CN101525462A - Liquid composition for making pigment fixed, ink set, method for producing ink jet recorded matter on fabric and ink jet recorded matter on fabric - Google Patents

Liquid composition for making pigment fixed, ink set, method for producing ink jet recorded matter on fabric and ink jet recorded matter on fabric Download PDF

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Publication number
CN101525462A
CN101525462A CNA2009100080005A CN200910008000A CN101525462A CN 101525462 A CN101525462 A CN 101525462A CN A2009100080005 A CNA2009100080005 A CN A2009100080005A CN 200910008000 A CN200910008000 A CN 200910008000A CN 101525462 A CN101525462 A CN 101525462A
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China
Prior art keywords
pigment
fabric
recorded matter
dispersion
stop bath
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Chinese (zh)
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矢竹正弘
田村庆政
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Seiko Epson Corp
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Seiko Epson Corp
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  • Ink Jet Recording Methods And Recording Media Thereof (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Ink Jet (AREA)

Abstract

There are provided a liquid composition for making pigment fixed having a high resistance to rubbing and a good dry-cleanability; an ink set including the liquid composition for making pigment fixed and an ink composition excellent in terms of color intensity, discharge stability, and adhesiveness; and a method for producing ink-jet-recorded matter on a fabric having a high resistance to rubbing and good dry-cleanability using the liquid composition for making pigment fixed and the ink composition. The liquid composition for making pigment fixed according to the present invention contains at least polymer fine particles synthesized using an alkyl (meth)acrylate and/or cyclic alkyl (meth)acrylate and a reactive compound having an ethylene-based unsaturated compound and a reactive group, the glass transition temperature and the acid value of the liquid composition being equal to or lower than -10 DEG C. and equal to or lower than 100 mg KOH/g, respectively.

Description

The manufacture method and the jet recorded matter on fabric of pigment stop bath, black liquid group, jet recorded matter on fabric
Technical field
The present invention relates to wear resistance and dry-cleaning (dry cleaning) property excellence the pigment stop bath, have the ink composition of this pigment stop bath and color developing, ejection stability, fixation performance excellence black liquid group, and use the manufacture method of jet recorded matter on fabric of the wear resistance (erasibility) of this pigment stop bath and this ink composition and dry-cleaning property excellence and the jet recorded matter on fabric that utilizes this method to obtain.
Background technology
The black liquid that is used in ink-vapor recording is required in the printing of paper that is recorded body to conduct or cloth and silk etc., do not ooze out, drying property is good, can print equably on the diversified surface that is recorded body, and adjacent color is not mixed etc. in the lettering of polychromes such as colored lettering systems.
In described black liquid, especially for the major part of having used the black liquid of pigment as the look material, mainly inquired into by suppressing impregnability the black liquid that is recorded body, inhibition is wetting to the black liquid that is recorded the surface, guarantee the lettering quality near black drop being rested on be recorded the surface, and carried out practicability.Yet, in suppressing the wetting black liquid that is recorded body, according to the raw-material difference that is recorded body, the difference of oozing out of black liquid becomes big, especially in the composition blended recycled writing paper of various paper, the problem of oozing out generation that exists the difference to the wetting property of the black liquid of its each composition to cause.In addition, in so black liquid, exist: the dried floral of print is time-consuming, the problem of adjacent color generation colour mixture (generation of blend of colors) in the lettering of polychromes such as colored lettering system.In addition, in the print that has used pigment inks liquid, pigment remains in the surface that is recorded body, therefore, has the problem of the wear resistance variation of print.
In order to solve such problem, attempted the raising to the impregnability that is recorded body of black liquid, inquired into and in black liquid, added diglycol monotertiary butyl ether (with reference to patent documentation 1), adding in black liquid as alkyne diol is the Sa Fei Nore 465 (day letter chemistry system) (with reference to patent documentation 2) of tensio-active agent, or adds the two material (with reference to patent documentation 3) etc. in black liquid.
In addition, in having used the black liquid of pigment, when being difficult to guarantee dispersing of pigments stability, improve the impregnability of black liquid, therefore, the narrow range of the selection of penetrant is so in the past as the combination of glycol ethers and pigment, inquired into the combination (with reference to patent documentation 5) etc. of the ethers of the combination (with reference to patent documentation 4) of using pigment to use the triglycol monomethyl ether or ethylene glycol, glycol ether or triglycol.
In addition, use black liquid as weaving, knowing has black liquid (with reference to patent documentation 6) that uses dyestuff or the black liquid (with reference to patent documentation 7) that relates to binding agent.
In addition, knowing has the print that relates to being printed with image etc. to contaminate the technology that (パ デ イ Application グ) handles, and comprises (with reference to patent documentations 8,9) such as dip-dyeing solution that the compound of regulation forms or dip-dye methods.
[prior art document]
[patent documentation]
No. 5156675 specification sheets of [patent documentation 1] United States Patent (USP)
No. 5183502 specification sheets of [patent documentation 2] United States Patent (USP)
No. 5196056 specification sheets of [patent documentation 3] United States Patent (USP)
[patent documentation 4] Japanese kokai publication sho 56-147861 communique
[patent documentation 5] Japanese kokai publication hei 9-111165 communique
[patent documentation 6] TOHKEMY 2007-515561 communique
[patent documentation 7] TOHKEMY 2007-126635 communique
[patent documentation 8] TOHKEMY 2005-281952 communique
[patent documentation 9] TOHKEMY 2004-149934 communique
Yet the wear resistance of dip-dyeing solution in the past and dry-cleaning property are insufficient.In addition, not do not inquire into the pigment stop bath of the excellent ink composition for ink-jet recording of color developing, ejection stability, the fixation performance of the manufacturing that is fit to described jet recorded matter on fabric and the most suitable such specific ink composition for the jet recorded matter on fabric of making wear resistance and dry-cleaning property excellence.In addition, also inquire into the manufacture method of the jet recorded matter on fabric of the wear resistance of having used above-mentioned ink composition for ink-jet recording and above-mentioned pigment stop bath and the property dry-cleaned excellence.
In addition, from the viewpoint of ink composition for ink-jet recording, water-based paint China ink liquid is in the past used as weaving, and fixation performance is insufficient, and depth of shade or color developing are also insufficient.In addition, pigment dispersion in the past tensio-active agent or glycol ethers etc. in black liquid have under the situation that the material of hydrophilic portion and hydrophobic portion exists, and cause the adsorption-desorption from pigment of dispersed polymeres easily, exist dispersed unstable, in addition, the problem of storage stability ejection poor stability.Usually, aqueous ink needs tensio-active agent or glycol ethers etc. to have the material of hydrophilic portion and hydrophobic portion in order to reduce being recorded oozing out of body.In not using the black liquid of these materials, insufficient to the impregnability that is recorded body, cause causing easily the problem of the reduction of lettering image in addition, having the range limited problem of the kind that is recorded body that can use in order to carry out uniform lettering.
And then, if (alkyne diol system or alkynol are tensio-active agent, two (three) ethylene glycol monobutyl ether, (two) propylene glycol single-butyl ether or 1 to use the additive that can contain in the black liquid of the present invention in pigment dispersion in the past, 2-aklylene glycol or these mixture), then can not get secular storage stability, the China ink liquid poorly soluble again, therefore, there is black liquid drying, stops up the problem of front portion etc. of the nozzle of ink gun easily.
Summary of the invention
Therefore, the present invention addresses the above problem, its purpose be to provide wear resistance and dry-cleaning property excellence pigment stop bath (dip-dyeing solution), have this pigment stop bath and color developing, ejection stability, fixation performance excellence, can be suitable as the ink composition that ink-vapor recording uses black liquid group, and use the manufacture method and the jet recorded matter on fabric of the jet recorded matter on fabric of the wear resistance of this pigment stop bath and this ink composition and dry-cleaning property excellence.
The present invention is as described below.
(1) a kind of pigment stop bath is characterized in that,
Contain high molecular particle, the second-order transition temperature of this high molecular particle is below-10 ℃, acid number is below the 100mgKOH/g, this high molecular particle is that to use (methyl) acrylate at least as its constituent be that the reactive compounds of unsaturated group and reactive group comes synthetic with having ethene, and described (methyl) acrylate is (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester.
(2) according to described (1) described pigment stop bath, it is characterized in that,
Described reactive group is a blocked isocyanate Huo oxazolinyl.
(3) according to described (1) or (2) described pigment stop bath, it is characterized in that,
With respect to described high molecular particle total amount, contain 70 quality % above described (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester.
(4) according to each described pigment stop bath in described (1)～(3), it is characterized in that,
Described (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester are (methyl) vinylformic acid C 1-24Alkyl ester and/or (methyl) vinylformic acid C 3-24The cyclic alkyl ester.
(5) according to each described pigment stop bath in described (1)～(4), it is characterized in that,
The vinylbenzene conversion weight-average molecular weight of using gel permeation chromatography (GPC) mensuration of described high molecular particle is more than 100000 and below 1000000.
(6) a kind of black liquid group is characterized in that having:
Each described pigment stop bath in ink composition and described (1)～(5), described ink composition contain can be with the dispersion of colo(u)rant dispersion in water.
(7) according to described (6) described black liquid group, it is characterized in that,
The median size of described dispersion is more than the 50nm and below the 300nm.
(8) according to described (7) described black liquid group, it is characterized in that,
Described dispersion be can under not having the situation of dispersion agent, be scattered in the water, median size be more than the 50nm and below the 300nm from disperse black carbon.
(9) according to described (8) described black liquid group, it is characterized in that,
Described dispersion can use polymkeric substance that pigment dyestuff is scattered in the water, and median size is that 50nm is above and below the 300nm, the vinylbenzene conversion weight-average molecular weight of using gel permeation chromatography (GPC) mensuration of this polymkeric substance is more than 10000 and below 200000.
(10) according to each described black liquid group in described (6)～(9), it is characterized in that described ink composition contains 1, the 2-aklylene glycol.
(11) according to each described black liquid group in described (6)～(10), it is characterized in that,
It is that tensio-active agent and/or alkynol are tensio-active agent that described ink composition contains alkyne diol.
(12) according to each described black liquid group in described (6)～(11), it is characterized in that,
The content of described high molecular particle (quality %) is more than the content (quality %) of described pigment.
(13) a kind of manufacture method of jet recorded matter on fabric is characterized in that, comprising:
To contain can make the dispersion of colo(u)rant dispersion in water the ink composition ink jet printing in the operation of cloth and silk;
This print be impregnated in the operation of each described pigment stop bath in described (1)～(5);
More than 110 ℃ and below 200 ℃, the operation of print thermal treatment more than 1 minute that this is impregnated.
