CN101705028B - Black ink composition for inkjet - Google Patents

Black ink composition for inkjet Download PDF

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CN101705028B
CN101705028B CN 200910228091 CN200910228091A CN101705028B CN 101705028 B CN101705028 B CN 101705028B CN 200910228091 CN200910228091 CN 200910228091 CN 200910228091 A CN200910228091 A CN 200910228091A CN 101705028 B CN101705028 B CN 101705028B
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ink
black
pigment
composition
agent
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CN 200910228091
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CN101705028A (en )
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王立园
石金永
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天津兆阳纳米科技有限公司
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Abstract

The invention discloses a black ink composition, comprising dispersion solution, moisturizing agent, surfactant and deionized water, wherein, the dispersion solution is prepared by grinding colorant, dispersing agent, deionized water and other assistants, and is characterized in that the colorant at least contains black pigment C.I.P.B.7 and blue pigment C.I.Pigment Blue 61, the weight ratio of which ranges from 20:1 to 2:1. The black ink composition of the invention has the advantage that a* is less than 0 and b* is less than 0 when L* value is 50-60 in an L*a*b* colormetric system of the ink stipulated by CIE, so that the black and gray printed by the ink can not be inclined to be red, the color is neutral and the printing effect is good.

Description

喷墨用黑色墨水组合物(-)技术领域:[0001] 本发明涉及一种黑色墨水,特别是一种用于喷墨领域的黑色墨水组合物及其制备方法。 The inkjet black ink composition (-) Technical Field: [0001] The present invention relates to a black ink, particularly black ink composition and a method for preparing an ink jet field. [0002] ( 二)背景介绍:[0003] LW是人类视觉的颜色空间,它依照的是视觉唯一的原则,即在色彩空间内相同的移动量在眼睛看来造成彩色的改变感觉是一样的,是均勻色度空间。 [0002] (b) Background: [0003] LW is the color space of human vision, it is in accordance with the unique vision of the principle that the same amount of movement of the eye seems to cause a color change in the feeling is the same as in the color space , uniform color space. ΙΛ a*和b*表示描述所有可看见的参数,L*表示色调的亮度,f和b*表示色度,a*和b*可以代表正值和负值。 ΙΛ a * and b * represent a description of all parameters visible, L * indicates the brightness of the hue, f and b * represents chroma, a * and b * may represent positive and negative values. 一种色调的a*部分描述它是红或绿,a*为正表示偏红,a*为负表示偏绿;b*部分表明它是黄或蓝,b*为正表示偏黄,b*为负表示偏蓝,如果a*、b*都趋于零,表明颜色中性。 One kind of hue a * describes part which is red or green, a * is positive indicates reddish, a * represents a negative greenish; b * indicate that it is part of blue or yellow, b * represents a yellow is positive, b * negative representation bluish, if a *, b * are to zero, indicating a neutral color. [0004] 使用卤化银感光材料冲洗照片,色彩鲜艳,图像过渡自然。 [0004] The silver halide photographic materials using photographs, colorful, image natural transition. 为了达到和卤化银感光材料相同的成像效果,喷墨打印机需要不同的黑色墨水。 And silver halide photographic materials in order to achieve the same imaging results, the ink jet printer requires a different black ink. 在这其中淡黑可以使图像过渡自然,照片黑可以提高色密度和增加黑色的色阶范围。 In this one can make the image black light natural transition, photo black and color density can be increased to increase the range of gradation of black. 喷墨打印黑色墨水所用的着色剂一般采用炭黑颜料。 Ink jet printing a black colorant generally used for a carbon black pigment employed. 炭黑作为黑色颜料颜色虽然都是黑的,但是炭黑粒径研磨很小时炭黑呈红相,因为炭黑具有这一缺点:在打印时特别是低浓度打印时黑色偏红,红光现象很明显。 Although carbon black as a black pigment colors are black, but the carbon black particle size carbon black was milled very small reddish, since carbon black has the disadvantage: in particular, when printing at low concentrations reddish black printing, the phenomenon of red It is clear. 为了消除红相,可用蓝色颜料作补色剂。 In order to eliminate the red phase, it can be used as a complementary color of blue pigment agent. 对此一些专利文献有报道。 Some of this patent document have been reported. [0005] 美国专利US6565202介绍了一种由黑色墨水和CIPigment Blue 60的分散液按比例混合而成的黑色墨水组合物。 [0005] U.S. Patent No. US6565202 describes a mixing proportion of the black ink and the dispersion CIPigment Blue 60 formed by the black ink composition. 该墨水组合物中黑色颜料和蓝色颜料的比例在1.7 : 1 左右,这样蓝色颜料的所占比例过大,这样在图像打印时很容易出现黑色严重偏蓝和黑色的色密度过低。 The proportion of black pigment ink composition and a blue pigment of 1.7: 1 or so, so that the proportion of the blue pigment is excessively large, so that when the printed image is prone to severe bluish black and black color density is too low. 在本公司试验时发现当L*值在50〜60之间时黑色颜料和蓝色颜料的比例从20 : 1到20 : 2时色密度会从0.62降至0.58。 Found that L * is between 50 to 60 ratio a black pigment and a blue pigment from the value at the time of our test 20: 1 to 20: 2 when the color density will be reduced to 0.58 from 0.62. 还有蓝色颜料的添加量过大还会导致成本过高。 There adding excessive blue pigment can also lead to high costs. [0006] 美国专利US7503968介绍了一种含有炭黑、酞菁颜料和苯并咪唑酮颜料的黑色墨水组合物。 [0006] U.S. Patent No. US7503968 describes a black ink composition containing carbon black, phthalocyanine pigments, and benzimidazolone pigments. 该墨水组合物中黑色颜料、酞菁颜料和苯并咪唑酮颜料所占重量百分比分别在0. 172〜0. 287,0. 041〜0. 069和0. 032〜0. 054。 The ink composition of black pigment, a phthalocyanine pigment and benzimidazolone pigment percentage by weight, respectively 0. 172~0. 287,0. 041~0. 069 and 0. 032~0. 054. 这样由于有苯并咪唑酮颜料的存在,CIE 规定的a*值始终大于0,所以该墨水打印输出后黑色和灰色部分偏红。 Thus due to the presence of benzimidazolone pigments, the CIE a * predetermined value is always greater than 0, so the output of the black and gray ink print portion reddish. (三)发明内容:[0007] 本发明涉及一种黑色墨水,特别是一种用于喷墨领域的黑色墨水组合物,使用该墨水打印黑色文档、色块或图像时,黑色部分不偏红,颜色呈中性。 (Iii) Disclosure of the Invention: [0007] The present invention relates to a black ink, particularly black ink composition for ink jet field, when using the black ink printing a document, or a color image, partially reddish black, color neutral. [0008] 本发明的技术方案:一种黑色墨水组合物,包括分散液、保湿剂、表面活性剂和去离子水,其中分散液由着色剂、分散剂、去离子水以及其它助剂研磨制备所得,其特征在于所说的着色剂至少含有黑色颜料CIPB 7和蓝色颜料CI Pigment Blue 61,其中黑色颜料CIPB 7和蓝色颜料CI Pigment Blue 61的重量比例在20 : 1至2 : 1之间。 [0008] The aspect of the present invention: one black ink composition comprising a dispersion, humectant, surfactant and deionized water, wherein the dispersion of the colorant, the dispersant, deionized water, and other additives was prepared polishing the resulting, wherein said colorant comprises a black pigment and a blue pigment CIPB 7 CI pigment blue 61 at least, wherein the weight ratio of black pigment and a blue pigment CIPB 7 CI pigment blue 61 in 20: 1 to 2: 1 of between. [0009] 上述所说的黑色颜料CIPB 7和蓝色颜料CI Pigment Blue 61的重量比例优选10 : 1至20 : 3之间。 [0009] The said black pigment and a blue pigment CIPB 7 CI Pigment Blue 61 weight ratio of preferably between 10: 3: 1-20. [0010] 上述所说的黑色颜料CIPB 7占整个墨水的重量百分比为1〜10%。 [0010] The said black pigment CIPB 7 percentage by weight of the entire ink is 1~10%. [0011] 上述所说的黑色颜料选用以下其中一种:卡博特(Cabot)公司的Mongul-L、REGAL 400R、Monarch 1300、Monarch 900、REGAL 330R ;三菱化学公司(Mitsubishi Chemical Corporation)的MA_7、MA100、MA40 ;德固赛公司(Degussa)的Special black 4 ;哥伦比亚化学公司(Columbian Chemical)的Raven 3500、Ravenl255、Raven 3600 ultra。 [0011] The said black pigment is one of two types: Cabot (Cabot) companies Mongul-L, REGAL 400R, Monarch 1300, Monarch 900, REGAL 330R; Mitsubishi Chemical Corporation (Mitsubishi Chemical Corporation) of MA_7, MA100, MA40; Degussa (Degussa) the Special black 4; Columbian chemicals company (Columbian chemical) of Raven 3500, Ravenl255, Raven 3600 ultra. [0012] 上述所说的分散剂可选用明凌(Munzing Chemie Gmbh)公司的EDPLAN 482。 [0012] The above-mentioned dispersants may be chosen Mingling (Munzing Chemie Gmbh) companies EDPLAN 482. [0013] 上述所说的保湿剂可选用异丙醇、N-甲基-2-吡咯烷酮、2-吡咯酮、乙二醇乙醚、 乙二醇丁醚、二乙二醇乙醚、二乙二醇丁醚、三乙二醇丁醚、丙二醇丁醚和二丙二醇丁醚、丙三醇、乙二醇、二乙二醇、三乙二醇、三羟甲基丙烷、1,2-丙二醇、1,3-丙二醇、1,4_ 丁二醇、 1,5-戊二醇、1,2-己二醇、1,2,6-己三醇、聚乙二醇400、聚乙二醇600中的至少一种。 [0013] The choice of said humectant isopropanol, N- methyl-2-pyrrolidone, 2-pyrrolidone, ethylene glycol ethyl ether, ethylene glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol ether, triethylene glycol butyl ether, propylene glycol butyl ether and diethylene glycol butyl ether, glycerol, ethylene glycol, diethylene glycol, triethylene glycol, trimethylolpropane, 1,2-propanediol, 1 1,3-propanediol, 1,4_-butanediol, 1,5-pentanediol, 1,2-hexanediol, 1,2,6-hexanetriol, polyethylene glycol 400, polyethylene glycol 600 at least one. [0014] 上述所说的助剂包括pH调节剂和杀菌剂。 [0014] The above-mentioned adjuvants include pH adjusting agents and fungicides. 其中pH调节剂可选用三乙醇胺;杀菌剂可选用科莱恩公司(Clariant)的Nipacide BIT-20。 Wherein optional pH adjusting agent triethanolamine; bactericides optional Clariant (Clariant) is Nipacide BIT-20. [0015] 上述所说的表面活性剂可选用空气化工公司(Air Products)的产品Surfynol465 和Surfynol 485 中的任意一种。 [0015] The above-mentioned surfactants may be selected from any of an air Chemical Company (Air Products) products of Surfynol465 and Surfynol 485. [0016] 一种黑色墨水组合物的制备方法,其特征在于包括分散液的制备与墨水的制备, 其中:[0017]( 一)分散液的制备包括以下步骤:[0018] ①将分散剂和去离子水按照比例混合于容器中,并搅拌均勻;[0019] ②按比例加入黑色颜料和蓝色颜料,充分润湿;[0020] ③用高速剪切机将步骤②所得的分散液高速剪切0. 5〜8小时,转速为1000〜 lOOOOrpm,剪切完成后放置10〜20分钟;[0021] ④将步骤③所得的剪切分散液泵入研磨机中进行研磨分散;[0022] ⑤将步骤④中研磨机出料口所得分散液进入研磨机的储料槽,再次泵入研磨机进行循环研磨0. 5〜M小时;[0023] ⑥研磨过程中,每隔15分钟进行粒度检测,直到分散液的粒径达到要求,得到分散液。 Preparation [0016] A method for the black ink composition, wherein the ink Preparation dispersion comprising, wherein: (a) Preparation of [0017] the dispersion liquid comprises the steps of: [0018] ① dispersing agent and of deionized water in a vessel in accordance with the mixing ratio, and stir well; [0019] ② added proportionally black pigment and a blue pigment, sufficiently wetted; [0020] ③ the high-speed shear dispersion obtained in step ② High speed shear cut 0. 5 ~ 8 hours, speed 1000~ lOOOOrpm, 10-20 minutes after placing the cut is finished; [0021] ④ the resultant shear dispersing step ③ pumped into the grinding mill dispersion; [0022] ⑤ in step ④ mill feed mouth resulting dispersion mill into the hopper again pumped into the recirculation polishing grinder 0. 