CN104031478B - Painted pigment dyestuff aqueous color paste of a kind of synthetic leather and preparation method thereof - Google Patents
Painted pigment dyestuff aqueous color paste of a kind of synthetic leather and preparation method thereof Download PDFInfo
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- CN104031478B CN104031478B CN201410315143.1A CN201410315143A CN104031478B CN 104031478 B CN104031478 B CN 104031478B CN 201410315143 A CN201410315143 A CN 201410315143A CN 104031478 B CN104031478 B CN 104031478B
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Abstract
The present invention relates to painted pigment dyestuff aqueous color paste of a kind of synthetic leather and preparation method thereof, the painted pigment dyestuff aqueous color paste of described synthetic leather comprises the components such as the pigment dyestuff of modification, wetting agent, dispersion agent, deionized water, wetting Agent for Printing Inks, pH value regulator and antimildew disinfectant, through dispersion, grinding, filter, deaeration preparation and obtaining.The painted pigment dyestuff aqueous color paste of the synthetic leather that the present invention prepares, has tinting strength and fastness to wet rubbing is high, the feature of pigment migration can not occur in coloring process, is specially adapted to the painted field of wet-method synthetic leather.
Description
Technical field
The invention belongs to technical field of fine, specifically, the present invention relates to painted pigment dyestuff aqueous color paste of a kind of synthetic leather and preparation method thereof.
Background technology
Along with the development of human society, between natural leather supply and consumer demand, imbalance between supply and demand is more and more outstanding, in order to solve the shortage problem of natural leather, meet the ever-increasing demand to various dress ornament and decorative fabric of human consumer, the surrogate using different chemical raw material to manufacture natural leather becomes an important industry gradually; Wherein, Synthetic Leather, owing to having the advantages such as wear-resisting, cold-resistant, good hand touch, ageing-resistant, moisture-penetrable ventilated performance are good, becomes one of optimal selection of alternative natural leather, has been widely used in the fields such as clothes, shoemaking, case and bag, furniture.
Wet polyurethane synthetic leather technique is current topmost synthetic leather production technique, this technique by stock dispersion such as urethane resin and tinting material, Mierocrystalline cellulose, processing aids at N, mixed slurry is made in dinethylformamide, subsequently this mixed slurry is evenly attached to Ji Bushang through techniques such as dipping or single paintings, to enter in precipitation bath after wet type film forming again, through washing, tentering, drying, form bass, then carry out the rear processing finishings such as dry adhered, sharpening skin, printing, embossing as required and obtain synthetic leather.In order to obtain the synthetic leather of different color, need to add tinting material in synthetic leather preparation process.At present, major part use for synthetic leather tinting material is all that dispersion medium prepares the solvent-borne type mill base or color that obtain with organic solvent, solvent-borne type mill base and color not only can bring pollution to environment in production and application process, certain injury is produced to the health of production operation personnel, and also there is huge potential safety hazard in production, transport and storage link.
The advantage such as aqueous color paste has environmental protection, is harmful to human health, price is low, the problems such as the environmental pollution that solvent-borne type mill base not only can be avoided to bring, Occupational Disease Hazards and potential safety hazard, also have that pigment content is high, fineness is little, viscosity is low, tinting strength is high, low cost and other advantages.Pigment dyestuff is compared with mineral dye with dyestuff, has the advantages such as lovely luster, tinctorial strength are high, good weatherability, is the conventional tinting material of synthetic leather industry.
In recent years, disclose the preparation method of the painted use mill base of multiple synthetic leather, Chinese patent application CN201110305616.6 discloses a kind of fatty alcohol-polyoxyethylene ether that uses and makes dispersion agent, and add a small amount of Water/oil dual-purpose acrylic resin, adopt the mode of ball mill grinding to prepare the method for wet-method synthetic leather use black slurry; Chinese patent application CN200810147698.4 uses dispersion agent, one package stabilizer and stably dispersing auxiliary agent dispersed inorganic nano dye, prepares leather nano pigment paste, has good antibacterial and mouldproof performance, resistance to uv irradiating performance and flame retardant properties.