(14) a kind of manufacture method of jet recorded matter on fabric is characterized in that, comprising:
To contain can make the dispersion of colo(u)rant dispersion in water the ink composition ink jet printing in the operation of cloth and silk;
Utilize ink jet method, each described pigment stop bath in described (1)～(5) is coated on the operation of this print;
More than 110 ℃ and below 200 ℃, the operation of print thermal treatment more than 1 minute that this is coated.
(15) according to the manufacture method of described (13) or (14) described jet recorded matter on fabric, it is characterized in that,
The median size of described dispersion is more than the 50nm and below the 300nm
(16) according to the manufacture method of described (15) described jet recorded matter on fabric, it is characterized in that,
Described dispersion be can under not having the situation of dispersion agent, be scattered in the water, median size be more than the 50nm and below the 300nm from disperse black carbon.
(17) according to the manufacture method of each described jet recorded matter on fabric in described (15), it is characterized in that,
Described dispersion can use polymkeric substance that pigment dyestuff is scattered in the water, and median size is that 50nm is above and below the 300nm, the vinylbenzene conversion weight-average molecular weight of using gel permeation chromatography (GPC) mensuration of this polymkeric substance is more than 10000 and below 200000.
(18) according to the manufacture method of each described jet recorded matter on fabric in described (13)～(17), it is characterized in that,
Described ink composition contains 1, the 2-aklylene glycol.
(19) according to the manufacture method of each described jet recorded matter on fabric in described (13)～(18), it is characterized in that,
It is that tensio-active agent and/or alkynol are tensio-active agent that described ink composition contains alkyne diol.
(20) according to the manufacture method of each described jet recorded matter on fabric in described (13)～(19), it is characterized in that,
The content of described high molecular particle (quality %) is more than the content (quality %) of described pigment.
(21) a kind of jet recorded matter on fabric is characterized in that,
It is to utilize the manufacture method of each described jet recorded matter on fabric in described (13)～(20) to obtain.
Embodiment
[pigment stop bath]
Pigment stop bath of the present invention, it is characterized in that, contain high molecular particle, the second-order transition temperature of this high molecular particle is below-10 ℃, acid number is below the 100mgKOH/g, this high molecular particle is that to use (methyl) acrylate at least as its constituent be that the reactive compounds of unsaturated group and reactive group comes synthetic with having ethene, and described (methyl) acrylate is (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester.Constitute by this, improve the friction fastness of unlubricated friction scrape along wet friction among both of jet recorded matter on fabric, improve the dry-cleaning property.
Below, each composition is described.
High molecular particle
The second-order transition temperature of high molecular particle is below-10 ℃.Thus, improve the fixation performance of the pigment of jet recorded matter on fabric.If surpass-10 ℃, then the fixation performance of pigment reduces gradually.Preferably-15 ℃, more preferably-20 ℃ below.
The acid number of high molecular particle is below the 100mgKOH/g.If surpass 100mgKOH/g, then the washing fastness of jet recorded matter on fabric reduces.Below the preferred 50mgKOH/g, more preferably below the 30mgKOH/g.
The molecular weight of high molecular particle is preferred more than 100,000.More preferably more than 200,000.If less than 100,000, the washing fastness of jet recorded matter on fabric reduces.
Constituent as high molecular particle is (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester, preferred (methyl) vinylformic acid C 1-24Alkyl ester and/or (methyl) vinylformic acid C 3-24The cyclic alkyl ester.As its example, can enumerate (methyl) methyl acrylate; (methyl) vinylformic acid ethyl ester; (methyl) vinylformic acid propyl diester; (methyl) n-butylacrylate; (methyl) vinylformic acid isobutyl; (methyl) vinylformic acid amyl group ester; (methyl) vinylformic acid polyhexamethylene; (methyl) 2-ethylhexyl acrylate; (methyl) vinylformic acid octyl group ester; (methyl) vinylformic acid nonyl ester; (methyl) vinylformic acid decyl ester; (methyl) vinylformic acid tert-butylcyclohexyl ester; (methyl) vinylformic acid Lauryl Ester; the different boronate of (methyl) vinylformic acid (イ ソ ボ ロ ニ Le) ester; (methyl) vinylformic acid cetyl ester; the hard ester acyl ester of (methyl) vinylformic acid; (methyl) vinylformic acid iso stearate base ester; base (methyl) vinylformic acid tetramethyl piperidine ester; (methyl) vinylformic acid two cyclopentyl esters; (methyl) vinylformic acid dicyclopentenyl ester; (methyl) vinylformic acid dicyclopentenyl hydroxy ester; and (methyl) vinylformic acid docosyl ester etc.
In addition, above-mentioned (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester preferably contain more than the 70 quality % with respect to the high molecular particle total amount.Because can further improve friction fastness and the dry-cleaning property of unlubricated friction scrape along wet friction among both of jet recorded matter on fabric like this.
In addition, the reactive group that has as the reactive compounds of the constituent of high molecular particle is meant by suitable processing such as thermal treatments, the group of the reactions such as functional group that the functional group's (for example, hydroxyl that contains in the Mierocrystalline cellulose) that has with cloth and silk, the functional group that high molecular particle has or dispersion (resin etc.) have.Reactive group contains at least more than one and gets final product in reactive compounds, contain a plurality ofly also can.On the other hand, the ethene in the reactive compounds be unsaturated group be supplied in as (methyl) alkyl acrylate of other constituents of high molecular particle and/or the reaction of (methyl) vinylformic acid cyclic alkyl ester.
Except the group that can react separately with this reactive group, for example, also comprise group in the reactive group for torpescence but by upsweeps such as heating under the independent situation as blocked isocyanate.Blocked isocyanate has following character: make the free isocyanate group of the terminal precursor of isocyanate group and contain activity hydroxy compound (end-capping reagent) reaction, be torpescence at normal temperatures, under the situation about being heated, end-capping reagent dissociates, the character of regeneration isocyanate group.
In pigment stop bath of the present invention, to use ink-vapor recording purposes, preferred reactive group be blocked isocyanate Huo oxazolinyl in order to be used in weaving.
In addition, be that the ethene that reactive compounds has is the example of unsaturated group as the constituent of high molecular particle, can enumerate vinyl, (methyl) acryl etc.
Have the example that ethene is the blocked isocyanate of unsaturated group as high molecular particle with what constituent contained, can obtain clear and electrician's fabrication from (カ レ Application ズ) MOI-BM, card from MOI-BP etc.
In addition, as having ethene is that unsaturated group is with the compound of oxazolinyl, can enumerate (methyl) vinylformic acid castor-oil plant Chun oxazoline ester, 2-vinyl-2-oxazoline, 4,4-dimethyl-2-vinyl-2-oxazoline, 4,4-dimethyl-2-pseudoallyl-2-oxazoline, 5-methyl-2-vinyl-2-oxazoline, 2-pseudoallyl (イ ソ プ リ ペ ニ Le)-2-oxazoline etc.Wherein, preferred (methyl) vinylformic acid castor-oil plant Chun oxazoline ester.
High molecular particle preferably uses the vinylbenzene conversion weight-average molecular weight of gel permeation chromatography (GPC) mensuration more than 100000 and below 1000000.By in described scope, improve the fixation performance of the pigment of jet recorded matter on fabric.
Median size with the light scattering determining high molecular particle.With more than the preferred 50nm of particle diameter of the high molecular particle of light scattering determining and below the 500nm, more preferably 60nm is above and below the 300nm.If less than 50nm, then the fixation performance of jet recorded matter on fabric reduces, if surpass 500nm, then stably dispersing becomes unstable.In addition, under situation, become unstable easily from the ejection of ink gun with the ink jet printing of pigment stop bath.
Other compositions
Pigment stop bath of the present invention as mentioned above, in the manufacture method of jet recorded matter on fabric of the present invention, to contain and to make ink composition ink jet printing that the dispersion of colo(u)rant dispersion in water form behind cloth and silk, (A) this print be impregnated in the pigment stop bath, or (B) utilize ink ejecting method, when being coated on this print, uses by the pigment stop bath.
Pigment stop bath of the present invention except above-mentioned must composition, can contain suitably that the aftermentioned ink composition for ink-jet recording contains 1,2-aklylene glycol, glycol ethers, alkyne diol are that tensio-active agent and/or alkynol are tensio-active agent etc.
[black liquid group]
Black liquid group of the present invention is characterized in that having: ink composition and above-mentioned pigment stop bath, above-mentioned ink composition contain can be with the dispersion of colo(u)rant dispersion in water.
Below, each composition of ink composition is described.The ink composition of following explanation can be used as ink composition for ink-jet recording and is suitable for.
Pigment dispersion
Median size with the light scattering determining pigment dispersion.Under the situation of the median size of pigment dispersion less than 50nm, the color developing of print or jet recorded matter on fabric reduces.In addition, if surpass 300nm, then fixation performance reduces.More preferably 70nm～230nm, and then preferred 80nm～130nm.
As pigment dispersion, preferably comprise can under not having the situation of dispersion agent, be scattered in the water, median size be more than the 50nm and below the 300nm from disperse black carbon (oneself disperse カ one ボ Application Block ラ Star Network).Should improve the color developing of jet recorded matter on fabric from disperse black carbon by using.Can under not having the situation of dispersion agent, be scattered in method in the water and be the method etc. of the sooty surface being carried out the oxidation of ozone or Textone etc.Preferred 50nm～the 150nm of described median size from the disperse black carbon dispersion.If less than 50nm, then can not get color developing.In addition, if surpass 150nm, then fixation performance reduces.Preferred particle diameter is 70nm～130nm, and then preferred 80nm～120nm.
In addition, as pigment dispersion, comprise and can use polymkeric substance that pigment dyestuff is scattered in median size in the water as more than the 50nm and below the 300nm, the vinylbenzene conversion weight-average molecular weight of measuring with gel permeation chromatography (GPC) of this polymkeric substance be 10000 or more and 200000 below materials.Thus, improve the fixation performance of the pigment of jet recorded matter on fabric, also improve pigment inks liquid self memory stability.In addition, with described polymkeric substance differently, can add water dispersible or water-soluble polymkeric substance or tensio-active agent as dispersion stabilizer for pigment dispersion stably is scattered in the black liquid.In addition, preferred (methyl) acrylate more than at least 70% of the constituent of above-mentioned polymkeric substance reaches the polymkeric substance that (methyl) acrylic acid copolymerization causes.Because dispersion stabilization is good.
As pigment, use as black ink liquid, carbon black (C.I. Pigment black 7) classes such as especially preferred furnace black, dim, acetylene black, thermally oxidized black, but can also use metal species, nigrosine pigment dyestuffs such as (C.I. Pigment blacks 1) such as copper oxide, ferriferous oxide (C.I. Pigment black 11), titanium oxide.
