN A2006800271702 A CNA2006800271702 A CN A2006800271702A CN 200680027170 A CN200680027170 A CN 200680027170A CN 101228236 A CN101228236 A CN 101228236A
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- 238000001556 precipitation Methods 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000012063 pure reaction product Substances 0.000 description 1
- KXXXUIKPSVVSAW-UHFFFAOYSA-K pyranine Chemical compound [Na+].[Na+].[Na+].C1=C2C(O)=CC(S([O-])(=O)=O)=C(C=C3)C2=C2C3=C(S([O-])(=O)=O)C=C(S([O-])(=O)=O)C2=C1 KXXXUIKPSVVSAW-UHFFFAOYSA-K 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 150000003470 sulfuric acid monoesters Chemical class 0.000 description 1
- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- VSAISIQCTGDGPU-UHFFFAOYSA-N tetraphosphorus hexaoxide Chemical compound O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- NZFNXWQNBYZDAQ-UHFFFAOYSA-N thioridazine hydrochloride Chemical compound Cl.C12=CC(SC)=CC=C2SC2=CC=CC=C2N1CCC1CCCCN1C NZFNXWQNBYZDAQ-UHFFFAOYSA-N 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- JSPLKZUTYZBBKA-UHFFFAOYSA-N trioxidane Chemical compound OOO JSPLKZUTYZBBKA-UHFFFAOYSA-N 0.000 description 1
- 235000013799 ultramarine blue Nutrition 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- AVWRKZWQTYIKIY-UHFFFAOYSA-N urea-1-carboxylic acid Chemical group NC(=O)NC(O)=O AVWRKZWQTYIKIY-UHFFFAOYSA-N 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- UQMZPFKLYHOJDL-UHFFFAOYSA-N zinc;cadmium(2+);disulfide Chemical compound [S-2].[S-2].[Zn+2].[Cd+2] UQMZPFKLYHOJDL-UHFFFAOYSA-N 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及包含如下组分作为基本组分的固体颜料制剂:(A)45%~90%重量的至少一种包含下述物质的赋予颜色的组分:(A1)5%~100%重量的至少一种颜料和(A2)0%~95%重量的至少一种本身无色的填料,(B)5%~50%重量的至少一种水溶性表面活性添加剂,其选自含有氧化烯基团的添加剂(B1)和不含氧化烯基团的添加剂(B2),其中含有氧化烯基团的添加剂(B1)在颜料制剂中的比例等于和大于5%重量,以及(C)0.1%~5%重量的抗氧化剂。还公开了所述颜料制剂的制备和该颜料制剂在着色高分子有机或无机材料以及塑料材料中的用途。
Description
本发明涉及包含如下组分作为基本组分的固体颜料制剂
(A)45%~90%重量的至少一种包含下述物质的赋予颜色的组分:
(A1)5%~100%重量的至少一种颜料和
(A2)0%~95%重量的至少一种无本色的填料,
(B)5%~50%重量的至少一种选自下组的水溶性表面活性添加剂:含有氧化烯基团的添加剂(B1)和不含氧化烯基团的添加剂(B2),其中含有氧化烯基团的添加剂(B1)占颜料制剂的至少5%重量,以及
(C)0.1%~5%重量的抗氧化剂。
本发明还涉及这些颜料制剂的制备及它们在着色大分子有机和无机材料以及塑料中的应用。
与液体颜料制剂一样,通过搅拌或摇振简单分散在液体应用介质中的固体颜料制剂(即具有搅入特性的颜料制剂)变得日益重要。
WO-A-03/64540、03/66743、04/00903、04/29159、04/46251和04/50770以及在先德国专利申请102005005846.9和102005005975.9描述了包含基于聚醚的非离子表面活性添加剂和/或基于这些聚醚的酸酯、基于烯属不饱和羧酸的聚合物和/或基于聚氨酯的阴离子水溶性表面活性添加剂以及还包含填料并具有此搅入特性的颜料制剂。
制备固体颜料制剂的一个必要步骤是:当颜料精细分散且将所有成分混合时,将产生的水悬浮体干燥。然而,含有氧化烯基团的表面活性添加剂在尤其是基于铁氧化物的无机颜料存在下在>80℃这样的低干燥温度下倾向于分解。它们的分解自身表现在干燥材料的温度突然增加高达300℃。因此存在安全隐患。
本发明的目的是弥补该问题,并提供不仅具有所有有利性能特性而且在技术上生产安全的固体颜料制剂。
我们已经发现,上述目的通过包含如下组分作为基本组分的颜料制剂得以实现,
(A)45%~90%重量的至少一种包含下述物质的赋予颜色的组分:
(A1)5%~100%重量的至少一种颜料和
(A2)0%~95%重量的至少一种无本色的填料,