5~M hours; [0023] ⑥ grinding process, every 15 minutes for particle size measurement , until the particle size of the dispersion to meet the requirements to obtain a dispersion. [0024] 步骤①-③为剪切分散步骤,其中步骤③中的高速剪切主要作用是使分散剂分散乳化均勻,打碎部分黑色颜料中的较大粒子,剪切时间优选1-2小时;上述步骤④-⑥为研磨分散步骤;其中步骤④中的研磨机为销棒式研磨机,转速为600〜4200rpm,研磨介质采用直径为0. 05〜Imm的氧化锆珠,优选直径0. 05〜0. 2mm之间;所说的步骤④中的研磨目的是使黑色纳米水性颜料分散液粒径继续降低,研磨时间优选1-2小时;所说的步骤⑤ 中的出料口的温度控制在20〜40°C之间;所说的步骤⑥为颜料粒度检测,粒径要求D5tl在IOOnm 左右。 [0024] Step ①-③ shear dispersing step, wherein in the step ③ main function is to make high-speed shearing dispersing emulsification uniformly dispersing, breaking the larger part of the black pigment particles, shearing time is preferably 1-2 hours ; above step ④-⑥ the step of grinding the dispersion; wherein in the step ④ mill is a pin mill, speed 600~4200rpm, grinding media with a diameter of 0. 05~Imm zirconia beads, diameter of preferably 0. between 05~0 2mm;. ④ polishing step of said object is in the black aqueous pigment liquid dispersion of nano particle size continues to decrease, the polishing time is preferably 1-2 hours; temperature spout in said step ⑤ controlled between 20~40 ° C; ⑥ said step of detecting pigment particle size, the particle size required in IOOnm D5tl around. . [0025] ( 二)墨水的制备包括以下步骤:[0026] 按重量百分比取上述步骤⑥所制得的分散液50%,另加2-吡咯酮4%,乙二醇3%,1,2-丙二醇3%,1,2-己二醇6%,Surfynol 4651. 2%,三乙醇胺0. 2%,杀菌剂和余量去离子水,制成墨水组合物。 [0025] Preparation of (two) ink comprising the steps of: [0026] by taking the above step ⑥ weight percent of the obtained dispersion was 50%, 2-pyrrolyl ketone plus 4%, 3% ethylene glycol, 1,2 - 3% propylene glycol, 1,2-hexanediol 6%, Surfynol 4651. 2%, 0.2% triethanolamine, bactericides and the balance deionized water to prepare an ink composition. [0027] 注:D5(i :—个样品的累计粒度分布体积百分数达到50%时所对应的粒径。[0028] 本发明的优越性和技术效果在于:该墨水在CIE规定的LW色度系统中当L*值在50〜60之间时,a* < 0, b*< 0。这样该墨水打印出来黑色和灰色不会偏红,颜色呈中性,打印效果好。(四)具体实施方式:[0029] 色彩评估:[0030] 评价本发明墨水的技术效果采用CIE(Commission Internationale deL' Eclairage ;国际发光照明委员会)制定测量颜色的国际标准,对色值进行测定。CIE 制定了IAf和b*值来测量色值,这种测量方法称为CIELAB。L*代表着明度,从明亮(此时L* = 100)到黑暗(此时L* = 0)之间变化。a*值表示颜色从绿色到红色(+a*)之间变化,而b*值表示颜色从黄色(+b*)到蓝色(-b*)之间变化。[0031] 将实施例1〜3和比较例1〜3描述的墨水组合物装入墨盒,放入喷墨打印机Stylus Photo R230(爱普生公司制)在 [0027] Note: D5 (i: -. Cumulative particle size distribution of the sample volume percentage reaches 50% when the particle diameter corresponding to [0028] Technical effects and advantages of the present invention is that: the ink is specified in the CIE chromaticity LW when the system when the L * value between 50~60, a * <0, b * <0. printed out so that the ink is not reddish black and gray, neutral color, good print quality. (d) specific embodiment: [0029] the color evaluation: technical effects [0030] evaluation of the ink according to the present invention employs the CIE (Commission Internationale deL 'Eclairage; emission international Commission on illumination) color development of international standards of measurement, measured values ​​of the color developed IAf .CIE and b * values ​​measured color values, this measurement method is referred CIELAB.L * represents lightness, a change from bright (where L * = 100) to dark (where L * = 0) between a value .a * represents a change in color from green to red between (+ a *), and b * value represents a change between color from yellow (+ b *) to blue (-b *). [0031] Examples 1 ~ 3 and ink composition of Comparative Example 1 ~ 3 described in the print cartridge, into the ink jet printer Stylus Photo R230 (manufactured by Epson Corporation) in 乐凯水晶照片纸上以1440*720dpi打印样张,用爱色丽公司制的Eye-one Pro通过在光源D50,视野角2度下,当L*值在50〜60之间时测量a*、b* 值。[0032] 实施例中的“份”以重量计。[0033] 表1各实施例和比较例的配方(单位:份,重量计)[0034] 实施例1 实施例2 实施例3 比较例1 比较例2 比较例32-吡咯酮 4 4 4 4 4 4乙二醇 3 3 3 3 3 31,2-丙二醇 3 3 3 3 3 31,2-己二醇 6 6 6 6 6 6Surfynol 465 1. 2 1. 2 1. 2 1. 2 1. 2 1. 2Nipacide BIT-20 0. 2 0. 2 0. 2 0. 2 0. 2 0. 2三乙醇胺 0. 2 0. 2 0. 2 0. 2 0. 2 0. 2EDAPLAN 482 4 4 4 4 4 4水 余量 余量 余量 余量 余量 余量Carbon black 4 4 4 4 4 4C. I. Pigment Blue 61 0. 2 0. 4 0. 6 CI Pigment Blue 15:3 0. 4 Lucky crystal photo paper to 1440 * 720dpi print the sample with X-Rite manufactured by Eye-one Pro D50 light source, the visual field angle of 2 degrees, when measured in the L * value between 50~60 a *, b * values ​​[0032] Examples, "parts" are by weight embodiment [0033] table 1 formulation Examples and Comparative Examples. (unit: parts by weight) [0034] Example 1 Example Example 2 Comparative Example 3 Comparative Example 1 Comparative Example 32 - 2-pyrrolidone 444 444 3 3 3 3 3 ethylene glycol 31,2- 33333 31,2- hexylene glycol 6 6 6 6 6 6Surfynol 465 1. 2 1. 2 1. 2 1. 2 1. 2 1. 2Nipacide BIT-20 0. 2 0. 2 0. 2 0. 2 0. 2 0. 2 0.2 0.2 triethanolamine zero. 2 0. 2 0. 2 0. 2EDAPLAN 482 4 4 4 4 4 4 water balance balance balance balance balance balance Carbon black 4 4 4 4 4 4C. I. Pigment Blue 61 0. 2 0. 4 0. 6 CI Pigment Blue 15: 3 0. 4