In addition, use as color ink liquid, can use C.I. Pigment Yellow 73 1 (not taking off yellow G), 3,12 (the yellow AAA of two diazonium), 13,14,17,24,34,35,37,42 (Zh 1s), 53,55,74,81,83 (the yellow HR of two diazonium), 93,94,95,97,98,100,101,104,108,109,110,117,120,128,138,153,155,180,185, C.I. Pigment red 1,2,3,5,17,22 (bright do not take off scarlet), 23,31,38,48:2 (permanent red 2B (Ba)), 48:2 (permanent red 2B (Ca)), 48:3 (permanent red 2B (Sr)), 48:4 (permanent red 2B (Mn)), 49:1,52:2,53:1,57:1 (bright fuchsin 6B), 60:1,63:1,63:2,64:1,81 (rhodamine 6G color lakes), 83,88,101 (Indian reds), 104,105,106,108 (cadmium reds), 112,114,122 (quinoline a word used for translation ketone magentas), 123,146,149,166,168,170,172,177,178,179,185,190,193,202,206,209,219, C.I. pigment violet 19,23, C.I. pigment orange 36, C.I. pigment blue 1,2,15 (phthalocyanine blue R), 15:1,15:2,15:3 (phthalocyanine blue G), 15:4,15:6 (phthalocyanine blue-E), 16,17:1,56,60,63, C.I. Pigment green 1,4,7,8,10,17,18,36 etc., as toner, can use various pigment.
In addition, above-mentioned pigment uses dispersion machine to disperse, but as dispersion machine, can use commercially available various dispersion machines.From the few viewpoint of contaminant, preferred non-medium disperses.As its concrete example, can enumerate wet shotcrete technology shredder (Ji Nasi company), nano unkind (Na ノ マ one ザ one, nano Mo Ci company), homogenizer (Gu Ling (go one リ Application) company), A Dimeizi (ア Le テ イ マ イ ザ one, Si Jinuo equipment company) and wear kind (マ イ Network ロ Off Le イ ダ イ ザ one, miniature Buddhist Roy Otto Dix company) etc. for miniature Buddhist Roy.
The preferred 0.5 quality % of the addition of pigment～30 quality % (below, also abbreviate " % " sometimes as), more preferably 1.0 quality %～15 quality %.Under situation less than the addition of 0.5 quality %, can not guarantee lettering concentration, in addition, under situation greater than the addition of 30 quality %, the viscosity that black liquid takes place increases or the structural viscosity of viscosity characteristics aspect, is in the tendency of variation from the ejection stability of the black liquid of ink gun.
1, the 2-aklylene glycol
Ink composition of the present invention preferably contains 1, the 2-aklylene glycol.By using 1, the 2-aklylene glycol reduces oozing out of print or jet recorded matter on fabric, improves the lettering quality.As 1, the example of 2-aklylene glycol, preferred 1,2-hexylene glycol, 1,2-pentanediol, 4-methyl isophthalic acid, carbonatoms 5 such as 2-pentanediol or 61, the 2-aklylene glycol.Wherein, 1 of preferred carbonatoms 6,2-hexylene glycol and 4-methyl isophthalic acid, 2-pentanediol.In addition, 1, the preferred 0.3 quality % of the addition of 2-aklylene glycol～30 quality %, more preferably 0.5 quality %～10 quality %.
Glycol ethers
Ink composition of the present invention preferably contains glycol ethers.Because reduce oozing out of print or jet recorded matter on fabric thus.As glycol ethers, preferred one or more that are selected from diglycol monotertiary butyl ether, triglycol single-butyl ether, propylene glycol single-butyl ether and dipropylene glycol single-butyl ether that use.In addition, the preferred 0.1 quality % of the addition of glycol ethers～20 quality %, more preferably 0.5 quality %～10 quality %.
Alkyne diol is that tensio-active agent and/or alkynol are tensio-active agent
It is that tensio-active agent and/or alkynol are tensio-active agent that ink composition of the present invention preferably contains alkyne diol.By using alkyne diol is that tensio-active agent and/or alkynol are tensio-active agent, further reduces and oozes out, and improves the lettering quality.In addition,, improve the drying property of lettering, can carry out high speed printing by these interpolation.
As alkyne diol is that tensio-active agent and/or alkynol are tensio-active agent, be preferably selected from 2,4,7,9-tetramethyl--5-decine-4,7-glycol and 2,4,7,9-tetramethyl--5-decine-4, the oxyalkylene affixture, 2 of 7-glycol, 4-dimethyl-5-decine-4-alcohol and 2, more than one of the oxyalkylene affixture of 4-dimethyl-5-decine-4-alcohol.These E series such as alkene 104 series, alkene E1010, day letter chemistry system Sa Fei Nore 465 or Sa Fei Nores 61 that can be used as Ai Erpuluoci (Britain) company wait and obtain.
In the present invention, be selected from by above-mentioned 1 by use, 2-aklylene glycol, above-mentioned alkyne diol are that tensio-active agent and/or alkynol are one or more of the group that constitutes of tensio-active agent and above-mentioned glycol ethers, and reduction is oozed out.
In addition, black liquid group of the present invention is characterized in that, the total content (quality %) of the above-mentioned high molecular particle that the pigment stop bath contains is more than the content (quality %) of the above-mentioned pigment that ink composition contains.Thus, improve the pigment fixation performance of jet recorded matter on fabric.
In addition, for be used for the guaranteeing of shelf-stability, from the stable ejection of ink gun, stop up and improve or the purposes such as deterioration preventing of black liquid, in ink composition of the present invention, also can suitably add dissolution aids, soak into control agent, viscosity modifier, pH regulator agent, dissolution aids, oxidation retarder, sanitas, mould inhibitor, anticorrosive agent, be used to catch various additives such as sequestrant the metal ion that disperses to exert an influence.
[manufacture method of jet recorded matter on fabric]
The manufacture method of jet recorded matter on fabric of the present invention is characterized in that, will contain can make the dispersion of colo(u)rant dispersion in water the ink composition ink jet printing in the operation of cloth and silk; This print be impregnated in the operation of described pigment stop bath; More than 110 ℃ and below 200 ℃, the operation of print thermal treatment more than 1 minute that this is impregnated.
In addition, the manufacture method of jet recorded matter on fabric of the present invention is characterized in that, will contain can make the dispersion of colo(u)rant dispersion in water the ink composition ink jet printing in the operation of cloth and silk; Utilize ink jet method, described pigment stop bath is coated on the operation of this print; More than 110 ℃ and below 200 ℃, the operation of print thermal treatment more than 1 minute that this is coated.
About ink composition and pigment stop bath, as mentioned above.
Heating temperature in heat treatment step does not improve the fixation performance of jet recorded matter on fabric less than under 110 ℃ the situation.In addition, if surpass 200 ℃, cloth and silk or pigment or polymkeric substance etc. self deterioration then.Heating temperature is preferred more than 120 ℃ and below 170 ℃.In addition, need more than 1 minute heat-up time.If less than 1 minute, then be contained in insufficient the carrying out of reaction of the blocked isocyanate Huo oxazolinyl isoreactivity group of the high molecular particle in the pigment stop bath.Preferred more than 2 minutes.
In addition, add water between the operation of preferred above-mentioned ink jet printing and dipping operation or the working procedure of coating or contain the operation that the water of tensio-active agent cleans print.By described cleaning, can be from the water soluble component the print flush away China ink liquid, the photographic fixing to cloth of high molecular particle becomes firmly, thereby can further improve the wear resistance of jet recorded matter on fabric.
In addition, when ink composition was printed in cloth and silk, this China ink liquid preferably sprayed by the method for having used electrostriction (Electricity the is askew) element that piezoelectric element etc. do not heat.Because under the situation that causes the heating that thermal head is the same, the polymkeric substance that uses in the dispersing of pigments in high molecular particle in the pigment stop bath or the black liquid etc. is rotten, and it is unstable that ejection becomes easily.In the manufacturing as jet recorded matter on fabric, require in its operation, to spray for a long time under the situation of a large amount of black liquid, preferably do not cause the head of heating.
[jet recorded matter on fabric]
Jet recorded matter on fabric of the present invention obtains by the manufacture method of above-mentioned jet recorded matter on fabric.
Below, by embodiment etc., be described more specifically the present invention.Also have, the present invention is not limited to described embodiment.Also have, in each composition of following embodiment, " part " " % " represents " weight part " " quality % " respectively under situation about not limiting especially.
(embodiment A-1)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion A1 that is made by following method, mixes with the vehicle composition shown in the table 2 and carries out.Also have, contain in " ion exchanged water (residual quantity) " in the black liquid of the present embodiment in present embodiment A and other embodiment, comparative example and reference example and be useful on the how general Saden of the corrosive that prevents black liquid (De ッ プ サ イ De) 240 (Palma Jim (パ one マ ケ system) Asian company system) 0.05%, be used for preventing the corrosive benzotriazole 0.02% of ink gun parts and be used to reduce EDTA (ethylene diamine tetra acetic acid ester) the 2Na salt 0.04% of influence of the metal ion of black liquid.
The making of pigment dispersion A1
It is that corporate system is not received can (モ Na one Network) 880 for the U.S. this spy of first (rice state キ ヤ ボ ッ ト) that pigment dispersion A1 uses carbon black (Pigment black 7).Utilize with special and open the identical method of flat 8-3498 communique, the surface of oxygenated black can be scattered in the water it, forms dispersion A1.Through using minisize track particle size distribution device UPA250 (day machine dress system), the result who measures particle diameter is 110nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is by using the high molecular particle aqueous dispersions of being made by following method (emulsion AA), mixes with the vehicle composition shown in the table 3 and carries out.Also have, contain in " ion exchanged water (residual quantity) " in this pigment stop bath in present embodiment A and the pigment stop bath of other embodiment, comparative example and reference example and be useful on the how general Saden 240 of the corrosive that prevents black liquid (Palma Jim Asian company system) 0.05%, be used for preventing the corrosive benzotriazole 0.02% of ink gun parts and be used to reduce EDTA (ethylene diamine tetra acetic acid ester) the 2Na salt 0.04% of influence of the metal ion of black liquid.
The making of high molecular particle
Possessing the drippage device, thermometer, the water-cooled reflux exchanger, in the reaction vessel of stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.2 part of the Potassium Persulphate of interpolation polymerization starter, and will in 7 parts of ion exchanged waters, put into 0.05 part of Sodium Lauryl Sulphate BP/USP, 4 parts of glycidoxy acrylate, 15 parts of vinylformic acid ethyl esters, 15 parts of butyl acrylate cores, 6 parts of tetrahydrofurfuryl acrylate, the monomer solution that 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan are 0.02 part drips down at 70 ℃, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 30 parts of vinylformic acid ethyl esters, 25 parts of methyl acrylate, clear and electrician's fabrication is from MOI-BM6 part, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion AA (EM-AA).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC) to measure second-order transition temperature is-15 ℃.Use the gel permeation chromatography (GPC) of system L7100 system of Hitachi Co., Ltd, as THF, measuring periodic vinylbenzene conversion molecular weight is 150000 with solvent.In addition, the acid number based on volumetry is 20mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use above-mentioned black liquid,, use the system PX-V600 of Seiko Epson Corp, be produced on the print of comprehensive lettering on the cotton as ink-jet printer.Then, use described printer, on this print, carry out comprehensive lettering, under 150 ℃, carried out heat treated 5 minutes, obtain the jet recorded matter on fabric of sample with described pigment stop bath.