But, the painted use mill base of synthetic leather prepared by prior art uses acrylic-type dispersion agent mostly, due to acrylic resin and urethane resin poor compatibility, when using the mill base of acrylic acid dispersant grinding painted for the synthesis of leather, granules of pigments reunion often occurs because of the desorption of dispersion agent causes tinting strength to decline, pigment migration is to the phenomenon in precipitation bath, simultaneously, with synthetic leather prepared by pigment dyestuff aqueous color paste, because the consistency of organic pigment particle and other component of synthetic leather is poor, its fastness to wet rubbing is often difficult to the requirement reaching client.
Surface modification is carried out to granules of pigments, the physical and chemical performance of pigment particle surface can be changed, promote its effect in field, downstream.Such as, US Patent No. 6358308A describes a kind of liquid or supercritical co of using and carries out the method for aftertreatment to pigment dyestuff, Chinese patent application CN201210545201.0 discloses a kind of use rosin process granules of pigments, to improve the method for its dielectric loss.But do not disclose by carrying out surface modification to organic pigment particle and preparing the method for use for synthetic leather aqueous color paste with modified pigment in prior art, to solve consistency and the synthetic leather fastness to wet rubbing of other component of synthetic leather and granules of pigments, and prevent the technical problem that pigment migration occurs in surperficial synthetic leather coloring process.
Summary of the invention
In view of this, in order to solve the technical problem existing for aqueous color paste described in the prior art, the object of the present invention is to provide painted pigment dyestuff aqueous color paste of a kind of synthetic leather and preparation method thereof.
In order to solve the problems of the technologies described above, a first aspect of the present invention provides following technical scheme:
A pigment dyestuff for modification, is characterized in that being prepared by following steps:
A) in the toluene occupying machine pigment mass 300% to 500%, add pigment dyestuff and be uniformly mixed at least 30 minutes, obtain premixed slurries;
B) properties-correcting agent occupying machine pigment mass 2-5% is added in the premixed slurries that step a) obtains, stir at least 30 minutes, and grind;
C) by step b) slurry after grinding after filtration and vacuum-drying, obtain the pigment dyestuff of described modification.
Wherein, step b) in can select three-roll grinder, grind 20 to 50 minutes.
Wherein, step b) properties-correcting agent used is for having the compound of general formula (I) structure:
In general formula (I), A is any one and the reacted residue of isocyanate groups in 4-hydroxyethyl imidazole, 2-AMINO-4-PICOLINE, nonyl phenol, octyl phenol; R is the part in tolylene diisocyanate or ditane-4,4 '-vulcabond except isocyanate groups; Wherein, m and n is integer, and 5≤m≤20,3≤n≤8.
Wherein, the described material with general formula (I) structure, can by tolylene diisocyanate or ditane-4, the polyether glycol of 4 '-vulcabond and different polymerization degree is at toluene, in acetone and other organic solvent, first reaction forms molecular chain two ends is by a certain percentage the urethane of isocyanate groups, add 4-hydroxyethyl imidazole again, 2-AMINO-4-PICOLINE, nonyl phenol, any one in octyl phenol carries out end-blocking preparation to it and obtains, in reaction process, for increasing speed of response, stannous octoate can be used, catalyzer conventional in the urethane building-up processes such as dibutyl tin laurate.The polymerization degree that can control polyether glycol used, to control the m value in general formula (I), controls the n value in general formula (I) by the mol ratio controlled between polyether glycol and vulcabond.
According to " pigment index " (C.I., the method of the concrete pigment material of expression commonly used of pigment relevant industries such as ColourIndex), can by the sequentially numbering arrangement of the pigment of same color, as phthalocyanine blue 15:1 pigment is named as pigment Blue 15: 1, benzimidazolone yellow is named as pigment yellow 154.In the present invention, any one pigment in Pigment red 170, Pigment red 254, pigment orange 38, pigment Violet 23 and Pigment Yellow 73 74 can be chosen, and the concrete structure of above-mentioned pigment and title can be inquired about from conventional books such as " pigment dyestuff index cards ".