(B)5%~50%重量的至少一种选自下组的水溶性表面活性添加剂:含有氧化烯基团的添加剂(B1)和不含氧化烯基团的添加剂(B2),其中含有氧化烯基团的添加剂(B1)占颜料制剂的至少5%重量,以及
(C)0.1%~5%重量的抗氧化剂。
本发明还提供一种制备这些颜料制剂的方法,该方法包括:首先将所述颜料(A1)以包含所述抗氧化剂(C)和部分或全部添加剂(B)的水悬浮体进行湿粉碎,如果需要的话在所述颜料(A1)的所述湿粉碎之前或之后将所述填料(A2)加入到所述悬浮体中,然后干燥所述悬浮体,如果合适的话该干燥在加入所述添加剂(B)的其余部分之后进行。
本发明进一步提供一种着色大分子有机或无机材料的方法,其包括通过搅拌或摇振将颜料制剂掺入到所述材料中。
本发明最后提供一种着色塑料材料的方法,其包括通过挤出、辊压、捏合或研磨将这些颜料制剂掺入到所述塑料材料中。
本发明颜料制剂包含作为基本组分的赋予颜色的组分(A)、水溶性表面活性添加剂(B)和抗氧化剂(C)。
赋予颜色的组分(A)基于至少一种可与至少一种无本色的填料(A2)组合存在的颜料(A1)。
本发明颜料制剂中的颜料(A1)可包含有机或无机颜料。应当认识到,颜料制剂也可包含各种有机或各种无机颜料的混合物或有机和无机颜料的混合物。
颜料以细碎形式存在。因此,它们的平均粒度通常为0.1~5μm。
使用的无机颜料可以是彩色、黑色和白色颜料(有色颜料),也可以是珠光颜料。典型的有机颜料是彩色和黑色颜料。
合适的无机颜料的实例是:
-白色颜料:二氧化钛(C.I.颜料白6)、锌白、颜料级氧化锌、硫化锌、锌钡白;
-黑色颜料:氧化铁黑(C.I.颜料黑11)、铁锰黑、尖晶石黑(C.I.颜料黑27)、炭黑(C.I.颜料黑7);
-彩色颜料:氧化铬;水合氧化铬绿;铬绿(C.I.颜料绿48);钴绿(C.I.颜料绿50);群青绿;
钴蓝(C.I.颜料蓝28和36;C.I.颜料蓝72);群青色;锰蓝;
群青紫;钴紫和锰紫;氧化铁红(C.I.颜料红101);硫硒化镉(C.I.颜料红108);
硫化铈(C.I.颜料红265);钼铬红(C.I.颜料红104);群青红;
棕色氧化铁(C.I.颜料棕6和7),混合棕色尖晶石相和刚玉相(C.I.颜料棕29、31、33、34、35、37、39和40),铬钛黄(C.I.颜料棕24),铬橙;
硫化铈(C.I.颜料橙75);
黄色氧化铁(C.I.颜料黄42);镍钛黄(C.I.颜料黄53;C.I.颜料黄157、158、159、160、161、162、163、164和189);铬钛黄;尖晶石相(C.I.颜料黄119);硫化镉和硫化镉锌(C.I.颜料黄37和35);铬黄(C.I.颜料黄34);钒酸铋(C.I.颜料黄184)。
珠光颜料是其颜色作用在于干涉、反射和吸收现象的相互作用的具有单相或多相构造的片状颜料。实例是具有一个或多个涂层(尤其是金属氧化物的涂层)的铝片和铝、氧化铁和云母片。
合适的有机颜料的实例是:
-单偶氮颜料:
C.I.颜料棕25;
C.I.颜料橙5、13、36、38、64和67;
C.I.颜料红1、2、3、4、5、8、9、12、17、22、23、31、48:1、48:2、48:3、48:4、49、49:1、51:1、52:1、52:2、53、53:1、53:3、57:1、58:2、58:4、63、112、146、148、170、175、184、185、187、191:1、208、210、245、247和251;
C.I.颜料黄1、3、62、65、73、74、97、120、151、154、168、181、183和191;
C.I.颜料紫32;
-双偶氮颜料:
C.I.颜料橙16、34、44和72;
C.I.颜料黄12、13、14、16、17、81、83、106、113、126、127、155、174、176、180和188;
-双偶氮缩合颜料:
C.I.颜料黄93、95和128;
C.I.颜料红144、166、214、220、221、242和262;
C.I.颜料棕23和41;
-二并蒽酮颜料:C.I.颜料红168;
-蒽醌颜料:C.I.颜料黄147、177和199;C.I.颜料紫31;
-蒽素嘧啶颜料:C.I.颜料黄108;
-喹吖啶酮颜料:
C.I.颜料橙48和49;
C.I.颜料红122、202、206和209;
C.I.颜料紫19;
-喹诺酞酮(Chinophthalon)颜料:C.I.颜料黄138;
-二酮基吡咯并吡咯颜料:
C.I.颜料橙71、73和81;
C.I.颜料红254、255、264、270和272;
-二嗪颜料:C.I.颜料紫23和37;C.I.颜料蓝80;
-黄烷士酮颜料:C.I.颜料黄24;
-阴丹酮颜料:C.I.颜料蓝60和64;
-二氢异吲哚颜料:
C.I.颜料橙61和69;
C.I.颜料红260;
C.I.颜料黄139和185;
-异吲哚啉酮颜料:C.I.颜料黄109、110和173;
-异宜和蓝酮颜料:C.I.颜料紫31;
-金属配合物颜料:
C.I.颜料红257;
C.I.颜料黄117、129、150、153和177;
C.I.颜料绿8;
-紫环酮(Perinon)颜料:C.I.颜料橙43;C.I.颜料红194;
-苝颜料:
C.I.颜料黑31和32;
C.I.颜料红123、149、178、179、190和224;
C.I.颜料紫29;
-酞菁颜料:
C.I.颜料蓝15、15:1、15:2、15:3、15:4、15:6和16;
C.I.颜料绿7和36;
-皮蒽酮颜料:C.I.颜料橙51;C.I.颜料红216;
-吡唑喹唑酮颜料:C.I.颜料橙67;C.I.颜料红251;
-硫靛颜料:C.I.颜料红88和181;C.I.颜料紫38;
-三芳基碳颜料:
C.I.颜料蓝1、61和62;
C.I.颜料绿1;
C.I.颜料红81、81:1和169;
C.I.颜料紫1、2、3和27;
-C.I.颜料黑1(苯胺黑);
-C.I.颜料黄101(醛连氮黄);
-C.I.颜料棕22。
无机颜料作为用作本发明颜料制剂的赋予颜色的组分(A1)是特别重要的。特别合适的无机颜料是基于氧化铁,尤其是氧化铁黑(C.I.颜料黑11)还有氧化铁红(C.I.颜料红101)和氧化铁黄(C.I.颜料黄42)的颜料,该颜料可以不透明或透明形式使用。
本发明颜料制剂可包含与无本色的填料(A2)、尤其是无机填料(A2)组合的颜料(A1)。