(4) cut resistance test and the test of dry-cleaning property
Use of Te Site (テ ス one) Industry Co., Ltd formula friction fastness (shake formula friction Kennedy jail property) the trier AB-301S that shakes,, above-mentioned sample (jet recorded matter on fabric) is carried out the friction fastness of wiping 200 times with loading 300g.Utilize JIS (JIS) the JIS L0849 of the situation of peeling off of confirming black liquid, estimate with dry and two moistening levels.In addition, similarly utilize the B method of JIS L0860, estimate the dry-cleaning test.With the results are shown in the table 1 of cut resistance test and dry-cleaning test.
The mensuration of (5) ejection stability
As ink-jet printer, use the system PX-V600 of Seiko Epson Corp, with above-mentioned ink composition for ink-jet recording under 35 ℃, 35% atmosphere, open at the Qi Luosi of Fuji (ゼ ロ ッ Network ス) corporate system XeroxP paper A4, with the ratio of MS-WORD with the standard of character size 11, MSP black matrix, 4000 word/pages or leaves, print 100 pages, estimate.The AA that is made as that does not have the lettering entanglement fully has the A that is made as of 1 place lettering entanglement, and the B that is made as of 2 places～3 places lettering entanglement is arranged, and the C that is made as of 4 places～5 places lettering entanglement is arranged, and the D that is made as of the above lettering entanglement in 6 places is arranged, and the results are shown in the table 1.
(embodiment A-2)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion A2 that is made by following method, mixes with the vehicle composition shown in the table 2 and carries out.
The making of pigment dispersion A2
Pigment dispersion A2 uses pigment Blue 15: 3 (the blue or green pigment of copper phthalein: grace is special in carat).After the reaction vessel that possesses stirrer, thermometer, return line and dropping funnel carried out nitrogen displacement, put into 75 parts of vinylformic acid benzyl esters, 2 parts in vinylformic acid, 0.3 part of uncle's lauryl mercaptan, be heated to 70 ℃, and 150 parts of the vinylformic acid benzyl esters that will prepare separately, 15 parts in vinylformic acid, 5 parts of butyl acrylate cores, 1 part of uncle's lauryl mercaptan, 20 parts of butanone and Sodium Persulfate are put into dropping funnel for 1 part, through 4 hours, when in reaction vessel, splashing into, make dispersed polymeres carry out polyreaction.Secondly, in reaction vessel, add butanone, make the dispersing polymer solution of 40% concentration.Take out the part of this polymkeric substance, after being dried, utilize differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC), the result who measures second-order transition temperature is 40 ℃.
In addition, mix 40 parts of above-mentioned dispersing polymer solutions, 30 parts of pigment Blue 15s: 3,100 parts of the aqueous sodium hydroxide solutions of 0.1mol/L, 30 parts of butanone.Then, use ultra-high voltage homogenizer (Si Jinuo of Co., Ltd. equipment system A Ludimaici HJP-25005), enforcement 15 times under 200MPa and disperseing.Then, it is transferred in other containers, add 300 parts of ion exchanged waters, and then stirred 1 hour.Then, use the rotary type vaporizer, heat up in a steamer the total amount of butanone and the part of water, the sodium hydroxide neutralization with 0.1mol/L is adjusted to pH9 with it.Then, filter, regulate, form pigment concentration and be 15% pigment dispersion A2 with ion exchanged water with the film filter of 0.3 μ m.The result who utilizes the method identical with embodiment A-1 to measure particle diameter is 80nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the high molecular particle aqueous dispersions of making by following method by using (emulsion AB), mixes with the vehicle composition shown in the table 3 and carries out.
The making of high molecular particle
In the reaction vessel that possesses drippage device, thermometer, water-cooled reflux exchanger, stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.2 part of the Potassium Persulphate of interpolation polymerization starter, and the monomer solution that will put into 0.02 part of 0.05 part of Sodium Lauryl Sulphate BP/USP, 19 parts of vinylformic acid ethyl esters, 15 parts of butyl acrylate cores, 6 parts of tetrahydrofurfuryl acrylate, 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan in 7 parts of ion exchanged waters is at 70 ℃ of drippages down, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 30 parts of vinylformic acid ethyl esters, 25 parts of methyl acrylate, 10 parts of butyl acrylate cores, clear and electrician's fabrication is from 6 parts of MOI-BM, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion AB (EM-AB).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC) to measure second-order transition temperature is-17 ℃.With embodiment A-1 in the same manner the result of determining molecular weight be 200000.In addition, the acid number based on volumetry is 20mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of embodiment A-2, utilize the method identical, obtain the jet recorded matter on fabric of sample with embodiment A-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with embodiment A-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 1.
The mensuration of (5) ejection stability
Use the black liquid of embodiment A-2, utilize method identical and identical evaluation method, spray the mensuration of stability with embodiment A-1.The measurement result of ejection stability is illustrated in the table 1.
(embodiment A-3)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion A3 that is made by following method, mixes with the vehicle composition shown in the table 2 and carries out.
The making of pigment dispersion A3
Pigment dispersion A3 is to use pigment violet 19, and (quinoline a word used for translation ketone pigment: carat Li Ente (Network ラ リ ア Application ト) system), A2 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with embodiment A-1 to measure particle diameter is 90nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion AB that makes in embodiment A-2 by using, and carries out with the vehicle composition shown in the table 3.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of embodiment A-3, utilize the method identical, obtain the jet recorded matter on fabric of sample with embodiment A-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with embodiment A-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 1.
The mensuration of (5) ejection stability
Use the black liquid of embodiment A-3, utilize method identical and identical evaluation method, spray the mensuration of stability with embodiment A-1.The measurement result of ejection stability is illustrated in the table 1.
(embodiment A-4)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion A4 that is made by following method, mixes with the vehicle composition shown in the table 2 and carries out.
The making of pigment dispersion A4
Pigment dispersion A4 is to use pigment Yellow 14 (azo pigment: grace is special in carat), and A2 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with embodiment A-1 to measure particle diameter is 115nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion AB that makes in embodiment A-2 by using, and carries out with the vehicle composition shown in the table 3.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of embodiment A-4, utilize the method identical, obtain the jet recorded matter on fabric of sample with embodiment A-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with embodiment A-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 1.
The mensuration of (5) ejection stability
Use the black liquid of embodiment A-4, utilize method identical and identical evaluation method, spray the mensuration of stability with embodiment A-1.The measurement result of ejection stability is illustrated in the table 1.
(Comparative examples A-1)
In Comparative examples A-1, in the pigment stop bath of embodiment A-1, using and changing to 45 parts of second-order transition temperatures of making for identical adjusting in addition of vinylformic acid benzyl ester by the total amount (45 parts) with the vinylformic acid ethyl ester is 0 ℃ high molecular particle, in addition, with embodiment A-1 in the same manner, regulate the pigment stop bath.To use the emulsion of this high molecular particle making as emulsion AC (EM-AC).Pigment stop bath composition is illustrated in the table 3.In addition, the black liquid of Comparative examples A-1 is to use the pigment dispersion identical with embodiment A-1 to regulate.Black liquid composition is illustrated in the table 2.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.The results are shown in the table 1.
(Comparative examples A-2)
In Comparative examples A-2, in the pigment stop bath of embodiment A-2, use and pass through vinylformic acid ethyl ester total amount (49 parts) instead of the methacrylic acid benzyl ester, it is 10 ℃ high molecular particle that 10 parts of butyl acrylate cores are changed to the second-order transition temperatures of making for identical adjusting beyond 10 parts of the methacrylic acid benzyl esters, in addition, with embodiment A-2 pigment preparation stop bath in the same manner.To use the emulsion of this high molecular particle making as emulsion AD (EM-AD).The composition of pigment stop bath is illustrated in the table 3.In addition, the black liquid of Comparative examples A-2 is to use the pigment dispersion identical with embodiment A-2 to regulate.Black liquid composition is illustrated in the table 2.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.The results are shown in the table 1.
(reference example A-3)
In reference example A-3, in the black liquid of embodiment A-3, the making particle diameter is that the pigment dispersion of 350nm and 45nm is prepared black liquid in the same manner with embodiment A-3 in addition.Particle diameter is to measure by the method identical with embodiment A-1.The dispersion that with particle diameter is 350nm is as pigment dispersion A3A, and the dispersion that with particle diameter is 45nm is as pigment dispersion A3B.Black liquid composition is illustrated in the table 2.In addition, reference example A-3 pigment stop bath uses the pigment stop bath identical with embodiment A-3.Pigment stop bath composition is illustrated in the table 3.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.The results are shown in the table 1.
(Comparative examples A-4)
In Comparative examples A-4, in the pigment stop bath of embodiment A-4, the acid number of high molecular particle is made as beyond 120mgKOH/g, the 150mgKOH/g and embodiment A-4 pigment preparation stop bath in the same manner.With the emulsion that uses acid number to make as the high molecular particle of 120mgKOH/g as emulsion AE (EM-AE), with uses acid number as the emulsion of the high molecular particle making of 150mgKOH/g as emulsion AF (EM-AF).Pigment stop bath composition is illustrated in the table 3.In addition, the black liquid of Comparative examples A-4 uses the black liquid identical with embodiment A-4.Black liquid composition is illustrated in the table 2.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.The results are shown in the table 1.
(Comparative examples A-5)
In Comparative examples A-5, in the pigment stop bath of embodiment A-2, use blocked isocyanate with (methyl) acryl (clear and electrician's fabrication from MOI-BM) in addition with embodiment A-2 pigment preparation stop bath in the same manner.To use emulsion that the high molecular particle that this has the blocked isocyanate (clear and electrician's fabrication from MOI-BM) of (methyl) acryl of no use makes as emulsion AG (EM-AG), and the pigment stop bath is formed be illustrated in the table 3.In addition, the black liquid of Comparative examples A-5 uses the black liquid identical with embodiment A-2.Black liquid composition is illustrated in the table 2.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.The results are shown in the table 1.
(Comparative examples A-6)
In Comparative examples A-6, in the pigment stop bath of embodiment A-3, do not use blocked isocyanate with (methyl) acryl (clear and electrician's fabrication from MOI-BM) in addition with embodiment A-3 pigment preparation stop bath in the same manner.Pigment stop bath composition is illustrated in the table 3.In addition, the black liquid of Comparative examples A-6 uses the black liquid identical with embodiment A-3.Black liquid composition is illustrated in the table 2.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.The results are shown in the table 1.