A second aspect of the present invention, also relates to the painted pigment dyestuff aqueous color paste of a kind of synthetic leather, it is characterized in that, described aqueous color paste comprises the pigment dyestuff of above-mentioned modification, wetting agent, dispersion agent, wetting Agent for Printing Inks, pH value regulator and deionized water; Wherein, the pigment dyestuff of described modification accounts for the 30-45% of aqueous color paste total mass, the pigment dyestuff mass ratio of described wetting agent and modification is 0.02-0.08:1, and the mass ratio of the pigment dyestuff of described dispersion agent and modification is 0.08-0.12:1, and described wetting Agent for Printing Inks accounts for the 8-15% of aqueous color paste total mass.
Wherein, described wetting agent is at least one in phosphatidylcholine, Dodecyl Glucoside.
Wherein, dispersion agent used is for having the compound of general formula (II) structure:
In general formula (II), m
1and n
1for integer, and 5≤m
1≤ 30,1≤n
1≤ 5.
There is the material of general formula (II) structure, can be prepared oxyethane open loop again by nonyl phenol and formaldehyde reaction product and be obtained, its preparation technology, known by organic synthesis those skilled in the art, can control m in general formula (II) by the mol ratio controlled between nonyl phenol, formaldehyde, oxyethane
1and n
1concrete numerical value.But in actual industrial production, have in the material of general formula (II) structure, m
1and n
1value in fact have numerical value differ, in certain numerical value distribution may, and formaldehyde also likely and between hydroxyl the hydrogen of position react.
Wherein, described wetting Agent for Printing Inks is at least one in ethylene glycol, propylene glycol, glycerol and glycol ether.PH value regulator used comprises at least one in sodium hydroxide, potassium hydroxide, ammoniacal liquor, triethylamine and trolamine.
In addition, in described aqueous color paste, for avoiding occurring to occur the phenomenons such as mill base is rotten, mould-growth in some cases because of the microbial growth such as bacterium, yeast, in use also add a certain amount of antimildew disinfectant.In the present invention, antimildew disinfectant used is selected from least one in BIT, 5-chloro-2-methyl-1-isothiazoline-3-ketone.These two kinds of antimildew disinfectants commercial generally exist all in form of an aqueous solutions, and in the present invention, its effective constituent is generally no more than 0.05% of aqueous color paste total mass.
A third aspect of the present invention, also relates to the preparation method of the painted pigment dyestuff aqueous color paste of above-mentioned synthetic leather, it is characterized in that comprising the steps:
A) all the other deionized waters and wetting agent, dispersion agent, wetting Agent for Printing Inks are disperseed by the 10-20% of reserved deionized water total mass in dispersion machine, add pH value regulator subsequently and regulate the pH value of mixed solution between 8-9, obtain premix;
B) pigment dyestuff of modification is added in the premix that step a) obtains and disperse, use dispersion machine to be not less than 30 minutes higher than the Rate Dispersion of 200 revs/min, and add in dispersion process step a) in reserved deionized water, obtain pre-mixing pigment slurry;
C) by step b) the pre-mixing pigment slurry that obtains grinds in horizontal mill, and the median size being ground to granules of pigments is less than 0.5 μm, then adds antimildew disinfectant and mix, and after filtration, deaeration, obtains described aqueous color paste.
In this preparation process, the median size of granules of pigments can adopt the laser particle analyzer of industrial conventional test aqueous color paste size distribution, as the Mastersizer2000 laser particle size analyzer of Malvern Instr Ltd. of Britain.
Compared with prior art, the present invention has following beneficial effect:
Aqueous color paste of the present invention has higher tinting strength and fastness to wet rubbing, and pigment migration can not occur in coloring process, and described aqueous color paste is specially adapted to use as the tinting material of wet polyurethane synthetic leather technique.