这些无色或白色填料(A2)通常具有≤1.7的折射率。例如,白垩的折射率为1.55,重晶石为1.64,高岭土为1.56,滑石为1.57,云母为1.58,和硅酸盐为1.55。
填料(A2)与颜料(A1)一样不溶于应用介质中,并尤其选自下述化学类别(不仅是天然来源的产物,而且是例如所述合成来源的产物):
-氧化物和氢氧化物:
天然:氧化铝和氧化镁;
合成:氢氧化铝和氢氧化镁;
-二氧化硅和硅酸盐:
天然:石英、方英石、硅藻土、滑石、高岭土、硅藻土、云母、硅灰石和长石;
合成:热解法二氧化硅、沉淀二氧化硅、硅铝酸盐和煅烧硅铝酸盐;
-碳酸盐:
天然:碳酸钙和碳酸镁,如方解石、白垩、白云石和菱镁矿;
合成:沉淀碳酸钙;
-硫酸盐:
天然:硫酸钡和硫酸钙,如重晶石和石膏;
合成:沉淀硫酸钡。
填料(A2)可具有各种颗粒形状。颗粒例如可以为球形、立方体、片状或纤维。天然基填料通常具有约1~300μm的粒度。例如基于天然白垩的商品通常具有1~160μm的d50值。小于1μm的粒度通常仅存在于合成(尤其是通过沉淀)生产的填料情形。
优选用于本发明颜料制剂的填料(A2)是碳酸盐和硫酸盐,特别优选天然和沉淀白垩还有硫酸钡。这些产物可市购,例如Omyacarb和Omyalite(得自Omya)和Blanc fixe(得自Sachtleben)。
本发明颜料制剂的赋予颜色的组分(A)包含5%~100%重量的颜料(A1)和0%~95%重量的填料(A2)。当填料(A2)是赋予颜色的组分(A)的成分时,它们最小的含量基于组分(A)通常是20%重量。
本发明颜料制剂的组分(B)包含至少一种含有氧化烯基团的水溶性表面活性添加剂(B1)或所述添加剂(B1)与其它不包含氧化烯基团的水溶性添加剂(B2)的组合。在任一情形下,本发明颜料制剂包含氧化烯基团的添加剂(B1)的含量至少为5%重量。
有用的添加剂(B1)尤其包括基于聚醚的非离子添加剂(B11)和基于这些聚醚的酸性磷酸酯、膦酸酯、硫酸酯和/或磺酸酯的阴离子添加剂(B12)以及基于烯属不饱和羧酸的聚合物的烷氧化产物的阴离子添加剂(B13)。添加剂(B11)和(B13)是优选的添加剂(B1)。
除了未混合的聚氧化烯,优选聚C2-C4-氧化烯和苯基取代的C2-C4-氧化烯聚合物,尤其是聚氧化乙烯、聚氧化丙烯和聚(苯基氧化乙烯)以外,它尤其是适于用作非离子添加剂(B11)的嵌段共聚物,特别是具有聚氧化丙烯和聚氧化乙烯嵌段的嵌段共聚物,或者具有聚(苯基氧化乙烯)和聚氧化乙烯嵌段的嵌段共聚物,以及还有这些氧化烯的无规共聚物。
这些聚氧化烯可通过将这些氧化烯在起始剂分子上加聚制得,例如在饱和或不饱和的脂族和芳族醇、饱和或不饱和的脂族和芳族胺、饱和或不饱和的脂族羧酸和羧酰胺以及还有芳族羧酰胺和磺酰胺上加聚制得。芳族起始剂分子可以被C1-C20烷基或C7-C30-芳烷基取代。尽管在芳族起始剂分子的情形下,每摩尔起始剂分子使用的氧化烯数量尤其为2~100mol、优选为5~50mol、尤其为10~30mol,但每摩尔起始剂分子通常使用1~300mol、优选3~150mol的氧化烯。加聚产物可具有端OH基或封端端基,例如作为C1-C6烷基醚。
合适的脂族醇通常包含6~26个碳原子,优选8~18个碳原子并可具有未支化、支化或环状结构。实例是辛醇、壬醇、癸醇、异癸醇、十一烷醇、十二烷醇、2-丁基辛醇、十三烷醇、异十三烷醇、十四烷醇、十五烷醇、十六烷醇(鲸蜡醇)、2-己基癸醇、十七烷醇、十八烷醇(硬脂醇)、2-庚基十一烷醇、2-辛基癸醇、2-壬基十三烷醇、2-癸基十四烷醇、油醇和9-十八烷醇以及这些醇的混合物,如C8/C10、C13/C15和C16/C18醇,以及环戊醇及环己醇。特别令人感兴趣的是由天然原材料通过脂解和还原获得的饱和与不饱和的脂肪醇以及由羰基合成方法得到的合成脂肪醇。氧化烯与这些醇的加合物通常具有200~5000的平均分子量Mn。
上述芳族醇的实例不仅包括未取代的苯酚和α-与β-萘酚而且包括烷基取代产物,尤其是C1-C12烷基、优选C4-C12烷基或C1-C4烷基取代的产物,以及芳烷基取代产物,尤其是C7-C30-芳烷基取代的苯酚,如己基苯酚、庚基苯酚、辛基苯酚、壬基苯酚、异壬基苯酚、十一烷基苯酚、十二烷基苯酚、二-和三丁基苯酚以及二壬基苯酚,以及双酚A及它与苯乙烯的反应产物,尤其是在两个OH基的邻位被总计4个苯基-1-乙基取代的双酚A。
合适的脂族胺对应于上述脂族醇。此处尤其重要的是优选具有14~20个碳原子的饱和与不饱和的脂肪胺,芳族胺的实例是苯胺及其衍生物。
有用的脂族羧酸尤其包括优选含有14~20个碳原子的饱和与不饱和脂肪酸,以及完全氢化、部分氢化和未氢化的树脂酸及多官能羧酸,例如二羧酸,如马来酸。
合适的羧酰胺衍生自这些羧酸。
对于氧化烯与单官能的胺和醇的加合物,非常特别令人感兴趣的是氧化烯与至少双官能的胺和醇的加合物。
至少双官能的胺优选具有2~5个胺基且尤其具有式H2N-(R1-NR2)n-H(R1:C2-C6亚烷基;R2:氢或C1-C6烷基;n:1-5)。具体实例是:乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、1,3-丙二胺、二亚丙基三胺、3-氨基-1-亚乙基氨基丙烷、六亚甲基二胺、二六亚甲基三胺、1,6-双(3-氨基丙基氨基)己烷和N-甲基二亚丙基三胺,其中更优选六亚甲基二胺和二亚乙基三胺,最优选乙二胺。
这些胺优选首先与氧化丙烯反应,然后与氧化乙烯反应。嵌段共聚物的氧化乙烯含量通常为约10%~90%重量。
基于多官能胺的嵌段共聚物的平均分子量Mn通常为1000~40 000,优选为1500~30 000。
至少双官能的醇优选具有2~5个羟基。实例是C2-C6亚烷基二醇以及相应的二-和多亚烷基二醇,如乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,4-丁二醇、1,6-己二醇、二丙二醇和聚乙二醇、甘油和季戊四醇,其中更优选乙二醇和聚乙二醇,最优选丙二醇和二丙二醇。
特别优选的氧化烯与至少双官能的醇的加合物具有中心聚氧化丙烯嵌段,即,该加合物基于丙二醇或聚丙二醇,该二醇先与其它氧化丙烯反应后与氧化乙烯反应。嵌段共聚物的氧化乙烯含量通常为10%~90%重量。