[table 1]
The result of the wear resistance among table 1 embodiment A-1～4, Comparative examples A-1～2,4～6, the reference example A-3, dry-cleaning property, ejection stability
Figure A20091000800000231
The unit of Tg is ℃, and particle diameter is the median size of pigment, and unit is nm, and the unit of acid number is mgKOH/g, and wear resistance, dry-cleaning property are based on the metewand of JIS.
[table 2]
The black liquid of table 2 embodiment A-1～4, Comparative examples A-1～2,4～6, reference example A-3 is formed (quality %)
Figure A20091000800000232
Represent pigment concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
The TMP TriMethylolPropane(TMP)
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
[table 3]
The pigment stop bath of table 3 embodiment A-1～4, Comparative examples A-1～2,4～6, reference example A-3 is formed (quality %)
Figure A20091000800000241
Represent polymer concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
The TMP TriMethylolPropane(TMP)
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
(embodiment A-5)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is the pigment dispersion A5 that is made by following method by using, and mixes with the vehicle composition shown in the table 5 and carries out.
The making of pigment dispersion A5
It is the system MA100 of Mitsubishi Chemical Industrial Co., Ltd that pigment dispersion 5 uses carbon black (PBk7).Utilize with special and open the identical method of flat 8-3498 communique, the surface of oxygenated black can be scattered in the water it, forms dispersion A5.The result who utilizes the identical method of embodiment A-1 to measure particle diameter is 120nm.
2) preparation of pigment stop bath
The preparation of pigment stop bath is the high molecular particle aqueous dispersions of being made by following method by using (emulsion AI), carries out with the vehicle composition shown in the table 6.
The making of high molecular particle
In the reaction vessel that possesses drippage device, thermometer, water-cooled reflux exchanger, stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.3 part of the Potassium Persulphate of interpolation polymerization starter, and the monomer solution that will put into 0.02 part of 0.05 part of Sodium Lauryl Sulphate BP/USP, 20 parts of vinylformic acid ethyl esters, 15 parts of butyl acrylate cores, 6 parts of vinylformic acid Lauryl Ester, 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan in 7 parts of ion exchanged waters is at 70 ℃ of drippages down, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 24 parts of vinylformic acid ethyl esters, clear and electrician's fabrication is from 6 parts of MOI-BP, 25 parts of butyl acrylate cores, 16 parts of vinylformic acid Lauryl Ester, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion AI (EM-AI).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC) to measure second-order transition temperature is-19 ℃.With embodiment A-1 in the same manner the result of determining molecular weight be 180000.In addition, the acid number based on volumetry is 18mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of embodiment A-5, utilize the method identical, obtain the jet recorded matter on fabric of sample with embodiment A-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with embodiment A-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 4.
The mensuration of (5) ejection stability
Use the black liquid of embodiment A-5, utilize method identical and identical evaluation method, spray the mensuration of stability with embodiment A-1.The measurement result of ejection stability is illustrated in the table 1
(embodiment A-6)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is the pigment dispersion A6 that is made by following method by using, and mixes with the vehicle composition shown in the table 5 and carries out.
The manufacturing of pigment dispersion A6
Pigment dispersion A6 uses pigment Blue 15: 3 (the blue or green pigment of copper phthalein: grace is special in carat).To possessing stirrer, thermometer, after the reaction vessel of return line and dropping funnel carries out the nitrogen displacement, put into 45 parts of vinylbenzene, 30 parts of poly(oxyethylene glycol) 400 acrylate, 10 parts of vinylformic acid benzyl esters, 2 parts in vinylformic acid, 0.3 part of uncle's lauryl mercaptan, be heated to 70 ℃, with 150 parts of the vinylbenzene prepared separately, 100 parts of poly(oxyethylene glycol) 400 acrylate, 15 parts in vinylformic acid, 15 parts of butyl acrylate cores, 1 part of uncle's lauryl mercaptan and Sodium Persulfate are put into dropping funnel for 5 parts, through 4 hours, when in reaction vessel, splashing into, make dispersed polymeres carry out polyreaction.Secondly, in reaction vessel, add water, make the dispersing polymer solution of 40% concentration.Take out the part of this polymkeric substance, after being dried, utilize differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC), the result who measures second-order transition temperature is 40 ℃.
In addition, mix 40 parts of above-mentioned dispersing polymer solutions, 30 parts of pigment Blue 15s: 100 parts of the aqueous sodium hydroxide solutions of 3 (the blue or green pigment of copper phthalein: grace is special in carat), 0.1mol/L, Ai Ge (the ア イ ガ one) grinding machine of zirconium oxide bead has been used in employing, disperses through 2 hours.Then, it is transferred to other containers, add 300 parts of ion exchanged waters, and then stirred 1 hour.Also have, the sodium hydroxide neutralization with 0.1mol/L is adjusted to pH9 with it.Then, filter, form solid state component (dispersed polymeres and pigment Blue 15: 3) be 20% dispersion A5 with the film filter of 0.3 μ m.The result who utilizes the method identical with embodiment A-1 to measure particle diameter is 100nm.The result of determining molecular weight is 210000.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the high molecular particle aqueous dispersions of making by following method by using (emulsion AJ), mixes with the vehicle composition shown in the table 6 and carries out.
The making of high molecular particle
In the reaction vessel that possesses drippage device, thermometer, water-cooled reflux exchanger, stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.3 part of the Potassium Persulphate of interpolation polymerization starter, the monomer solution that to put into 0.02 part of 0.05 part of Sodium Lauryl Sulphate BP/USP, 20 parts of vinylformic acid ethyl esters, 25 parts of butyl acrylate cores, 6 parts of vinylformic acid Lauryl Ester, 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan in 7 parts of ion exchanged waters is at 70 ℃ of drippages down, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 14 parts of vinylformic acid ethyl esters, clear and electrician's fabrication is from 6 parts of MOI-BM, 20 parts of butyl acrylate cores, 20 parts of vinylformic acid Lauryl Ester, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion AJ (EM-AJ).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC) to measure second-order transition temperature is-21 ℃.In addition, the acid number based on volumetry is 18mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of embodiment A-6, utilize the method identical, obtain the jet recorded matter on fabric of sample with embodiment A-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with embodiment A-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 4.
The mensuration of (5) ejection stability
Use the black liquid of embodiment A-6, utilize method identical and identical evaluation method, spray the mensuration of stability with embodiment A-1.The measurement result of ejection stability is illustrated in the table 4.
(embodiment A-7)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion A7 that is made by following method, mixes with the vehicle composition shown in the table 5 and carries out.
The making of pigment dispersion A7
Pigment dispersion A7 is to use pigment red 122 (dimethyl quinoline a word used for translation ketone pigment: grace is special in carat), and A6 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with embodiment A-1 to measure particle diameter is 80nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion AJ that makes in embodiment A-6 by using, and carries out with the vehicle composition shown in the table 6.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of embodiment A-7, utilize the method identical, obtain the jet recorded matter on fabric of sample with embodiment A-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with embodiment A-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 4.
The mensuration of (5) ejection stability
Use the black liquid of embodiment A-7, utilize method identical and identical evaluation method, spray the mensuration of stability with embodiment A-1.The measurement result of ejection stability is illustrated in the table 4.
(embodiment A-8)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion A8 that is made by following method, mixes with the vehicle composition shown in the table 5 and carries out.
The making of pigment dispersion A8
Pigment dispersion A8 is to use Pigment Yellow 73 180 (the benzene imidazolone is two diazonium series pigments: grace is special in carat), and A6 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with embodiment A-1 to measure particle diameter is 130nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion AJ that makes in embodiment A-6 by using, and carries out with the vehicle composition shown in the table 6.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of embodiment A-8, utilize the method identical, obtain the jet recorded matter on fabric of sample with embodiment A-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with embodiment A-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 4.
The mensuration of (5) ejection stability
Use the black liquid of embodiment A-8, utilize method identical and identical evaluation method, spray the mensuration of stability with embodiment A-1.The measurement result of ejection stability is illustrated in the table 4.
(reference example A-7)
In reference example A-7, the molecular weight of the high molecular particle of the pigment stop bath of embodiment A-5 changed to 90000 and 1100000 beyond with embodiment A-5 pigment preparation stop bath in the same manner.With molecular weight be 90000 emulsion as emulsion AK (EM-AK), be that 1100000 emulsion is as emulsion AL (EM-AL) with molecular weight.Pigment stop bath composition is illustrated in the table 6.In addition, the black liquid of reference example A-7 is to use the pigment dispersion identical with embodiment A-5 to regulate.Black liquid composition is illustrated in the table 5.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.Structure is illustrated in the table 4.
(reference example A-8)
In reference example A-8, in embodiment A-6, will be as 1,1 of 2-aklylene glycol, 2-hexylene glycol are prepared black liquid and pigment stop bath in the same manner with embodiment A-6 beyond being replaced into glycerine.Black liquid composition is illustrated in the table 5, pigment stop bath composition is illustrated in the table 6.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.Structure is illustrated in the table 4.
(reference example A-9)
In reference example A-9, in embodiment A-7, be that tensio-active agent and alkynol are to prepare black liquid and pigment stop bath in the same manner with embodiment A-7 beyond tensio-active agent is replaced into glycerine with alkyne diol.Black liquid composition is illustrated in the table 5, pigment stop bath composition is illustrated in the table 6.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and embodiment A-1 are carried out in the same manner.Structure is illustrated in the table 4.
(reference example A-10)
In reference example A-10, in embodiment A-8, the high molecular particle of pigment stop bath prepared black liquid and pigment stop bath in the same manner with embodiment A-8 beyond pigment ratio being made as 80%, 50%.Black liquid composition is illustrated in the table 5, pigment stop bath composition is illustrated in the table 6.Cut resistance test, the test of dry-cleaning property and ejection stability test and embodiment A-1 are carried out in the same manner.Structure is illustrated in the table 4.
(reference example A-11～15)
In reference example A-11～15, in embodiment A-6, be produced on the sample of the comprehensive lettering of cotton, will carry out various changes and estimate wear resistance in the same manner with embodiment A-6 beyond handling in 5 minutes condition of 150 ℃ of heat treated.Will be in order to compare with embodiment A-6, the example that changes various conditions the results are shown in the table 7 as a reference example A-11～15.
[table 4]
The result of the wear resistance in table 4 embodiment A-5～8, reference example A-7～10, dry-cleaning property, ejection stability
Figure A20091000800000301
The unit of Tg is ℃, and particle diameter is the median size of pigment, and unit is nm, and the unit of acid number is mgKOH/g.
Molecular weight in the table 4 is * 10 5
Pigment ratio is represented % with respect to the high molecular particle of pigment.
Wear resistance, dry-cleaning property are based on the metewand of JIS.