Embodiment
Below with reference to specific embodiment, the painted pigment dyestuff aqueous color paste of synthetic leather of the present invention and raw material, preparation method and performance etc. are described in further detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, the scope be not intended to limit the present invention.
(1) preparation of the pigment dyestuff of modification
Embodiment 1 to 5 properties-correcting agent used has the structure of general formula (I):
Wherein, in modifier A, m is 5, n be 6, A is 4-hydroxyethyl imidazole and the reacted residue of isocyanate groups, and R is the part in tolylene diisocyanate except isocyanate groups; In properties-correcting agent B, m is 20, n be 3, A is 2-AMINO-4-PICOLINE and the reacted residue of isocyanate groups, and R is the part in ditane-4,4 '-vulcabond except isocyanate groups; In properties-correcting agent C, m is 10, n be 8, A is nonyl phenol and the reacted residue of isocyanate groups, and R is the part in tolylene diisocyanate except isocyanate groups; In properties-correcting agent D, m is 15, n be 5, A is octyl phenol and the reacted residue of isocyanate groups, and R is the part in ditane-4,4 '-vulcabond except isocyanate groups.
Embodiment 1
In 1200 grams of toluene, add 400 grams of Pigment reds 170 and be uniformly mixed 50 minutes, obtain premixed slurries, again 20 grams of modifier As are added in premixed slurries, stir 50 minutes, again after three-roll grinder grinds 20 minutes, by the slurry after grinding after filtration and vacuum-drying, obtain the Pigment red 170 through modification.
Embodiment 2
In 2000 grams of toluene, add 400 grams of Pigment reds 254 and be uniformly mixed 30 minutes, obtain premixed slurries, again 8 grams of properties-correcting agent B are added in premixed slurries, stir 40 minutes, again after three-roll grinder grinds 30 minutes, by the slurry after grinding after filtration and vacuum-drying, obtain the Pigment red 254 through modification.
Embodiment 3
In 2000 grams of toluene, add 500 grams of pigment oranges 38 and be uniformly mixed 30 minutes, obtain premixed slurries, again 15 grams of properties-correcting agent C are added in premixed slurries, stir 50 minutes, again after three-roll grinder grinds 50 minutes, by the slurry after grinding after filtration and vacuum-drying, obtain the pigment orange 38 through modification.
Embodiment 4
In 2000 grams of toluene, add 450 grams of pigment Violet 23s and be uniformly mixed 45 minutes, obtain premixed slurries, again 18 grams of properties-correcting agent D are added in premixed slurries, stir 30 minutes, again after three-roll grinder grinds 40 minutes, by the slurry after grinding after filtration and vacuum-drying, obtain the pigment Violet 23 through modification.
Embodiment 5
In 2000 grams of toluene, add 350 grams of Pigment Yellow 73s 74 and be uniformly mixed 40 minutes, obtain premixed slurries, again 12 grams of properties-correcting agent B are added in premixed slurries, stir 30 minutes, again after three-roll grinder grinds 50 minutes, by the slurry after grinding after filtration and vacuum-drying, obtain the Pigment Yellow 73 74 through modification.
(2) preparation of the painted pigment dyestuff aqueous color paste of synthetic leather
In table 1, component used is implemented in each embodiment and contrast, all account for the percentage calculation of synthetic leather painted pigment dyestuff aqueous color paste total mass with it, embodiment 6-10 and comparative example 11-14, dispersant A, dispersant B and dispersing agent C are the compound with general formula (II) structure:
The compound of general formula (II) structure is prepared oxyethane open loop by nonyl phenol and formaldehyde reaction product and is obtained, mol ratio between dispersant A nonyl phenol used, formaldehyde, oxyethane raw material is 3:2:90, mol ratio between dispersant B nonyl phenol used, formaldehyde, oxyethane raw material is 7:6:35, and the mol ratio between dispersing agent C nonyl phenol used, formaldehyde, oxyethane raw material is 5:4:90.