基于多元醇的嵌段共聚物的平均分子量Mn通常为1000~20000,优选为1000~15000。
这类氧化烯嵌段共聚物是已知的并可市购,例如以商品名Tetronic、Pluronic和Pluriol(BASF),Atlas(Uniquema)、Emulgator WN和386(Lanxess)以及还有Soprophor(Rhodia)市购。
阴离子添加剂(B12)是基于这些聚醚一方面与磷酸、五氧化磷和膦酸的反应产物,而另一方面与硫酸和磺酸的反应产物(B11)。在反应中,一方面,将聚醚转化成相应的磷酸单-或二酯和膦酸酯,另一方面转化成硫酸单酯和磺酸酯。这些酸性酯优选以水溶性盐,尤其是碱金属盐,特别是钠盐和铵盐形式存在,但也可以以游离酸形式使用。
优选的磷酸酯和膦酸酯尤其衍生自烷氧基化(尤其是乙氧基化)的脂肪醇和羰基合成醇,烷基苯酚,脂肪胺,脂肪酸和树脂酸,优选的硫酸酯和磺酸酯尤其是基于烷氧基化(尤其是乙氧基化)的脂肪醇,烷基苯酚和胺,包括多官能胺,如六亚甲基二胺。
该类阴离子表面活性添加剂是已知的且可市购,例如以商品名Nekal(BASF)、Tamol(BASF)、Crodafos(Croda)、Rhodafac(Rhodia)、Maphos(BASF)、Texapon(Cognis)、Empicol(Albright&Wilson)、Matexil(ICI)、Soprophor(Rhodia)和Lutensit(BASF)市购。
阴离子添加剂(B13)是烯属不饱和羧酸的聚合物的烷氧基化产物。
以非烷氧化形式,羧酸聚合物也可用作阴离子水溶性表面活性添加剂(B21)。因此添加剂类别(B13)和(B21)现在将一起描述。
作为添加剂(B21)和(B13)的基础的不饱和羧酸聚合物尤其是烯属不饱和单羧酸和/或烯属不饱和二羧酸的均聚物和共聚物,其中这些均聚物和共聚物各自可进一步包含共聚的不带酸官能团的乙烯基单体及其盐。
可提到的含有羧基的单体和乙烯基单体的实例是:
-丙烯酸、甲基丙烯酸和巴豆酸;
-马来酸、马来酸酐、马来酸单酯、马来酸单酰胺,马来酸与二胺的反应产物,其可氧化形成含氧化胺基团的衍生物,以及富马酸,其中优选马来酸、马来酸酐和马来酸单酰胺;
-乙烯基芳族化合物,如苯乙烯、甲基苯乙烯和乙烯基甲苯;乙烯、丙烯、异丁烯、二聚异丁烯和丁二烯;乙烯基醚,如聚乙二醇单乙烯基醚;线性或支化单羧酸的乙烯基酯,如乙酸乙烯酯和丙酸乙烯酯;烯属不饱和单羧酸的烷基酯和芳基酯,尤其是丙烯酸和甲基丙烯酸酯,如丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸异丙酯、丙烯酸丁酯、丙烯酸戊酯、丙烯酸己酯、丙烯酸2-乙基己基酯、丙烯酸壬酯、丙烯酸月桂酯、丙烯酸羟乙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸异丙酯、甲基丙烯酸丁酯、甲基丙烯酸戊酯、甲基丙烯酸己酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸壬酯、甲基丙烯酸月桂酯和甲基丙烯酸羟乙酯以及丙烯酸苯酯、甲基丙烯酸苯酯、丙烯酸萘酯、甲基丙烯酸萘酯、丙烯酸苄酯和甲基丙烯酸苄酯;烯属不饱和二羧酸的二烷基酯,如马来酸二甲酯、马来酸二乙酯、马来酸二丙酯、马来酸二异丙酯、马来酸二丁酯、马来酸二戊酯、马来酸二己酯、马来酸二(2-乙基-己基)酯、马来酸二壬酯、马来酸二月桂酯、马来酸二(2-羟乙基)酯、富马酸二甲酯、富马酸二乙酯、富马酸二丙酯、富马酸二异丙酯、富马酸二丁酯、富马酸二戊酯、富马酸二己酯、富马酸二(2-乙基己基)酯、富马酸二壬酯、富马酸二月桂酯、富马酸二(2-羟乙基)酯;乙烯基吡咯烷酮;丙烯腈和甲基丙烯腈;其中优选苯乙烯、异丁烯、二异丁烯、丙烯酸酯和聚乙二醇单乙烯基醚。
作为这些单体的优选均聚物的实例,将尤其提及聚丙烯酸。
提到的单体的共聚物可以是由两种或更多种、尤其是三种不同单体构成。共聚物可以是无规共聚物、交替共聚物、嵌段共聚物或接枝共聚物。优选共聚物是苯乙烯-丙烯酸、丙烯酸-马来酸、丙烯酸-甲基丙烯酸、丁二烯-丙烯酸、异丁烯-马来酸、二聚异丁烯-马来酸和苯乙烯-马来酸共聚物,它们各自还可包含丙烯酸酯和/或马来酸酯作为额外的单体组分。
优选的是,非烷氧化的均聚物和共聚物的羧基全部和部分以盐形式存在,以可以确保在水中的溶解度。合适的例如是碱金属盐,如钠盐和钾盐以及铵盐。
非烷氧化的聚合添加剂(B21)的平均分子量Mw通常为900~250000。当然,特别适于各聚合物的分子量范围取决于它们的组成。作为举例给出对于各种聚合物之后的分子量数据:聚丙烯酸:Mw为900~250000;苯乙烯-丙烯酸共聚物:Mw为1000~50000;丙烯酸-甲基丙烯酸共聚物:Mw为1000~250000;丙烯酸-马来酸共聚物:Mw为2000~70000。
这些均聚物和共聚物的烷氧基化产物(B13)通过使用聚醚醇进行部分至(可能的话)完全酯化而形成。这些聚合物的酯化程度一般为30~80mol%。
对于酯化的有用聚醚醇尤其是聚醚醇本身,优选聚乙二醇和聚丙二醇,以及它们的单侧末端封端衍生物,尤其是相应的单醚,如单芳基醚,例如单苯基醚,尤其是单-C1-C26烷基醚,例如用脂肪醇醚化的乙二醇和丙二醇,以及聚醚胺,该聚醚胺可例如通过转化相应聚醚醇的末端OH基或通过将氧化烯加聚于脂族伯胺上而制备。此处优选聚乙二醇、聚乙二醇单醚和聚醚胺。所用的聚醚醇和它们的衍生物的平均分子量Mn通常为200~10000。
特定的表面活性特性对于添加剂(B13)或(B21)可通过改变极性与非极性基团的比例而实现。
阴离子表面活性添加剂(B13)或(B21)同样是已知的且可市购,例如以商品名Sokalan(BASF)、Joncryl(Johnson Polymer)、Alcosperse(Alco)、Geropon(Rhodia)、Good-Rite(Goodrich)、Neoresin(Avecia)、Orotan和Morez(Rohm&Haas)、Disperbyk(Byk)以及Tegospers(Goldschmidt)市购。
除了非烷氧化的羧酸聚合物(B21)--优选用作添加剂(B2),基于聚氨酯的阴离子添加剂(B22)也可用作水溶性表面活性添加剂(B2)。