[table 5]
The black liquid of table 5 embodiment A-5～8 and reference example A-7～10 is formed (quality %)
Figure A20091000800000311
Represent pigment concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
The TMP TriMethylolPropane(TMP)
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
[table 6]
The pigment stop bath of table 6 embodiment A-5～8 and reference example A-7～10 is formed (quality %)
Figure A20091000800000321
Represent polymer concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
The TMP TriMethylolPropane(TMP)
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
[table 7]
Frictional property test-results when having changed heating condition in table 7 embodiment A-6
Figure A20091000800000331
(Embodiment B-1)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is the pigment dispersion B1 that is made by following method by using, and mixes and carries out with the body composition that carries shown in the table 9.Also have, contain in " ion exchanged water (residual quantity) " in the black liquid of the present embodiment in present embodiment B and other embodiment, comparative example and reference example and be useful on the how general Saden 240 of the corrosive that prevents black liquid (Palma Jim Asian company system) 0.05%, be used for preventing the corrosive benzotriazole 0.02% of ink gun parts and be used to reduce EDTA (ethylene diamine tetra acetic acid ester) the 2Na salt 0.04% of influence of the metal ion of black liquid.
The making of pigment dispersion B1
It is that this special corporate system of U.S.'s first do not receive can 880 that pigment dispersion B1 uses carbon black (Pigment black 7).Utilize with special and open the identical method of flat 8-3498 communique, the surface of oxygenated black can be scattered in the water it, forms dispersion B1.Through using minisize track particle size distribution device UPA250 (day machine dress system), the result who measures particle diameter is 110nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is by using the high molecular particle aqueous dispersions of being made by following method (emulsion BA), mixes with the vehicle composition shown in the table 3 and carries out.Also have, contain in " ion exchanged water (residual quantity) " in this pigment stop bath in present embodiment B and the pigment stop bath of other embodiment, comparative example and reference example and be useful on the how general Saden 240 of the corrosive that prevents black liquid (Palma Jim Asian company system) 0.05%, be used for preventing the corrosive benzotriazole 0.02% of ink gun parts and be used to reduce EDTA (ethylene diamine tetra acetic acid ester) the 2Na salt 0.04% of influence of the metal ion of black liquid.
The making of high molecular particle
Possessing the drippage device, thermometer, the water-cooled reflux exchanger, in the reaction vessel of stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.2 part of the Potassium Persulphate of interpolation polymerization starter, to in 7 parts of ion exchanged waters, put into 0.05 part of Sodium Lauryl Sulphate BP/USP, 4 parts of glycidoxy acrylate, 15 parts of vinylformic acid ethyl esters, 15 parts of butyl acrylate cores, 6 parts of (methyl) vinylformic acid castor-oil plant Chun oxazoline esters, the monomer solution that 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan are 0.02 part drips down at 70 ℃, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 30 parts of vinylformic acid ethyl esters, 25 parts of methyl acrylate, 6 parts of vinylformic acid castor-oil plant Chun oxazoline esters, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion BA (EM-BA).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTBR6000DSC) to measure second-order transition temperature is-15 ℃.Use the gel permeation chromatography (GPC) of system L7100 system of Hitachi Co., Ltd, as THF, measuring periodic vinylbenzene conversion molecular weight is 150000 with solvent.In addition, the acid number based on volumetry is 20mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use above-mentioned black liquid,, use the system PX-V600 of Seiko Epson Corp, be produced on the print of comprehensive lettering on the cotton as ink-jet printer.Then, use described printer, on this print,, under 150 ℃, carried out heat treated 5 minutes, obtain the jet recorded matter on fabric of sample with the comprehensive lettering of described pigment stop bath.
(4) cut resistance test and the test of dry-cleaning property
Use of special this special product industry Co., Ltd. formula cut resistance test machine AB-301S that shakes,, above-mentioned sample (jet recorded matter on fabric) is carried out the friction fastness of wiping 200 times with loading 300g.Utilize JIS (JIS) the JIS L0849 of the situation of peeling off of confirming black liquid, estimate with dry and two moistening levels.In addition, similarly utilize the B method of JIS L0860, estimate the dry-cleaning test.With the results are shown in the table 8 of cut resistance test and dry-cleaning test.
The mensuration of (5) ejection stability
As ink-jet printer, use the system PX-V600 of Seiko Epson Corp, with above-mentioned ink composition for ink-jet recording under 35 ℃, 35% atmosphere, A4 opens at the Qi Luosi of Fuji corporate system XeroxP paper, with the ratio of MS-WORD with the standard of character size 11, MSP black matrix, 4000 word/pages or leaves, print 100 pages, estimate.The AA that is made as that does not have the lettering entanglement fully has the A that is made as of 1 place lettering entanglement, and the B that is made as of 2 places～3 places lettering entanglement is arranged, and the C that is made as of 4 places～5 places lettering entanglement is arranged, and the D that is made as of the above lettering entanglement in 6 places is arranged, and the results are shown in the table 8.
(Embodiment B-2)
(1) preparation of ink for inkjet recording liquid is by using the pigment dispersion B2 that is made by following method, mixes with the vehicle composition shown in the table 9 and carries out.
The making of pigment dispersion B2
Pigment dispersion B2 uses pigment Blue 15: 3 (the blue or green pigment of copper phthalein: grace is special in carat).After the reaction vessel that possesses stirrer, thermometer, return line and dropping funnel carried out nitrogen displacement, put into 75 parts of vinylformic acid benzyl esters, 2 parts in vinylformic acid, 0.3 part of uncle's lauryl mercaptan, be heated to 70 ℃, 20 parts of 1 part of 5 parts of 15 parts in 150 parts of vinylformic acid benzyl esters, vinylformic acid, butyl acrylate cores, uncle's lauryl mercaptan, butanone and the Sodium Persulfate prepared are separately put into dropping funnel for 1 part, through 4 hours, when in reaction vessel, splashing into, make dispersed polymeres carry out polyreaction.Secondly, in reaction vessel, add butanone, make the dispersing polymer solution of 40% concentration.Take out the part of this polymkeric substance, after being dried, utilize differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC), the result who measures second-order transition temperature is 40 ℃.
In addition, mix 40 parts of above-mentioned dispersing polymer solutions, 30 parts of pigment Blue 15s: 3,100 parts of the aqueous sodium hydroxide solutions of 0.1mol/L, 30 parts of butanone.Then, use ultra-high voltage homogenizer (Si Jinuo of Co., Ltd. equipment system A Ludimaici HJP-25005), enforcement 15 times under 200MPa and disperseing.Then, it is transferred in other containers, add 300 parts of ion exchanged waters, and then stirred 1 hour.Then, use the rotary type vaporizer, heat up in a steamer the total amount of butanone and the part of water, the sodium hydroxide neutralization with 0.1mol/L is adjusted to pH9 with it.Then, filter, regulate, form pigment concentration and be 15% pigment dispersion B2 with ion exchanged water with the film filter of 0.3 μ m.The result who utilizes the method identical with Embodiment B-1 to measure particle diameter is 80nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the high molecular particle aqueous dispersions of making by following method by using (emulsion BB), mixes with the vehicle composition shown in the table 10 and carries out.
The making of high molecular particle
In the reaction vessel that possesses drippage device, thermometer, water-cooled reflux exchanger, stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.2 part of the Potassium Persulphate of interpolation polymerization starter, the monomer solution that to put into 0.02 part of 0.05 part of Sodium Lauryl Sulphate BP/USP, 19 parts of vinylformic acid ethyl esters, 15 parts of butyl acrylate cores, 6 parts of (methyl) vinylformic acid castor-oil plant Chun oxazoline esters, 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan in 7 parts of ion exchanged waters is at 70 ℃ of drippages down, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 30 parts of vinylformic acid ethyl esters, 25 parts of methyl acrylate, 10 parts of butyl acrylate cores, 6 parts of vinylformic acid castor-oil plant Chun oxazoline esters, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion BB (EM-BB).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC) to measure second-order transition temperature is-17 ℃.With Embodiment B-1 in the same manner the result of determining molecular weight be 200000.In addition, the acid number based on volumetry is 20mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of Embodiment B-2, utilize the method identical, obtain the jet recorded matter on fabric of sample with Embodiment B-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with Embodiment B-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 8.
The mensuration of (5) ejection stability
Use the black liquid of Embodiment B-2, utilize method identical and identical evaluation method, spray the mensuration of stability with Embodiment B-1.The measurement result of ejection stability is illustrated in the table 8.
(Embodiment B-3)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion B3 that is made by following method, mixes with the vehicle composition shown in the table 9 and carries out.
The making of pigment dispersion B3
Pigment dispersion B3 is to use pigment violet 19 (quinoline a word used for translation ketone pigment: grace is special in carat), and B2 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with Embodiment B-1 to measure particle diameter is 90nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion BB that makes in Embodiment B-2 by using, and carries out with the vehicle composition shown in the table 10.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of Embodiment B-3, utilize the method identical, obtain the jet recorded matter on fabric of sample with Embodiment B-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with Embodiment B-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 8.
The mensuration of (5) ejection stability
Use the black liquid of Embodiment B-3, utilize method identical and identical evaluation method, spray the mensuration of stability with Embodiment B-1.The measurement result of ejection stability is illustrated in the table 8.
(Embodiment B-4)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion B4 that is made by following method, mixes with the vehicle composition shown in the table 9 and carries out.
The making of pigment dispersion B4
Pigment dispersion B4 is to use pigment Yellow 14 (azo pigment: grace is special in carat), and B2 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with Embodiment B-1 to measure particle diameter is 115nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion BB that makes in Embodiment B-2 by using, and carries out with the vehicle composition shown in the table 10.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of Embodiment B-4, utilize the method identical, obtain the jet recorded matter on fabric of sample with Embodiment B-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with Embodiment B-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 8.
The mensuration of (5) ejection stability
Use the black liquid of Embodiment B-4, utilize method identical and identical evaluation method, spray the mensuration of stability with Embodiment B-1.The measurement result of ejection stability is illustrated in the table 8.
(comparative example B-1)
In comparative example B-1, in the pigment stop bath of Embodiment B-1, using and changing to 45 parts of second-order transition temperatures of making for identical adjusting in addition of vinylformic acid benzyl ester by the total amount (45 parts) with the vinylformic acid ethyl ester is 0 ℃ high molecular particle, in addition, with Embodiment B-1 in the same manner, regulate the pigment stop bath.To use the emulsion of this high molecular particle making as emulsion BC (EM-BC).Pigment stop bath composition is illustrated in the table 10.In addition, the black liquid of comparative example B-1 is to use the pigment dispersion identical with Embodiment B-1 to regulate.Black liquid composition is illustrated in the table 9.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.The results are shown in the table 8.