Figure CN101705028BD00071

[0035] 共提供3个实施例,该3个实施例的前8项成分完全相同,相同成分如下表:[0036] 表2 3个实施例的前8项相同成分列表[ [0035] Example 3 were provided, the same as the prior three component embodiment 8, the same components as follows: [0036] Table 8 the same as before the component 23 of the embodiment list [

Figure CN101705028BD00072

[0039] 见表1,首先制分散液,其中将8份三菱化学(Mitsubishi ChemicalCorporation) 的黑色颜料MA-7,0.4份巴斯夫(BASF)的蓝色颜料Alkali Blue D6101 (CI Pigment Blue 61),8份明凌(Munzing Chemie Gmbh)公司的EDPLAN482,其有效成分含量85%和83. 6份去离子水用高速剪切搅拌器混合1小时至均勻后得剪切分散液,再在0. 14L容积的研磨机中对300g的剪切分散液研磨1小时,得到水性颜料分散液。 [0039] Table 1, a dispersion is first prepared in which 8 parts by Mitsubishi Chemical (Mitsubishi ChemicalCorporation) black pigment MA-7,0.4 parts by BASF (BASF) blue pigment Alkali Blue D6101 (CI Pigment Blue 61), 8 Mingling parts (Munzing Chemie Gmbh) companies EDPLAN482, its active ingredient content of 85% and 83.6 parts of deionized water were mixed for 1 hour to obtain uniformly shear dispersion with high shear mixer, then 0. 14L volume the mill dispersion of 300g shear milled for 1 hour to obtain an aqueous pigment dispersion. 颜料和分散剂的比例为1.18 : 1。 Ratio of the pigment and the dispersing agent was 1.18: 1. [0040] 将上述制备成的分散液和表2中8种添加物混合,常温下搅拌20分钟,用0. 5 μ 过滤器过滤得墨水组合物,即得到实施例产品1。 [0040] The dispersion was prepared as described above in Table 2 and 8 kinds of additives were mixed and stirred at room temperature for 20 minutes and filtered to obtain the ink composition with 0. 5 μ filter, i.e., the product obtained in Example 1. [0041] 实施例2[0042] 见表1,首先制分散液,其中将8份三菱化学(Mitsubishi ChemicalCorporation) 的黑色颜料MA-7,0.8份巴斯夫(BASF)的蓝色颜料Alkali Blue D6101 (CI Pigment Blue 61),8份明凌(Munzing Chemie Gmbh)公司的EDPLAN482,其有效成分含量85%和83. 2份去离子水用高速剪切搅拌器混合1小时至均勻后得剪切分散液,再在0. 14L容积的研磨机中对300g的剪切分散液研磨1小时,得到水性颜料分散液。 [0041] Example 2 [0042] Table 1, a dispersion is first prepared in which 8 parts by Mitsubishi Chemical (Mitsubishi ChemicalCorporation) black pigment MA-7,0.8 parts by BASF (BASF) blue pigment Alkali Blue D6101 (CI Pigment Blue 61), 8 parts Mingling (Munzing Chemie Gmbh) companies EDPLAN482, its active ingredient content of 85% and 83.2 parts of deionized water with a high shear mixer and mixed for 1 hour to obtain uniformly shearing dispersion, then 0. 14L volume in the mill for 300g of dispersion shear milled for 1 hour to obtain an aqueous pigment dispersion. 颜料和分散剂的比例为1.18 : 1。 Ratio of the pigment and the dispersing agent was 1.18: 1. [0043] 将上述制备成的分散液和表2中8种添加物混合,常温下搅拌20分钟,用0. 5 μ 过滤器过滤得墨水组合物,即得到实施例产品2。 [0043] The dispersion was prepared as described above in Table 2 and 8 kinds of additives were mixed and stirred at room temperature for 20 minutes and filtered to obtain the ink composition with 0. 5 μ filter, i.e., the product obtained in Example 2 embodiment. [0044] 实施例3[0045] 见表1,首先制分散液,其中将8份三菱化学(Mitsubishi ChemicalCorporation) 的黑色颜料MA-7,1.2份巴斯夫(BASF)的蓝色颜料Alkali Blue D6101 (CI Pigment Blue 61),8份明凌(Munzing Chemie Gmbh)公司的EDPLAN482,其有效成分含量85%和82. 8份去离子水用高速剪切搅拌器混合1小时至均勻后得剪切分散液,再在0. 14L容积的研磨机中对300g的剪切分散液研磨1小时,得到水性颜料分散液。 [0044] Example 3 [0045] Table 1, a dispersion is first prepared in which 8 parts by Mitsubishi Chemical (Mitsubishi ChemicalCorporation) black pigment MA-7,1.2 parts by BASF (BASF) blue pigment Alkali Blue D6101 (CI Pigment Blue 61), 8 parts Mingling (Munzing Chemie Gmbh) companies EDPLAN482, its active ingredient content of 85% and 82.8 parts of deionized water were mixed with a high shear mixer for 1 hour to obtain a uniform dispersion of shearing, then 0. 14L volume in the mill for 300g of dispersion shear milled for 1 hour to obtain an aqueous pigment dispersion. 颜料和分散剂的比例为1.18 : 1。 Ratio of the pigment and the dispersing agent was 1.18: 1. [0046] 将上述制备成的分散液和表2中8种添加物混合,常温下搅拌20分钟,用0. 5 μ 过滤器过滤得墨水组合物,即得到实施例产品3。 [0046] The dispersion was prepared as described above in Table 2 and 8 kinds of additives were mixed and stirred at room temperature for 20 minutes and filtered to obtain the ink composition with 0. 5 μ filter, i.e., the product obtained in Example 3 embodiment. [0047] 比较例1[0048] 见表1,首先制分散液,其中将8份三菱化学(Mitsubishi ChemicalCorporation) 的黑色颜料MA-7,8份明凌(Munzing Chemie Gmbh)公司的EDPLAN 482,其有效成分含量85%和84份去离子水用高速剪切搅拌器混合1小时至均勻后得剪切分散液,再在0. 