对本发明而言,术语“聚氨酯”应理解为不仅是多官能异氰酸酯(B22a)与包含对异氰酸酯呈反应性的羟基的有机化合物(B22b)的纯反应产物,而且是这些通过加成其它的对异氰酸酯呈反应性的化合物(实例是带有伯氨基或仲氨基的羧酸)而经额外官能化后的反应产物。
与其它表面活性添加剂相比,这些添加剂由于它们的低离子电导率以及它们的中性pH而著名。
制备添加剂(B22)的有用多官能异氰酸酯(B22a)尤其是二异氰酸酯,但也可使用具有三个或四个异氰酸酯基的化合物。芳族和脂族异氰酸酯都可以使用。
优选的二-和三异氰酸酯的实例是:2,4-甲苯二异氰酸酯(2,4-TDI)、4,4’-二苯基甲烷二异氰酸酯(4,4’-MDI)、对苯二亚甲基二异氰酸酯、1,4-二异氰酸酯基苯、四甲基苯二亚甲基二异氰酸酯(TMXDI)、2,4’-二苯基甲烷二异氰酸酯(2,4’-MDI)与三异氰酸酯甲苯以及异佛尔酮二异氰酸酯(IPDI)、2-丁基-2-乙基五亚甲基二异氰酸酯、四亚甲基二异氰酸酯、六亚甲基二异氰酸酯、十二亚甲基二异氰酸酯、2,2-双(4-异氰酸酯基环己基)丙烷、三甲基己烷二异氰酸酯、2-异氰酸酯基丙基环己基异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯、2,2,4-三甲基六亚甲基二异氰酸酯、2,4’-亚甲基双(环己基)二异氰酸酯、顺式-环己烷1,4-二异氰酸酯、反式-环己烷1,4-二异氰酸酯和4-甲基环己烷1,3-二异氰酸酯(H-TDI)。
应当理解的是,可使用异氰酸酯(B22a)的混合物。例如可提到:2,4-甲苯二异氰酸酯和三异氰酸酯基甲苯的结构异构体的混合物,例如是80mol%的2,4-甲苯二异氰酸酯与20mol%的2,6-甲苯二异氰酸酯的混合物;顺式-和反式-环己烷1,4-二异氰酸酯的混合物;2,4-或2,6-甲苯二异氰酸酯与脂族二异氰酸酯如六亚甲基二异氰酸酯和异佛尔酮二异氰酸酯的混合物。
有用的对异氰酸酯呈反应性的有机化合物(B22b)优选包括每分子具有至少两个对异氰酸酯呈反应性的羟基的化合物。然而,可用作(B22b)的化合物进一步包括每分子仅具有一个对异氰酸酯呈反应性的羟基的化合物。这些单官能化的化合物在与多异氰酸酯(B22a)反应时,可部分或完全替代每分子包含至少两个对异氰酸酯呈反应性的羟基的化合物。
特别优选的每分子中具有至少两个对异氰酸酯呈反应性的羟基的对异氰酸酯呈反应性的化合物(B22b)的实例现在将进行叙述。
它们是聚醚二醇、聚酯二醇、基于内酯的聚酯二醇、具有至多12个碳原子的二醇和三醇、二羟基羧酸、二羟基磺酸、二羟基膦酸、聚碳酸酯二醇、多羟基烯烃和每分子平均具有至少两个羟基的聚硅氧烷。
有用的聚醚二醇(B22b)包括例如C2-C4-氧化烯如氧化乙烯、氧化丙烯和氧化丁烯、四氢呋喃、氧化苯乙烯和/或表氯醇的均聚物和共聚物,它们可以在合适的催化剂如三氟化硼存在下获得。其它有用的聚醚二醇可通过在具有至少两个酸性氢原子的起始剂存在下(共)聚合而获得,起始剂的实例是水、乙二醇、 硫代乙二醇、巯基乙醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、1,12-十二烷二醇、乙二胺、苯胺或1,2-二-(4羟基苯基)丙烷。
特别合适的聚醚二醇(B22b)的实例是聚乙二醇、聚丙二醇、聚丁二醇和聚四氢呋喃以及还有它们的共聚物。
聚醚二醇的分子量Mn优选为250~5000,更优选为500~2500。
有用的对异氰酸酯呈反应性的化合物(B22b)进一步包括聚酯二醇(羟基聚酯),它们是公知常识。
优选的聚酯二醇(B22b)是二醇与二羧酸或它们的反应性衍生物例如酸酐或二甲基酯的反应产物。
有用的二羧酸包括饱和和不饱和脂族以及芳族二羧酸,这些二羧酸可带有额外的取代基,如卤素。优选的脂族二羧酸是包含3~22个、尤其是4~12个碳原子的饱和的未支化α,ω-二羧酸。
特别合适的二羧酸的实例是:琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、1,12-十二烷二甲酸、马来酸、马来酸酐、富马酸、衣康酸、邻苯二甲酸、间苯二甲酸、邻苯二甲酸酐、四氢化邻苯二甲酸酐、六氢化邻苯二甲酸酐、四氯邻苯二甲酸酐、内亚甲基四氢化邻苯二甲酸酐、对苯二甲酸、对苯二甲酸二甲酯和间苯二甲酸二甲酯。
有用的二醇尤其包括饱和和不饱和脂族和环脂族二醇。特别优选的脂族α,ω-二醇是未支化的并具有2~12个、尤其是2~8个、尤其是2~4个碳原子。优选的环脂族二醇衍生自环己烷。
特别合适的二醇的实例是:乙二醇、丙撑二醇、1,3-丙二醇、1,4-丁二醇、2-甲基丙烷-1,3-二醇、1,5-戊二醇、新戊二醇、1,6-己二醇、1,8-辛二醇、1,10-癸二醇、1,12-十二烷二醇、顺式-丁-2-烯-1,4-二醇、反式-丁-2-烯-1,4-二醇、2-丁炔-1,4-二醇、顺式-1,4-二(羟甲基)环己烷和反式1,4-二(羟甲基)环己烷。
聚酯二醇的分子量Mn优选为300~5000。
可用作对异氰酸酯呈反应性的化合物(B22b)的基于内酯的聚酯二醇尤其是基于具有4~22个、优选4~8个碳原子的脂族饱和的未支化ω-羟基羧酸。也可以使用在亚烷基链中的一个或多个-CH2-基团由-CH(C1-C4烷基)-替代的支化的ω-羟基羧酸。
优选的ω-羟基羧酸的实例γ-羟基丁酸和δ-羟基戊酸。
应当理解,上述二醇同样可用作对异氰酸酯呈反应性的化合物(B22b),在此情形中适用上述相同的优选情况。
三醇,尤其是具有3~12个碳原子的三醇,特别是具有3~8个碳原子的三醇,同样可用作对异氰酸酯呈反应性的化合物(B22b)。三羟甲基丙烷是特别合适的三醇的实例。
可用作对异氰酸酯呈反应性的化合物(B22b)的二羟基羧酸尤其是优选包含4~14个碳原子的脂族饱和二羟基羧酸。下式的二羟基羧酸是非常特别合适的
其中A1和A2代表相同或不同的C1-C4-亚烷基,R代表氢或C1-C4烷基。
二甲基丙酸(DMPA)是这些二羟基羧酸的特别优选的实例。
有用的对异氰酸酯呈反应性的化合物(B22b)进一步包括相应的二羟基磺酸和二羟基膦酸,如2,3-二羟基丙烷膦酸。
如此处使用的二羟基羧酸也应当包含含有多于1个羧基官能团的化合物(或者在此情形下也可为酸酐或酯官能团)。该类化合物可通过二羟基化合物与四羧酸二酐(如均苯四酸二酐或环戊烷四甲酸二酐)在加聚反应中以2∶1~1.05∶1的摩尔比反应而获得,并优选平均分子量Mn为500~10000。