(comparative example B-2)
In comparative example B-2, in the pigment stop bath of Embodiment B-2, use and pass through vinylformic acid ethyl ester total amount (49 parts) instead of the methacrylic acid benzyl ester, it is 10 ℃ high molecular particle that 10 parts of butyl acrylate cores are changed to the second-order transition temperatures of making for identical adjusting beyond 10 parts of the methacrylic acid benzyl esters, in addition, with Embodiment B-2 pigment preparation stop bath in the same manner.To use the emulsion of this high molecular particle making as emulsion BD (EM-BD).The composition of pigment stop bath is illustrated in the table 9.In addition, the black liquid of comparative example B-2 is to use the pigment dispersion identical with Embodiment B-2 to regulate.Black liquid composition is illustrated in the table 9.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.The results are shown in the table 8.
(reference example B-3)
In reference example B-3, in the black liquid of Embodiment B-3, the making particle diameter is that the pigment dispersion of 350nm and 45nm is prepared black liquid in the same manner with Embodiment B-3 in addition.Particle diameter is to measure by the method identical with Embodiment B-1.The dispersion that with particle diameter is 350nm is as pigment dispersion B3A, and the dispersion that with particle diameter is 45nm is as pigment dispersion B3B.Black liquid composition is illustrated in the table 9.In addition, reference example B-3 pigment stop bath uses the pigment stop bath identical with Embodiment B-3.Pigment stop bath composition is illustrated in the table 3.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.The results are shown in the table 8.
(comparative example B-4)
In comparative example B-4, in the pigment stop bath of Embodiment B-4, the acid number of high molecular particle is made as beyond 120mgKOH/g, the 150mgKOH/g and Embodiment B-4 pigment preparation stop bath in the same manner.With the emulsion that uses acid number to make as the high molecular particle of 120mgKOH/g as emulsion BE (EM-BE), with uses acid number as the emulsion of the high molecular particle making of 150mgKOH/g as emulsion BF (EM-BF).Pigment stop bath composition is illustrated in the table 10.In addition, the black liquid of comparative example B-4 uses the black liquid identical with Embodiment B-4.Black liquid composition is illustrated in the table 9.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.The results are shown in the table 8.
(comparative example B-5)
In comparative example B-5, in the pigment stop bath of Embodiment B-2, use that to have ethene be unsaturated group He the compound of oxazolinyl ((methyl) vinylformic acid castor-oil plant Chun oxazoline ester) in addition with Embodiment B-2 pigment preparation stop bath in the same manner.Be unsaturated group with using of no use this to have ethene with the emulsion that the high molecular particle of the compound of oxazolinyl ((methyl) vinylformic acid castor-oil plant Chun oxazoline ester) is made as emulsion BG (EM-BG), is formed the pigment stop bath is illustrated in the table 10.In addition, the black liquid of comparative example B-5 uses the black liquid identical with Embodiment B-2.Black liquid composition is illustrated in the table 9.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.The results are shown in the table 8.
(comparative example B-6)
In comparative example B-6, in the pigment stop bath of Embodiment B-3, do not use that to have ethene be unsaturated group He the compound of oxazolinyl ((methyl) vinylformic acid castor-oil plant Chun oxazoline ester) in addition with Embodiment B-3 pigment preparation stop bath in the same manner.Pigment stop bath composition is illustrated in the table 10.In addition, the black liquid of comparative example B-6 uses the black liquid identical with Embodiment B-3.Black liquid composition is illustrated in the table 9.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.The results are shown in the table 8.
[table 8]
The result of the wear resistance among table 8 Embodiment B-1～4, comparative example B-1～2,4～6, the reference example B-3, dry-cleaning property, ejection stability
Figure A20091000800000401
The unit of Tg is ℃, and particle diameter is the median size of pigment, and unit is nm, and the unit of acid number is mgKOH/g, and wear resistance, dry-cleaning property are based on the metewand of JIS.
[table 9]
The black liquid of table 9 Embodiment B-1～4, comparative example B-1～2,4～6, reference example B-3 is formed (quality %)
Figure A20091000800000402
Represent pigment concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
The TMP TriMethylolPropane(TMP)
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
[table 10]
The pigment stop bath of table 10 Embodiment B-1～4, comparative example B-1～2,4～6, reference example B-3 is formed (quality %)
Figure A20091000800000411
Represent polymer concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
Alkane in the TMP trishydroxymethyl
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
(Embodiment B-5)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is the pigment dispersion B5 that is made by following method by using, and mixes with the vehicle composition shown in the table 12 and carries out.
The making of pigment dispersion B5
It is the system MA100 of Mitsubishi Chemical Industrial Co., Ltd that pigment dispersion 5 uses carbon black (PBk7).Utilize with special and open the identical method of flat 8-3498 communique, the surface of oxygenated black can be scattered in the water it, forms dispersion B5.The result who utilizes the identical method of Embodiment B-1 to measure particle diameter is 120nm.
2) preparation of pigment stop bath
The preparation of pigment stop bath is the high molecular particle aqueous dispersions of being made by following method by using (emulsion BI), carries out with the vehicle composition shown in the table 13.
The making of high molecular particle
In the reaction vessel that possesses drippage device, thermometer, water-cooled reflux exchanger, stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.3 part of the Potassium Persulphate of interpolation polymerization starter, and the monomer solution that will put into 0.02 part of 0.05 part of Sodium Lauryl Sulphate BP/USP, 20 parts of vinylformic acid ethyl esters, 15 parts of butyl acrylate cores, 6 parts of vinylformic acid Lauryl Ester, 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan in 7 parts of ion exchanged waters is at 70 ℃ of drippages down, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 30 parts of vinylformic acid ethyl esters, 25 parts of butyl acrylate cores, 10 parts of vinylformic acid Lauryl Ester, 6 parts of methacrylic acid castor-oil plant Chun oxazoline esters, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion BI (EM-BI).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC) to measure second-order transition temperature is-17 ℃.With Embodiment B-1 in the same manner the result of determining molecular weight be 180000.In addition, the acid number based on volumetry is 18mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of Embodiment B-5, utilize the method identical, obtain the jet recorded matter on fabric of sample with Embodiment B-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with Embodiment B-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 11.
The mensuration of (5) ejection stability
Use the black liquid of Embodiment B-5, utilize method identical and identical evaluation method, spray the mensuration of stability with Embodiment B-1.The measurement result of ejection stability is illustrated in the table 11
(Embodiment B-6)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is the pigment dispersion B6 that is made by following method by using, and mixes with the vehicle composition shown in the table 12 and carries out.
The manufacturing of pigment dispersion B6
Pigment dispersion B6 uses pigment Blue 15: 3 (the blue or green pigment of copper phthalein: grace is special in carat).To possessing stirrer, thermometer, after the reaction vessel of return line and dropping funnel carries out the nitrogen displacement, under 70 ℃, put into 45 parts of vinylbenzene, 30 parts of poly(oxyethylene glycol) 400 acrylate, 10 parts of vinylformic acid benzyl esters, 2 parts in vinylformic acid, 0.3 part of uncle's lauryl mercaptan, and be heated, with 150 parts of the vinylbenzene prepared separately, 100 parts of poly(oxyethylene glycol) 400 acrylate, 15 parts in vinylformic acid, 15 parts of butyl acrylate cores, 1 part of uncle's lauryl mercaptan and Sodium Persulfate are put into dropping funnel for 5 parts, through 4 hours, when in reaction vessel, splashing into, make dispersed polymeres carry out polyreaction.Secondly, in reaction vessel, add water, make the dispersing polymer solution of 40% concentration.Take out the part of this polymkeric substance, after being dried, utilize differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC), the result who measures second-order transition temperature is 45 ℃.
In addition, mix 40 parts of above-mentioned dispersing polymer solutions, 30 parts of pigment Blue 15s: 100 parts of the aqueous sodium hydroxide solutions of 3 (the blue or green pigment of copper phthalein: grace is special in carat), 0.1mol/L, adopt the Chinese mugwort lattice grinding machine that has used zirconium oxide bead, disperseed through 2 hours.Then, it is transferred to other containers, add 300 parts of ion exchanged waters, and then stirred 1 hour.Also have, the sodium hydroxide neutralization with 0.1mol/L is adjusted to pH9 with it.Then, filter, form solid state component (dispersed polymeres and pigment Blue 15: 3) be 20% dispersion B5 with the film filter of 0.3 μ m.The result who utilizes the method identical with Embodiment B-1 to measure particle diameter is 100nm.The result of determining molecular weight is 210000.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the high molecular particle aqueous dispersions of making by following method by using (emulsion BJ), mixes with the vehicle composition shown in the table 13 and carries out.
The making of high molecular particle
In the reaction vessel that possesses drippage device, thermometer, water-cooled reflux exchanger, stirrer, put into 100 parts of ion exchanged waters, when stirring, under 70 ℃ of nitrogen atmosphere, 0.3 part of the Potassium Persulphate of interpolation polymerization starter, the monomer solution that to put into 0.02 part of 0.05 part of Sodium Lauryl Sulphate BP/USP, 20 parts of vinylformic acid ethyl esters, 25 parts of butyl acrylate cores, 6 parts of lauryl acrylate, 5 parts of methacrylic acid butyl esters and uncle's lauryl mercaptan in 7 parts of ion exchanged waters is at 70 ℃ of drippages down, make its reaction, make one time material.Stir when in a described material, adding 2 parts of ammonium persulphate 10% solution, and then will be by 30 parts of ion exchanged waters, 0.2 part of lauryl potassium sulfate, 20 parts of vinylformic acid ethyl esters, 20 parts of butyl acrylate cores, 14 parts of lauryl acrylate, 6 parts of methacrylic acid castor-oil plant Chun oxazoline esters, 5 parts in vinylformic acid, the reaction solution of 0.5 part of formation of uncle's lauryl mercaptan adds when 70 ℃ are stirred down, after making its polymerization reaction take place, neutralize with sodium hydroxide, make it become pH8～8.5, its strainer with 0.3 μ m is filtered, make the high molecular particle aqueous dispersions, form emulsion BJ (EM-BJ).Take out the part of this high molecular particle aqueous dispersions, after being dried, the result who utilizes differential operation type calorimeter (Seiko electronics system EXSTAR6000DSC) to measure second-order transition temperature is-18 ℃.In addition, the acid number based on volumetry is 18mgKOH/g.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of Embodiment B-6, utilize the method identical, obtain the jet recorded matter on fabric of sample with Embodiment B-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with Embodiment B-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 11.
The mensuration of (5) ejection stability
Use the black liquid of Embodiment B-6, utilize method identical and identical evaluation method, spray the mensuration of stability with Embodiment B-1.The measurement result of ejection stability is illustrated in the table 11.
(Embodiment B-7)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion B7 that is made by following method, mixes with the vehicle composition shown in the table 12 and carries out.
The making of pigment dispersion B7
Pigment dispersion B7 is to use pigment red 122 (dimethyl quinoline a word used for translation ketone pigment: grace is special in carat), and B6 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with Embodiment B-1 to measure particle diameter is 80nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion BJ that makes in Embodiment B-6 by using, and carries out with the vehicle composition shown in the table 13.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of Embodiment B-7, utilize the method identical, obtain the jet recorded matter on fabric of sample with Embodiment B-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with Embodiment B-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 11.