14L容积的研磨机中对300g的剪切分散液研磨1小时,得到水性颜料分散液。 [0047] Comparative Example 1 [0048] Table 1, a dispersion is first prepared in which 8 parts by Mitsubishi Chemical (Mitsubishi ChemicalCorporation) black pigment Mingling parts MA-7,8 (Munzing Chemie Gmbh) companies EDPLAN 482, which active ingredient content of 85% and 84 parts of deionized water were mixed with a high shear mixer 1 hour to obtain a uniform shear after dispersion, and then in a mill volume of 0. 14L shear 300g of the dispersion milled for 1 hour, to obtain an aqueous pigment dispersion. 颜料和分散剂的比例为1. 18 : 1。 Ratio of the pigment and the dispersing agent was 1.18: 1. [0049] 将上述制备成的分散液和表2中8种添加物混合,常温下搅拌20分钟,用0. 5 μ 过滤器过滤得墨水组合物,即得到比较例1。 [0049] The dispersion was prepared as described above in Table 2 and 8 kinds of additives were mixed and stirred at room temperature for 20 minutes and filtered to obtain the ink composition with 0. 5 μ filter, i.e., to obtain Comparative Example 1. [0050] 比较例2[0051] 见表1,首先制分散液,其中将8份三菱化学(Mitsubishi ChemicalCorporation) 的黑色颜料ΜΑ-7,0· 8 份科莱恩(Clariant)蓝色颜料PV Fast BlueBG (CI Pigment Blue 15:3),8 份明凌(Munzing Chemie Gmbh)公司的EDPLAN482,其有效成分含量85%和83. 2 份去离子水用高速剪切搅拌器混合1小时至均勻后得剪切分散液,再在0. 14L容积的研磨机中对300g的剪切分散液研磨1小时,得到水性颜料分散液。 [0050] Comparative Example 2 [0051] Table 1, a dispersion is first prepared in which 8 parts by Mitsubishi Chemical (Mitsubishi ChemicalCorporation) black pigment ΜΑ-7,0 · 8 parts by Clariant (Clariant) blue pigment PV Fast BlueBG (CI Pigment Blue 15: 3), 8 parts Mingling (Munzing Chemie Gmbh) companies EDPLAN482, its active ingredient content of 85% and 83.2 parts of deionized water were mixed with a high shear mixer for 1 hour to obtain a uniform shear cutting the dispersion, and then in a mill volume of 0. 14L 300g of dispersion shear milled for 1 hour to obtain an aqueous pigment dispersion. 颜料和分散剂的比例为1. 18 : 1。 Ratio of the pigment and the dispersing agent was 1.18: 1. [0052] 将上述制备成的分散液和表2中8种添加物混合,常温下搅拌20分钟,用0. 5 μ 过滤器过滤得墨水组合物,即得到比较例2。 [0052] The dispersion was prepared as described above in Table 2 and 8 kinds of additives were mixed and stirred at room temperature for 20 minutes and filtered to obtain the ink composition with 0. 5 μ filter, i.e., to obtain Comparative Example 2. [0053] 比较例3[0054] 见表1,首先制分散液,其中将8份三菱化学(Mitsubishi ChemicalCorporation) 的黑色颜料MA-7,0. 8 份汽巴(Ciba)蓝色颜料IRGALITE Blue GLVO(CI Pigment Blue 15:4),8 份明凌(Munzing Chemie Gmbh)公司的EDPLAN 482,其有效成分含量85%和83. 2 份去离子水用高速剪切搅拌器混合1小时至均勻后得剪切分散液,再在0. 14L容积的研磨机中对300g的剪切分散液研磨1小时,得到水性颜料分散液。 [0053] Comparative Example 3 [0054] Table 1, a dispersion is first prepared in which 8 parts by Mitsubishi Chemical (Mitsubishi ChemicalCorporation) black pigment MA-7,0. 8 parts of Ciba (Ciba) blue pigment IRGALITE Blue GLVO (CI Pigment Blue 15: 4), 8 parts Mingling (Munzing Chemie Gmbh) companies EDPLAN 482, its active ingredient content of 85% and 83.2 parts of deionized water were mixed with a high shear mixer for 1 hour to obtain a uniform shearing the dispersion, and then in a mill volume of 0. 14L 300g of dispersion shear milled for 1 hour to obtain an aqueous pigment dispersion. 颜料和分散剂的比例为1. 18 : 1。 Ratio of the pigment and the dispersing agent was 1.18: 1. [0055] 将上述制备成的分散液和表2中8种添加物混合,常温下搅拌20分钟,用0. 5 μ 过滤器过滤得墨水组合物,即得到比较例3。 [0055] The dispersion was prepared as described above in Table 2 and 8 kinds of additives were mixed and stirred at room temperature for 20 minutes and filtered to obtain the ink composition with 0. 5 μ filter, i.e., to obtain Comparative Example 3. [0056] 表1中的蓝色颜料CI Pigment Blue 61具有下面的结构,该结构式是CI PigmentBlue 61的完整结构式,但有时颜料结构相同,晶型不同时,性能差距也很大。 [0056] Table 1 blue pigment CI Pigment Blue 61 have the following structure which is a complete structural formula of formula CI PigmentBlue 61, but sometimes the same pigment structure, crystal form is not the same, the performance gap is also high. 本专利申请主要保护涉及该结构的产品。 This patent application generally relates to the protection of the product structure. [0057] [0057]