In table 1, the preparation process of embodiment 6-10 and comparative example 11-14 mill base is: 20% of reserved deionized water total mass, all the other deionized waters and wetting agent, dispersion agent and the wetting Agent for Printing Inks such as ethylene glycol, propylene glycol are disperseed in dispersion machine, adding pH value regulator subsequently regulates the pH value of mixed solution between 8-9, obtains premix; Disperse adding in above-mentioned premix through the pigment dyestuff of modification or the pigment dyestuff of non-modified, use dispersion machine to be not less than 30 minutes higher than the Rate Dispersion of 200 revs/min, and in dispersion process, add reserved deionized water, obtain pre-mixing pigment slurry; Ground in horizontal mill by above-mentioned pre-mixing pigment slurry, the median size being ground to granules of pigments is less than 0.5 μm, then adds antimildew disinfectant and mix, and after filtration, deaeration, obtains the painted pigment dyestuff aqueous color paste of described synthetic leather.
(3) performance test of the painted pigment dyestuff aqueous color paste of synthetic leather
The B method testing example 6 specified according to light industry standard QB/T4343-2012 " use for synthetic leather aqueous color paste " Appendix B and comparative example 11 and 12 prepare the colour strength vis-a-vis of the painted pigment dyestuff aqueous color paste of synthetic leather, using the aqueous color paste of embodiment 6 preparation as reference mill base; In like manner, using the aqueous color paste of embodiment 10 preparation as reference mill base, test comparison example 13 and 14 prepares the colour strength vis-a-vis of the painted pigment dyestuff aqueous color paste of synthetic leather.
Respectively get the painted pigment dyestuff aqueous color paste of synthetic leather prepared by 50 grams of embodiment 6-10 and comparative example 11-14, be dispersed in 3 kilograms of synthetic leather film forming binder that prepared, non-coloring material, again by this base-material blade coating on base cloth, blade coating thickness is 0.5 millimeter, the above-mentioned base cloth getting each 10 centimetres of length and width is extracted after solidifying 3 minutes in containing 200 milliliters of solidification liquids of 10%DMF, observes solidification liquid whether variable color.The fastness to wet rubbing of the method test synthetic leather specified with light industry standard QB/T1327-1991 " leather surface colour fastness test testing method ", the result display of test in table 2.
Claims (8)
1. a pigment dyestuff for modification, be is characterized in that: prepared by following steps:
A) in the toluene occupying machine pigment mass 300% to 500%, add pigment dyestuff and be uniformly mixed at least 30 minutes, obtain premixed slurries;
B) properties-correcting agent occupying machine pigment mass 2-5% is added in the premixed slurries that step a) obtains, stir at least 30 minutes, and grind; Properties-correcting agent used is for having the compound of general formula (I) structure:
In general formula (I), A is any one and the reacted residue of isocyanate groups in 4-hydroxyethyl imidazole, 2-AMINO-4-PICOLINE, nonyl phenol, octyl phenol; R is the part in tolylene diisocyanate or ditane-4,4 '-vulcabond except isocyanate groups; Wherein, m and n is integer, and 5≤m≤20,3≤n≤8;
C) by step b) slurry after grinding after filtration and vacuum-drying, obtain the pigment dyestuff of described modification.
2. the painted pigment dyestuff aqueous color paste of synthetic leather, is characterized in that: described aqueous color paste comprises the pigment dyestuff of claim 1 modification, wetting agent, dispersion agent, wetting Agent for Printing Inks, pH value regulator and deionized water; And described dispersion agent is for having the compound of general formula (II) structure:
In general formula (II), m
1and n
1for integer, and 5≤m
1≤ 30,1≤n
1≤ 5.
3. aqueous color paste according to claim 2, it is characterized in that: the pigment dyestuff of described modification accounts for the 30-45% of aqueous color paste total mass, the pigment dyestuff mass ratio of described wetting agent and modification is 0.02-0.08:1, the mass ratio of the pigment dyestuff of described dispersion agent and modification is 0.08-0.12:1, and described wetting Agent for Printing Inks accounts for the 8-15% of aqueous color paste total mass.