The mensuration of (5) ejection stability
Use the black liquid of Embodiment B-7, utilize method identical and identical evaluation method, spray the mensuration of stability with Embodiment B-1.The measurement result of ejection stability is illustrated in the table 11.
(Embodiment B-8)
(1) preparation of ink for inkjet recording liquid
The preparation of ink for inkjet recording liquid is by using the pigment dispersion B8 that is made by following method, mixes with the vehicle composition shown in the table 12 and carries out.
The making of pigment dispersion B8
Pigment dispersion B8 is to use Pigment Yellow 73 180 (the benzene imidazolone is two diazonium series pigments: grace is special in carat), and B6 makes in the same manner with pigment dispersion.In addition, the result who utilizes the method identical with Embodiment B-1 to measure particle diameter is 130nm.
(2) preparation of pigment stop bath
The preparation of pigment stop bath is the emulsion BJ that makes in Embodiment B-6 by using, and carries out with the vehicle composition shown in the table 13.
(3) manufacture method of jet recorded matter on fabric
Use the black liquid and the pigment stop bath of Embodiment B-8, utilize the method identical, obtain the jet recorded matter on fabric of sample with Embodiment B-1.
(4) cut resistance test and the test of dry-cleaning property
About above-mentioned sample (jet recorded matter on fabric), with Embodiment B-1 in the same manner, carry out cut resistance test and the test of dry-cleaning property.The results are shown in the table 11.
The mensuration of (5) ejection stability
Use the black liquid of Embodiment B-8, utilize method identical and identical evaluation method, spray the mensuration of stability with Embodiment B-1.The measurement result of ejection stability is illustrated in the table 11.
(reference example B-7)
In reference example B-7, the molecular weight of the high molecular particle of the pigment stop bath of Embodiment B-5 changed to 90000 and 1100000 beyond with Embodiment B-5 pigment preparation stop bath in the same manner.With molecular weight be 90000 emulsion as emulsion BK (EM-BK), be that 1100000 emulsion is as emulsion BL (EM-BL) with molecular weight.Pigment stop bath composition is illustrated in the table 13.In addition, the black liquid of reference example B-7 is to use the pigment dispersion identical with Embodiment B-5 to regulate.Black liquid composition is illustrated in the table 12.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.Structure is illustrated in the table 11.
(reference example B-8)
In reference example B-8, in Embodiment B-6, will be as 1,1 of 2-aklylene glycol, 2-hexylene glycol are prepared black liquid and pigment stop bath in the same manner with Embodiment B-6 beyond being replaced into glycerine.Black liquid composition is illustrated in the table 12, pigment stop bath composition is illustrated in the table 13.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.Structure is illustrated in the table 11.
(reference example B-9)
In reference example B-9, in Embodiment B-7, be that tensio-active agent and alkynol are to prepare black liquid and pigment stop bath in the same manner with Embodiment B-7 beyond tensio-active agent is replaced into glycerine with alkyne diol.Black liquid composition is illustrated in the table 12, pigment stop bath composition is illustrated in the table 13.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.Structure is illustrated in the table 11.
(reference example B-10)
In reference example B-10, in Embodiment B-8, with the high molecular particle of pigment stop bath be made as 80%, 50% by pigment ratio beyond prepare black liquid and pigment stop bath in the same manner with Embodiment B-8.Black liquid composition is illustrated in the table 12, pigment stop bath composition is illustrated in the table 13.The adjusting of jet recorded matter on fabric sample, cut resistance test, dry-cleaning test and ejection stability test and Embodiment B-1 are carried out in the same manner.Structure is illustrated in the table 11.
(reference example B-11～15)
In reference example B-11～15, in Embodiment B-6, be produced on the sample of the comprehensive lettering of cotton, will carry out various changes and estimate wear resistance in the same manner with Embodiment B-6 beyond handling in 5 minutes condition of 150 ℃ of heat treated.Will be in order to compare with Embodiment B-6, the example that changes various conditions the results are shown in the table 14 as a reference example B-11～15.
[table 11]
The result of the wear resistance in table 11 Embodiment B-5～8, reference example B-7～10, dry-cleaning property, ejection stability
Figure A20091000800000471
The unit of Tg is ℃, and particle diameter is the median size of pigment, and unit is nm, and the unit of acid number is mgKOH/g.
Molecular weight in the table 11 is * 10 5
Pigment ratio is represented % with respect to the high molecular particle of pigment.
Wear resistance, dry-cleaning property are based on the metewand of JIS.
[table 12]
The black liquid of table 12 Embodiment B-5～8 and reference example B-7～10 is formed (quality %)
Figure A20091000800000481
Represent pigment concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
The TMP TriMethylolPropane(TMP)
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
[table 13]
The pigment stop bath of table 13 Embodiment B-5～8 and reference example B-7～10 is formed (quality %)
Figure A20091000800000491
Represent polymer concentration by solid state component.
1,2-HD 1, the 2-hexylene glycol
1,2-PD 1, the 2-pentanediol
TEGmBE triglycol single-butyl ether
S-104 Sa Fei Nore 104 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-465 Sa Fei Nore 465 (a day letter chemistry system alkyne diol is a tensio-active agent)
S-61 Sa Fei Nore 61 (a day letter chemistry system alkynol is a tensio-active agent)
The TMP TriMethylolPropane(TMP)
The TEG triglycol
The 2-P 2-Pyrrolidone
The TEA trolamine
[table 14]
Frictional property test-results when having changed heating condition in table 14 Embodiment B-6
Figure A20091000800000492

Claims (21)

1. a pigment stop bath is characterized in that,
Contain high molecular particle, the second-order transition temperature of this high molecular particle is below-10 ℃, acid number is below the 100mgKOH/g, this high molecular particle is that to use (methyl) acrylate at least as its constituent be that the reactive compounds of unsaturated group and reactive group comes synthetic with having ethene, and described (methyl) acrylate is (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester.
2. pigment stop bath according to claim 1 is characterized in that,
Described reactive group is a blocked isocyanate Huo oxazolinyl.
3. pigment stop bath according to claim 1 and 2 is characterized in that,
With respect to described high molecular particle total amount, contain 70 quality % above described (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester.
4. according to each described pigment stop bath in the claim 1～3, it is characterized in that,
Described (methyl) alkyl acrylate and/or (methyl) vinylformic acid cyclic alkyl ester are (methyl) vinylformic acid C 1-24Alkyl ester and/or (methyl) vinylformic acid C 3-24The cyclic alkyl ester.
5. according to each described pigment stop bath in the claim 1～4, it is characterized in that,
The vinylbenzene conversion weight-average molecular weight of using gel permeation chromatography of described high molecular particle is more than 100000 and below 1000000.
6. black liquid group is characterized in that having:
Each described pigment stop bath in ink composition and the claim 1～5, described ink composition contain can be with the dispersion of colo(u)rant dispersion in water.
7. black liquid group according to claim 6 is characterized in that,
The median size of described dispersion is more than the 50nm and below the 300nm.
8. black liquid group according to claim 7 is characterized in that,
Described dispersion be can under not having the situation of dispersion agent, be scattered in the water, median size be more than the 50nm and below the 300nm from disperse black carbon.
9. black liquid group according to claim 8 is characterized in that,
Described dispersion can use polymkeric substance that pigment dyestuff is scattered in the water, and median size is that 50nm is above and below the 300nm, the vinylbenzene conversion weight-average molecular weight of using gel permeation chromatography of this polymkeric substance is more than 10000 and below 200000.
10. according to each described black liquid group in the claim 6～9, it is characterized in that,
Described ink composition contains 1, the 2-aklylene glycol.
11. according to each described black liquid group in the claim 6～10, it is characterized in that,
It is that tensio-active agent and/or alkynol are tensio-active agent that described ink composition contains alkyne diol.
12. according to each described black liquid group in the claim 6～11, it is characterized in that,
In quality %, the content of described high molecular particle is more than the content of described pigment.
13. the manufacture method of a jet recorded matter on fabric is characterized in that, comprising:
To contain can make the dispersion of colo(u)rant dispersion in water the ink composition ink jet printing in the operation of cloth and silk;
This print be impregnated in the operation of each described pigment stop bath in the claim 1～5;
More than 110 ℃ and below 200 ℃, the operation of print thermal treatment more than 1 minute that this is impregnated.
14. the manufacture method of a jet recorded matter on fabric is characterized in that, comprising:
To contain can make the dispersion of colo(u)rant dispersion in water the ink composition ink jet printing in the operation of cloth and silk;
Utilize ink jet method, each described pigment stop bath in the claim 1～5 is coated on the operation of this print;
More than 110 ℃ and below 200 ℃, the operation of print thermal treatment more than 1 minute that this is coated.
15. the manufacture method according to claim 13 or 14 described jet recorded matter on fabric is characterized in that,
The median size of described dispersion is more than the 50nm and below the 300nm.
16. the manufacture method of jet recorded matter on fabric according to claim 15 is characterized in that,
Described dispersion be can under not having the situation of dispersion agent, be scattered in the water, median size be more than the 50nm and below the 300nm from disperse black carbon.
17. the manufacture method according to each described jet recorded matter on fabric in the claim 15 is characterized in that,
Described dispersion can use polymkeric substance that pigment dyestuff is scattered in the water, and median size is that 50nm is above and below the 300nm, the vinylbenzene conversion weight-average molecular weight of using gel permeation chromatography of this polymkeric substance is more than 10000 and below 200000.
18. the manufacture method according to each described jet recorded matter on fabric in the claim 13～17 is characterized in that,
Described ink composition contains 1, the 2-aklylene glycol.
19. the manufacture method according to each described jet recorded matter on fabric in the claim 13～18 is characterized in that,
It is that tensio-active agent and/or alkynol are tensio-active agent that described ink composition contains alkyne diol.
20. the manufacture method according to each described jet recorded matter on fabric in the claim 13～19 is characterized in that,
In quality %, the content of described high molecular particle is more than the content of described pigment.
21. a jet recorded matter on fabric is characterized in that,
It is to utilize that the manufacture method of each described jet recorded matter on fabric obtains in the claim 13～20.
CNA2009100080005A 2008-03-06 2009-03-06 Liquid composition for making pigment fixed, ink set, method for producing ink jet recorded matter on fabric and ink jet recorded matter on fabric Pending CN101525462A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102741368A (en) * 2010-02-12 2012-10-17 惠普发展公司，有限责任合伙企业 Fixer fluid composition and inkjet ink sets including the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102741368A (en) * 2010-02-12 2012-10-17 惠普发展公司，有限责任合伙企业 Fixer fluid composition and inkjet ink sets including the same

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