Figure CN101705028BD00091

[0058] 表3实施例和比较例墨水相对应的ΙΛ a*, b*的值[0059] [0058] Table 3 Examples and Comparative Examples Ink embodiment corresponding ΙΛ a *, b * values ​​of the [0059]

Figure CN101705028BD00092

[0060] 按照CIE规定的LW色度系统方法,从表3中我们可以看出实施例1〜3的f值和b*值比比较例1的f值和b*值均小,说明添加CI Pigment Blue 61的墨水优于没有添加CI Pigment Blue 61的墨水。 [0060] The method in accordance with a predetermined color system LW CIE, from Table 3, we can see that the value of f embodiments of Examples 1 ~ 3 * value and b * values ​​are smaller than the values ​​of Comparative Examples 1 and f b, instructions to add CI Pigment Blue 61 than the ink of the ink without addition of CI Pigment Blue 61. 实施例2和比较例2〜3蓝色颜料的添加量相同,种类不同。 Example 2 or 3 was added the same amount of blue pigment and Comparative Example 2, different kinds. 从表3中我们可以看出实施例2的f值和b*值比比较例2〜3的f值和b*值均小, 说明添加CI Pigment Blue 61 的墨水优于添加CI Pigment Blue 15:3 禾口CI Pigment Blue 15:4的墨水。 From Table 3, we can see that the value of f embodiments of Example 2 * value and b * values ​​are smaller than the f value of Comparative Example 2 or 3 and b, illustrate adding CI Pigment Blue 61 than ink add CI Pigment Blue 15: Wo port 3 CI Pigment Blue 15: 4 ink.

Claims (10)