有用的聚碳酸酯二醇(B22b)的实例是光气与过量二醇,尤其是具有2~12个、特别是2~8个和尤其是2~4个碳原子的未支化的饱和脂族α,ω-二醇的反应产物。
可用作对异氰酸酯呈反应性的化合物(B22b)的多羟基烯烃尤其是α,ω-二羟基烯烃,优选α,ω-二羟基丁二烯。
此外,可用作对异氰酸酯呈反应性的化合物(B22b)的聚硅氧烷每分子中平均包含至少两个羟基。特别合适的聚硅氧烷平均包含5~200个硅原子(数均)并尤其被C1-C12烷基取代,尤其是被甲基取代。
包含仅仅一个对异氰酸酯呈反应性的羟基的对异氰酸酯呈反应性的化合物(B22b)的实例尤其是脂族、环脂族和芳脂族或芳族单羟基羧酸和单羟基磺酸。
基于聚氨酯的添加剂(B22)通过化合物(B22a)和(B22b)以(B22a)对(B22b)的摩尔比通常为2∶1~1∶1、优选为1.2∶1~1∶1.2的反应制得。
关于此,如前述的对异氰酸酯呈反应性的化合物(B22b)一样,可以加入具有对异氰酸酯呈反应性的基团的其它化合物,例如二硫醇、硫醇(如硫代乙醇)、氨基醇(如乙醇胺和N-甲基乙醇胺)或二胺(如乙二胺),由此制备聚氨酯,该聚氨酯除了氨基甲酸酯基团以外,还额外带有异氰脲酸酯基团、脲基甲酸酯基团、脲基、缩二脲基、脲二酮基或碳二亚胺基。该类对异氰酸酯呈反应性的化合物的其它实例是带有至少两个伯氨基和/或仲氨基的脂族、环脂族、芳脂族或芳族羧酸和磺酸。
应当理解,也可以加入相应的具有仅仅一个对异氰酸酯呈反应性的基团的化合物,例如单醇,单伯胺和单仲胺,单氨基的羧酸和磺酸,以及硫醇。常规的使用量基于(B22a)至多为10mol%。
优选的是,反应产物(B22)中的部分或全部羧基以盐形式存在,以确保在水中的溶解度。有用的盐包括例如碱金属盐,如钠盐和钾盐,以及铵盐。
通常而言,添加剂(B22)的平均分子量Mw为500~250000。
对于添加剂(B22),特定的表面活性特性可通过改变极性与非极性基团的比例来实现。
该类阴离子表面活性添加剂(B22)是已知的且可市购,例如以商品名BorchiGEN SN95(Borchers)市购。
应当理解,可使用多种添加剂(B1)的混合物以及多种添加剂(B2)的混合物。
本发明颜料制剂的组分(C)包含抗氧化剂。
抗氧化剂(C)的存在用以在干燥步骤中稳定本发明颜料制剂,以使得它们可在≥70℃的技术敏感的温度下干燥而没有自燃危险。
尽管抗氧化剂公知是水不容性化合物,然而它们惊奇地不削弱本发明颜料制剂在水性介质中的分散性。
有用的抗氧化剂(C)的实例包括已知类别的立体位阻酚、芳族胺、硫代增效剂、亚磷酸酯和亚膦酸酯以及立体位阻胺。
基于立体位阻酚的抗氧化剂包含在OH基的邻位被至少一个叔丁基取代,尤其是在OH基的两个邻位都被叔丁基取代的苯酚,作为主要结构单元。最公知的产物包含多种这些结构单元,这些单元彼此经由各种桥连成员键合。
基于芳族胺的抗氧化剂主要是二芳基胺、氨基-酮缩合产物,例如苯胺-丙酮缩合物,以及取代的对苯二胺。
含硫增效剂的实例是二烷基二硫代氨基甲酸的金属盐,二烷基二硫代磷酸锌以及硫代二丙酸酯(尤其是二月桂基酯、二肉豆蔻基酯和二硬脂基酯)。
基于亚磷酸酯和亚膦酸酯的抗氧化剂通常是相应含磷的酸与烷基取代的、尤其是叔丁基取代的苯酚的酯。
基于立体位阻胺的抗氧化剂(HALS)作为主要结构单元包含2,6-二烷基取代的、尤其是二甲基取代的哌啶,该哌啶在4位经由宽范围的桥连成员与各种哌啶结构单元连接。
抗氧化剂通常是已知的且可市购,例如以商品名Irganox、Irgaphos、Chimassorb和Irgastab(Ciba)、Topanol(ICI)、Hostanox(Clariant)和Goodrite(Goodyear)市购。
本发明颜料制剂包含45%~90%重量的组分(A),5%~50%重量的组分(B)和0.1%~5%重量的组分(C)。
优选的是,本发明颜料制剂包含55%~90%重量的组分(A),10%~45%重量的组分(B)和0.1%~2%重量的组分(C),所述组分(A)、(B)和(C)的总量不超过100%重量。
本发明颜料制剂有利地可通过这样的同样是根据本发明的制备方法获得:首先将所述颜料(A1)以包含所述抗氧化剂(C)和部分或全部所述添加剂(B)的水悬浮体进行湿粉碎,如果需要的话在所述颜料(A1)的所述湿粉碎之前或之后将填料(A2)加入到所述悬浮体中,然后干燥所述悬浮体,如果合适的话该干燥在加入所述添加剂(B)的其余部分之后进行。
在本发明方法中,颜料(A1)可作为干粉或以压饼的形式应用。
采用的颜料(A1)优选是成品,即,颜料的初级离子的粒度已经设定到对于计划应用的所需值。在有机颜料的情形下,该颜料成品是尤其明智的,因为直接合成的粗品颜料通常不直接适合计划应用。在无机颜料的情形下,例如氧化物和矾酸铋颜料,也可在合成颜料的过程中设定初级离子的粒度,以使得所得颜料悬浮体可直接应用于本发明方法中。
由于成品颜料(A1)通常在干燥过程中或者在过滤器组件上会再附聚,因此将其以水悬浮体进行湿粉碎,例如在搅拌的介质磨中研磨。
湿粉碎的进行应当使得,部分或全部的添加剂(B)包含在已经制得的颜料制剂中;优选在湿粉碎之前加入全部量的添加剂(B)。
为了获得抗氧化剂(C)的非常均匀的分布,在湿粉碎之前加入抗氧化剂(C)也是有利的。
当使用填料(A2)时,可将其在湿粉碎之前或之后加入。如果已经具有希望的粒度分布,则优选将其在颜料(A1)的湿粉碎后才分散在颜料悬浮体中。这特别适于软填料(如白垩),该软填料在颜料研磨过程中会受到不希望的共同粉碎。相反,太粗糙颗粒填料的必需粉碎可有利地与颜料粉碎结合。
本发明颜料制剂的粒度可以控制到特定的目标值,这取决于选择用以干燥的方法--喷雾造粒和流化床干燥、喷雾干燥、在桨式干燥器中的干燥、蒸发和随后的粉碎。
喷雾和流化床造粒可以生产出平均粒度为50~5000μm、尤其是100~1000μm粗碎颗粒。喷雾干燥通常生产出平均粒度<20μm的颗粒。细碎的制剂可通过在桨式干燥器中的干燥以及通过蒸发和随后的粉碎而获得。然而,优选本发明颜料制剂呈颗粒形式。
喷雾造粒优选在使用单物料喷嘴的喷雾塔中进行。此处,悬浮体以较大液滴的形式喷雾,并且水发生蒸发。添加剂在干燥温度下熔融并因此导致形成具有特别光滑表面的基本球形的颗粒(BET值通常≤15m2/g,尤其≤10m2/g)。