4. aqueous color paste according to claim 2, is characterized in that: described wetting agent is at least one in phosphatidylcholine, Dodecyl Glucoside.
5. aqueous color paste according to claim 2, is characterized in that: described wetting Agent for Printing Inks is at least one in ethylene glycol, propylene glycol, glycerol and glycol ether.
6. aqueous color paste according to claim 2, is characterized in that: pH value regulator used comprises at least one in sodium hydroxide, potassium hydroxide, ammoniacal liquor, triethylamine and trolamine.
7. aqueous color paste according to claim 2, is characterized in that: in described aqueous color paste, also comprise antimildew disinfectant; Described antimildew disinfectant is selected from least one in BIT, 5-chloro-2-methyl-1-isothiazoline-3-ketone.
8. the preparation method of the painted pigment dyestuff aqueous color paste of the synthetic leather described in any one of claim 2-7, is characterized in that comprising the steps:
A) all the other deionized waters and wetting agent, dispersion agent, wetting Agent for Printing Inks are disperseed by the 10-20% of reserved deionized water total mass in dispersion machine, add pH value regulator subsequently and regulate the pH value of mixed solution between 8-9, obtain premix;
B) pigment dyestuff of described modification is added in the premix that step a) obtains and disperse, use dispersion machine to be not less than 30 minutes higher than the Rate Dispersion of 200 revs/min, and in dispersion process, add deionized water reserved in step a), obtain pre-mixing pigment slurry;
C) by step b) the pre-mixing pigment slurry that obtains grinds in horizontal mill, and the median size being ground to granules of pigments is less than 0.5 μm, then adds antimildew disinfectant and mix, and after filtration, deaeration, obtains described aqueous color paste.
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| CN105153400B (en) * | 2015-06-30 | 2017-08-04 | 晋江市池店镇娇鹏贸易有限公司 | Outdoor shoe bottom microporous polyurethane elastomer |
| CN104962136B (en) * | 2015-07-03 | 2017-08-11 | 苏州世名科技股份有限公司 | A kind of aqueous carbon black pigment mill base coloured for synthetic leather |
| CN105038414B (en) * | 2015-08-24 | 2018-01-23 | 苏州世名科技股份有限公司 | Organic pigment aqueous color paste for paint toning machine toning and preparation method thereof |
| CN108285710B (en) * | 2018-02-09 | 2020-05-01 | 上海马利画材销售有限公司 | Pigment composition and preparation method and application thereof |
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|---|---|---|---|---|
| JPS61136555A (en) * | 1984-12-07 | 1986-06-24 | Ajinomoto Co Inc | Surface modifier for organic pigment |
| CN102504622A (en) * | 2011-11-04 | 2012-06-20 | 湖北鼎龙化学股份有限公司 | Modified pigment and preparation method and application thereof and nanometer pigment dispersoid |
| CN103709834A (en) * | 2013-12-20 | 2014-04-09 | 苏州世名科技股份有限公司 | Phthalocyanine pigment water-based color paste for coloring synthetic leather and preparation method thereof |
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2014
- 2014-07-03 CN CN201410315143.1A patent/CN104031478B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61136555A (en) * | 1984-12-07 | 1986-06-24 | Ajinomoto Co Inc | Surface modifier for organic pigment |
| CN102504622A (en) * | 2011-11-04 | 2012-06-20 | 湖北鼎龙化学股份有限公司 | Modified pigment and preparation method and application thereof and nanometer pigment dispersoid |
| CN103709834A (en) * | 2013-12-20 | 2014-04-09 | 苏州世名科技股份有限公司 | Phthalocyanine pigment water-based color paste for coloring synthetic leather and preparation method thereof |
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Effective date of registration: 20170210 Address after: 215500 Haining Road, Changshu new material industrial park, Jiangsu, China, No. 12, No. Patentee after: Changshu Famous Chemical Technology Co., Ltd. Address before: 215337 Kunshan Province, Suzhou City, Zhou Town, Huangpu Road, No. 219, North Road, No. Patentee before: Suzhou Shiming Technology Co., Ltd. |