  1. 1. 一种黑色墨水组合物,包括分散液、保湿剂、表面活性剂和去离子水,其中分散液由着色剂、分散剂、去离子水以及其它助剂研磨制备所得,其特征在于所说的着色剂至少含有黑色颜料CIPB 7和蓝色颜料CI Pigment Blue 61,其中黑色颜料CIPB 7和蓝色颜料CI Pigment Blue 61的重量比例在20 : 1至2 : 1之间。 CLAIMS 1. A black ink composition comprising a dispersion, humectant, surfactant and deionized water, wherein the dispersion of the colorant, the dispersant, deionized water, and other additives resulting milled preparation, characterized in that colorants comprising at least a black pigment and a blue pigment CIPB 7 CI pigment blue 61, wherein the weight ratio of black pigment and a blue pigment CIPB 7 CI pigment blue 61 in 20: 1: 1-2.
  2. 2.根据权利要求1所说的一种黑色墨水组合物,其特征在于所说的黑色颜料CIPB 7和蓝色颜料CI Pigment Blue 61的重量比例优选10 : 1至20 : 3之间。 2. One of said black ink composition according to claim 1, wherein the weight ratio of said black pigment and a blue pigment CIPB 7 CI Pigment Blue 61 is preferably between 10: 3: 1-20.
  3. 3.根据权利要求1所说的一种黑色墨水组合物,其特征在于所说的黑色颜料CIPB 7占整个墨水的重量百分比为1〜10%。 The said one black ink composition as claimed in claim 1, wherein said black pigment CIPB 7 percentage by weight of the entire ink is 1~10%.
  4. 4.根据权利要求1所说的一种黑色墨水组合物,其特征在于所说的黑色颜料CIPB 7选用以下其中一种:卡博特(Cabot)公司的Mongul-L、REGAL 400R、 Monarch 1300, Monarch 900、REGAL 330R ;三菱化学公司(Mitsubishi Chemical Corporation)的MA_7、MA100、MA40 ;德固赛公司(Degussa)的Special black 4 ;哥伦比亚化学公司(Columbian Chemical)的Raven 3500、Raven 1255、Raven 3600ultrao The said one black ink composition as claimed in claim 1, wherein said black pigment CIPB 7 choose one of the following: Cabot (Cabot) companies Mongul-L, REGAL 400R, Monarch 1300, Monarch 900, REGAL 330R; Mitsubishi chemical Corporation (Mitsubishi chemical Corporation) of MA_7, MA100, MA40; Degussa (Degussa) the Special black 4; Columbian chemicals company (Columbian chemical) of Raven 3500, Raven 1255, Raven 3600ultrao
  5. 5.根据权利要求1所说的一种黑色墨水组合物,其特征在于所说的分散剂可选用明凌(Munzing Chemie Gmbh)公司的EDPLAN 482。 The said one black ink composition as claimed in claim 1, wherein said dispersing agent can be selected Mingling (Munzing Chemie Gmbh) companies EDPLAN 482.
  6. 6.根据权利要求1所说的一种黑色墨水组合物,其特征在于所说的保湿剂可选用异丙醇、N-甲基-2-吡咯烷酮、2-吡咯酮、乙二醇乙醚、乙二醇丁醚、二乙二醇乙醚、二乙二醇丁醚、三乙二醇丁醚、丙二醇丁醚和二丙二醇丁醚、丙三醇、乙二醇、二乙二醇、三乙二醇、三羟甲基丙烷、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、1,2-己二醇、1,2,6_己三醇、聚乙二醇400、聚乙二醇600中的至少一种。 The said one black ink composition as claimed in claim 1, wherein said humectant may be selected isopropanol, N- methyl-2-pyrrolidone, 2-pyrrolidone, ethylene glycol ethyl ether acetate, glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol butyl ether, triethylene glycol butyl ether, propylene glycol butyl ether and diethylene glycol butyl ether, glycerol, ethylene glycol, diethylene glycol, triethylene alcohols, trimethylolpropane, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, 1,2-hexanediol, 1,2,6_ hexanetriol, polyethylene glycol 400, at least one of polyethylene glycol 600.
  7. 7.根据权利要求1所说的一种黑色墨水组合物,其特征在于所说的助剂包括PH调节剂和杀菌剂,其中PH调节剂可选用三乙醇胺;杀菌剂可选用科莱恩公司(Clariant)的Nipacide BIT-20。 7. One of said black ink composition according to claim 1, wherein said adjuvant comprises a PH adjusting agents and fungicides, wherein the PH adjusting agent optional triethanolamine; bactericides optional Clariant (Clariant ) the Nipacide BIT-20.
  8. 8.根据权利要求1所说的一种黑色墨水组合物,其特征在于所说的表面活性剂可选用空气化工公司(Air Products)的产品Surfynol 465和Surfynol 485中的任意一种。 8. The said one black ink composition of claim 1, wherein said surfactant may be selected from any of an air Chemical Company (Air Products) Products Surfynol 465 and Surfynol 485 in.