喷雾塔的气体入口温度通常为180~300℃,优选为150~300℃。气体出口温度通常为70~150℃,优选70~130℃。
所得颗粒状颜料的残留水含量优选<5%重量。
本发明颜料制剂在包含液相的应用介质中因为如下原因是突出的:它们具有与液体颜料配制剂相当的优异颜色性能,尤其是关于颜色强度、亮度、色调和遮盖力,以及尤其是它们的搅入特性,即,它们可以最小的能量输入简单地通过搅拌或振摇分散到应用介质中。这尤其适用于粗碎颜料颗粒,所述颗粒构成本发明颜料制剂的优选实施方案。
与液体颜料配制剂相比,本发明颜料制剂额外具有如下优点:它们具有更高的颜料含量。尽管液体配制剂在其储存过程中倾向于发生粘度改变并不得不与防腐剂和用于增强防冻和/或防干燥(结壳)的性能的试剂混合,但本发明颜料制剂在储存时显示出非常良好的稳定性。它们关于包装、储存和运输而言在经济和生态上都是有利的。因为它们不含溶剂,因此它们在使用上更灵活。
本发明呈颗粒形式的颜料制剂因下列性能而是突出的:优异的耐磨性,最小的压紧或结块倾向,均匀的粒度分布,良好的倾倒性、流动性和计量加入性,以及在处理和应用时的无尘。
上述有利品质由所述制剂和它们的上述具有搅入特性的配对物所享有,所述配对物包含颜料和表面活性添加剂但不包含填料。它们还额外地因它们对于既定应用介质的特别有效的适应性而优越于所述颜料制剂,条件是不限制颜料和添加剂的组合。因而,由于填料的存在,甚至疏水颜料,例如炭黑也可与阴离子表面活性添加剂混合,由此可有利地用于含水应用介质中,例如含水底色漆中。本发明颜料制剂也可特别容易用于遮蔽,其中填料的稀释效果使得它们尤其容易计量加入。最后,它们包含呈非常均匀分布形式的填料,并因此显著优于一般的颜料/填料混合物。
本发明颜料制剂对任何种类的大分子有机和无机材料的着色非常有用。在本文中,液体应用介质也可以是纯含水的;可以是包含水和有机溶剂(例如醇)的混合物;或者可以仅基于有机溶剂,如醇类,二醇醚类,酮类如甲乙酮,酰胺类如N-甲基吡咯烷酮和二甲基甲酰胺,酯类如乙酸乙酯、乙酸丁酯和乙酸甲氧基丙酯,或者芳族或脂族烃类,如二甲苯、矿物油和矿物溶剂油。
如果需要的话,可以首先将制剂搅入与特定应用介质相容的溶剂中,并且该向溶剂中的搅入也可以使用最小能量输入进行,然后将其引入到该应用介质中。例如,颜料制剂在二醇或其它常用于油漆和涂料工业中的溶剂中如乙酸甲氧基丙酯中的浆体可用于使得适于含水体系的颜料制剂与烃类体系或基于硝化纤维的体系相容。
可以用本发明颜料制剂着色的材料的实例包括:涂料,例如建筑涂料、工业涂料、汽车涂料、可辐射固化涂料;油漆,包括建筑外墙和建筑内墙用漆,例如木漆、涂白漆、刷墙粉、乳胶漆;溶剂性印刷油墨,例如胶印油墨、胶印油墨、甲苯凹版印刷油墨、织物印染油墨、可辐射固化印刷油墨;水性油墨,包括喷墨油墨;滤色剂;建筑材料(通常仅在建筑材料和颗粒状颜料干混后加入水),例如硅酸盐打底体系、水泥、混凝土、灰浆、石膏;沥青,嵌缝剂;纤维素材料,例如纸张、纸板、卡纸板、木材和木材基材料,它们可以各自被涂敷或涂末道漆;粘合剂;例如用于药物工业中的成膜聚合物保护胶体;化妆品;洗涤剂。
本发明颜料制剂对于着色所有种类的塑料也是非常有用的。此处,下列塑料种类和类型可作为实例提及:
-改性的天然材料:
热固性材料,如酪蛋白塑料;热塑性塑料,如硝酸纤维素、乙酸纤维素、纤维素混合酯和纤维素醚;
-合成塑料:
缩聚物:热固性材料,如酚醛树脂、尿素树脂、硫脲树脂、蜜胺树脂、不饱和聚酯树脂、烯丙基树脂、聚硅氧烷、聚酰亚胺和聚苯并咪唑;热塑性材料,如聚酰胺、聚碳酸酯、聚酯、聚苯醚、聚砜和聚乙烯醇缩醛;
加成聚合物:热塑性材料,如聚烯烃,如聚乙烯、聚丙烯、聚-1-丁烯和聚-4-甲基-1-戊烯,离聚物,聚氯乙烯,聚偏二氯乙烯,聚甲基丙烯酸甲酯,聚丙烯腈,聚苯乙烯,聚缩醛,含氟聚合物,聚乙烯醇,聚乙酸乙烯酯和聚对二甲苯以及共聚物,如乙烯-乙酸乙烯酯共聚物、苯乙烯-丙烯腈共聚物、丙烯腈-丁二烯-苯乙烯共聚物、聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯;
聚加合物:热固性材料,如环氧树脂和交联聚氨酯;热塑性材料,如线性聚氨酯和氯化聚醚。
有利的是,塑料可通过最小的能量输入,例如通过联合挤出(优选使用单螺杆或双螺杆挤出机)、辊压、捏合或研磨而由本发明颜料制剂着色。此时塑料可以呈可塑性变形的物料或熔体,并且可加工成膜制品、膜和纤维。
本发明颜料制剂在塑料着色中也因如下性能而是突出的:全部有利的应用性能,特别是良好的颜色性能,尤其是高颜色强度和亮度,以及已经用它们着色的塑料的良好流变性,尤其是低压滤值(高过滤器寿命)和良好的纺丝性。
实施例
本发明颜料制剂的制备和测试
在150克水中通过将x克成品颜料(A1)、y克添加剂(B1)和z克抗氧化剂(C)的悬浮体(在pH值<7的情形下,通过加入25%重量的氢氧化钠水溶液调节到pH7)球磨至d50值<1μm而生产颜料制剂,然后将其在循环空气烘箱中在60℃下干燥。
为了研究本发明颜料制剂的干燥性能,测定它们的Onset温度。
Onset温度是在空气流中被加热的物质的温度超过在相同空气流中被加热的惰性参照物质的温度的加热温度。为了确保制造中的安全干燥(没有自燃),干燥温度应当比Onset温度低约50℃。
为了测定Onset温度,将10cm3的各颜料制剂的样品和作为参照样品的石墨样品以1℃/min的加热速率在2L/min空气流中进行加热,同时监测这两种样品的温度。
此外,将本发明颜料制剂进行测试。在此,它们显示出与各类似的市购含水配制剂相当的颜色强度。
下表列出了所制备的颜料制剂的组成以及还有它们各自测得的Onset温度。不包含抗氧化剂的各颜料制剂的Onset温度作为对比进行报道。所用的添加剂(B1)和抗氧化剂(C)如下:
(B1):具有中心PO嵌段的PO-EO嵌段共聚物(EO含量:50%重量;Mn:6500)
(C1):Irganox1010(Ciba)(四[亚甲基(3,5-二(叔丁基)-4-羟基氢化肉桂酸酯)]甲烷)
(C2):Irganox 1076(Ciba)(3,5-二(叔丁基)-4-羟基氢化肉桂酸十八烷酯)
(C3):Irgafos168(Ciba)(亚磷酸三[2,4-二(叔丁基苯基)酯]
表
实施例 | 颜料 | 添加剂(B1)y克 | 抗氧化剂 | Onset温度[℃] | ||
x克 | (A1) | z克 | (C) | |||
本发明1* | 84 | 黄色42(不透明) | 15 | 1 | (C1) | 194 |
对比例1 | 85 | 黄色42(不透明) | 15 | - | - | 125 |
本发明2** | 58 | 黄色42(透明) | 40 | 2 | (C1) | 185 |
对比例2 | 60 | 黄色42(透明) | 40 | - | - | 110 |
本发明3*** | 79 | 红色101(不透明) | 20 | 1 | (C1) | 205 |
对比例3 | 80 | 红色101(不透明) | 20 | - | - | 94 |
本发明4 | 79 | 黄色184 | 20 | 1 | (C1) | 294 |
对比例4 | 80 | 黄色184 | 20 | - | - | 160 |
本发明5 | 79 | 黑色11 | 20 | 1 | (C1) | 188 |
本发明6 | 79 | 黑色11 | 20 | 1 | (C2) | 178 |
本发明7 | 79 | 黑色11 | 20 | 0.50.5 | (C1)(C3) | 178 |
本发明8 | 79 | 黑色11 | 20 | 0.50.5 | (C1)(C2) | 180 |
对比例5 | 80 | 黑色11 | 20 | - | - | 150 |
*BET表面积13m2/g(BayferroxGelb 920(Lanxess))
**BET表面积90m2/g(SicotransGelb 1916(BASF))
***BET表面积6m2/g(Bayferrox Rot 130(Lanxess))
Claims (10)
1.一种包含如下组分作为基本组分的固体颜料制剂
(A)45%~90%重量的至少一种包含下述物质的赋予颜色的组分:
(A1)5%~100%重量的至少一种颜料和
(A2)0%~95%重量的至少一种无本色的填料,
(B)5%~50%重量的至少一种选自下组的水溶性表面活性添加剂:含有氧化烯基团的添加剂(B1)和不含氧化烯基团的添加剂(B2),其中含有氧化烯基团的添加剂(B1)占颜料制剂的至少5%重量,以及
(C)0.1%~5%重量的抗氧化剂。
2.根据权利要求1的颜料制剂,其中所述组分(A1)包含至少一种无机颜料。
3.根据权利要求1或2的颜料制剂,其中所述组分(A1)包含基于氧化铁的无机颜料。
4.根据权利要求1~3的颜料制剂,其中所述组分(B1)包含至少一种选自下组的水溶性表面活性添加剂:基于聚醚的非离子添加剂(B11),基于聚醚的酸性磷酸酯、膦酸酯、硫酸酯和/或磺酸酯的阴离子添加剂(B12)以及基于烯属不饱和羧酸的烷氧化聚合物的阴离子添加剂(B13)。
5.根据权利要求1~4的颜料制剂,其中所述组分(B2)包含至少一种选自基于烯属不饱和羧酸的非烷氧化聚合物(B21)和基于聚氨酯(B22)的阴离子添加剂的水溶性表面活性添加剂。
6.根据权利要求1~5的颜料制剂,其中所述组分(C)包含至少一种选自下组的抗氧化剂:立体位阻酚、芳族胺、硫代增效剂、亚磷酸酯、亚膦酸酯和立体位阻胺。
7.一种制备根据权利要求1~6的颜料制剂的方法,其包括:首先将所述颜料(A1)以包含所述抗氧化剂(C)和部分或全部所述添加剂(B)的水悬浮体进行湿粉碎,如果需要的话在所述颜料(A1)的所述湿粉碎之前或之后将所述填料(A2)加入到所述悬浮体中,然后干燥所述悬浮体,如果合适的话该干燥在加入所述添加剂(B)的其余部分之后进行。
8.一种着色大分子有机或无机材料的方法,其包括通过搅拌或摇振将根据权利要求1~6的颜料制剂掺入到所述材料中。
9.根据权利要求8的方法,用于着色涂料、油漆、包括印刷油墨在内的油墨,以及其中液相包含水、有机溶剂或水与有机溶剂的混合物的成品体系。
10.一种着色塑料材料的方法,其包括通过挤出、辊压、捏合或研磨将权利要求1~6的颜料制剂掺入到所述塑料材料中。
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EP (1) | EP1913095B1 (zh) |
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-
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2015
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CN106661341A (zh) * | 2014-05-01 | 2017-05-10 | 克罗玛夫洛技术公司 | 用于给漆料调色的固体着色剂 |
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CN108822618A (zh) * | 2018-05-25 | 2018-11-16 | 安徽猛牛彩印包装有限公司 | 一种提高耐热稳定性的印刷油墨 |
CN112513238A (zh) * | 2018-07-27 | 2021-03-16 | 美利肯公司 | 包含隐色化合物的稳定的组合物 |
CN114341276A (zh) * | 2019-08-09 | 2022-04-12 | 纳诺萨尔生产有限责任公司 | 使用具有涂覆表面的无机颗粒作为间隔件的着色和填料膏 |
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EP1913095B1 (de) | 2013-03-20 |
US20080190319A1 (en) | 2008-08-14 |
WO2007012575A2 (de) | 2007-02-01 |
US20150274977A1 (en) | 2015-10-01 |
DE102005035253A1 (de) | 2007-02-01 |
JP2009503168A (ja) | 2009-01-29 |
WO2007012575A3 (de) | 2008-01-03 |
EP1913095A2 (de) | 2008-04-23 |
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