  9. 9. 一种黑色墨水组合物的制备方法,其特征在于包括分散液的制备与墨水的制备,其中:(一)分散液的制备包括以下步骤:①将分散剂和去离子水按照比例混合于容器中,并搅拌均勻;②黑色颜料CIPB 7和蓝色颜料CI Pigment Blue 61按重量比例在20 : 1至2 : 1之间加入,充分润湿;③用高速剪切机将步骤②所得的分散液高速剪切0. 5〜8小时,转速为1000〜 lOOOOrpm,剪切完成后放置10〜20分钟;④将步骤③所得的剪切分散液泵入研磨机中进行研磨分散,研磨介质采用直径为0. 05〜Imm的氧化锆珠;⑤将步骤④中研磨机出料口所得分散液进入研磨机的储料槽,再次泵入研磨机进行循环研磨0. 5〜M小时;⑥研磨过程中,每隔15分钟进行粒度检测,直到分散液的粒径达到要求,得到分散液,(二)墨水的制备包括以下步骤:按重量百分比取上述步骤⑥所制得的分散液50%,另 A method for preparing the black ink composition, characterized by comprising preparing a dispersion prepared with the ink, wherein the preparation :( a) a dispersion comprising: ① From the dispersant and deionized water were mixed according to the proportion vessel and stir; CIPB 7 ② black pigment and a blue pigment CI pigment blue 61 in a weight ratio of 20: 1 to 2: 1 is added, thoroughly wetted; ③ the step of using a high shear machine ② obtained high-speed shearing dispersion 0. 5 ~ 8 hours, speed 1000~ lOOOOrpm, 10-20 minutes after placing the cut is finished; ④ the resultant shear dispersing step ③ pumped into a dispersion mill grinding, milling media employed 0. 05~Imm diameter zirconium oxide beads; ④ ⑤ the step of opening the mill feed resulting dispersion mill into the hopper again pumped into the recirculation polishing grinder 0. 5~M hours; ⑥ grinding process, the particle size measurement every 15 minutes, until the dispersion particle diameter to meet the requirements to obtain a dispersion, preparation of (two) ink comprising the steps of: by taking the above step ⑥ weight percent dispersion prepared 50% another 加2-吡咯酮4%,乙二醇3%,1, 2-丙二醇3%,1,2-己二醇6%,Surfynol 4651. 2%,三乙醇胺0. 2%,杀菌剂和余量去离子水,制成墨水组合物。 Add 2- pyrrolidone 4%, 3% ethylene glycol, 1,2-propylene glycol, 3% 1,2-hexanediol 6%, Surfynol 4651. 2%, triethanolamine 0.2%, and the balance bactericides deionized water to prepare an ink composition.
  10. 10.根据权利要求9所说的一种黑色墨水组合物的制备方法,其特征在于所说的步骤①-③为剪切分散步骤,其中步骤③中的高速剪切主要作用是使分散剂分散乳化均勻, 打碎部分黑色颜料中的较大粒子,剪切时间优选1-2小时;上述步骤④-⑥为研磨分散步骤;其中步骤④中的研磨机为销棒式研磨机,转速为600〜4200rpm,研磨介质采用直径为0. 05〜0. 2mm的氧化锆珠;所说的步骤④中的研磨目的是使黑色纳米水性颜料分散液粒径继续降低,研磨时间优选1-2小时;所说的步骤⑤中的出料口的温度控制在20〜40°C之间;所说的步骤⑥为颜料粒度检测,粒径要求D5tl在IOOnm左右。 10. A method for preparing 9 of said black ink composition according to claim, wherein said step of ①-③ shear dispersing step, wherein in the step ③ main function is to make the high-speed shearing dispersing agent dispersed uniform emulsion, breaking the larger part of the black pigment particles, shearing time is preferably 1-2 hours; the above step ④-⑥ the step of grinding the dispersion; wherein in the step ④ mill is a pin mill, a speed of 600 ~4200rpm, grinding media with a diameter of 0. 05~0 2mm zirconia beads;. ④ polishing step of said object is in the black aqueous pigment liquid dispersion of nano particle size continues to decrease, the polishing time is preferably 1-2 hours; temperature spout said step ⑤ control between 20~40 ° C; ⑥ said step of detecting pigment particle size, the particle size required in IOOnm D5tl around.
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CN101358051A (en) 2008-07-30 2009-02-04 曾观涛;黄洪山;黄春英 Jet ink for digital print and preparation method thereof
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US6565202B2 (en) 2000-12-23 2003-05-20 Ilford Imaging Uk Limited Pigmented aqueous inks and ink set for ink jet printing
US7503968B2 (en) 2005-01-27 2009-03-17 Sieko Epson Corporation Black ink composition, and recording method and recorded article using the same
CN101358051A (en) 2008-07-30 2009-02-04 曾观涛;黄洪山;黄春英 Jet ink for digital print and preparation method thereof

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