CN109456615B - Printing paste and preparation method and application thereof - Google Patents
Printing paste and preparation method and application thereof Download PDFInfo
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- CN109456615B CN109456615B CN201811191713.5A CN201811191713A CN109456615B CN 109456615 B CN109456615 B CN 109456615B CN 201811191713 A CN201811191713 A CN 201811191713A CN 109456615 B CN109456615 B CN 109456615B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
- C09B67/0046—Mixtures of two or more azo dyes
- C09B67/0051—Mixtures of two or more azo dyes mixture of two or more monoazo dyes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/008—Preparations of disperse dyes or solvent dyes
- C09B67/0082—Preparations of disperse dyes or solvent dyes in liquid form
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
- D06P1/18—Azo dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
- D06P1/5257—(Meth)acrylic acid
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
- D06P1/5292—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds containing Si-atoms
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/60—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
- D06P1/607—Nitrogen-containing polyethers or their quaternary derivatives
- D06P1/6076—Nitrogen-containing polyethers or their quaternary derivatives addition products of amines and alkylene oxides or oxiranes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention discloses a printing paste and a preparation method and application thereof, wherein the printing paste is prepared by mixing a black liquid disperse dye with high color fastness and low lightness, a thickening agent and an anti-migration agent; and in the presence of the printing color paste, the fabric is subjected to screen printing, drying, high-temperature baking, hot water washing and drying to finish the fabric printing. The liquid disperse dye is prepared by mixing a crude dye of a black dye compound, an anionic surfactant, a nonionic surfactant, a polyacrylate copolymer, amino silicone oil, benzisothiazolinone and water and grinding. The prepared black liquid disperse dye with high color fastness and low lightness can improve the color depth of the printed fabric, reduce the flooding of the dye and improve the color fastness of a dyed product; the dyeing product with same brightness can save the effective amount of dye, remarkably reduce the tasks of reduction cleaning and water washing after printing, save water resources and energy consumption and reduce the cost of wastewater treatment.
Description
The invention belongs to a black liquid disperse dye with high color fastness and low lightness, a preparation method thereof, a divisional application of patent applications with application numbers of 2017104057144 and application dates of 2017, 6 and 1, and belongs to the technical part of printing paste.
Technical Field
The invention relates to the technical field of textile printing and dyeing, in particular to a printing paste, a preparation method and application thereof, which are used for improving the color depth of black disperse dye and reducing the discharge of printing and dyeing wastewater.
Background
The polyester fiber is the synthetic fiber with the largest output, and the dyeing and printing of the textile mostly adopt disperse dyes, wherein the consumption of blue-black disperse dyes is the largest.
Most of blue-black disperse dyes are mixtures based on three primary colors dye components, and mainly relate to the purposes of improving the utilization rate of the dyes, improving the color fastness of dyed fabrics, expanding the adaptability of dye application and the like. In order to improve the grindability of the disperse dye, the mass percentage of the dispersant in the original dye is higher (more than 40%), and the dispersant mostly adopts methylene bis (methylnaphthalene) sulfonate, methylene dinaphthalene sulfonate and the like. However, the existence of a large amount of dispersant in the dye can obviously reduce the combination of the dye and the fiber, so that the flooding of the dye on the surface of the fiber is increased, and the times of subsequent reduction cleaning or soaping are required to be increased to remove the flooding of the dye, so that the utilization rate of the dye is low, and particularly the consumption of water is high.
With the increasing requirements of the printing and dyeing industry on energy conservation and emission reduction, the existing black disperse dyes have problems in use, such as heavier reduction cleaning task of polyester printed products of the disperse dyes, large water consumption and deep wastewater chromaticity; if the color fastness of the black polyester printed product is poor, the times of reduction cleaning or soaping need to be enhanced, and the better color fastness can be obtained by removing the dye flooding on the surface of the fiber, but the color depth becomes clear; for a long time, black products with low lightness (high color depth) are poor in color fastness, and the polyester printed products with low lightness and high color fastness are difficult to prepare at the same time. In addition, the printing and dyeing industry still has the problems of high wastewater discharge, high pollution, high water consumption and the like.
Disclosure of Invention
The invention aims to solve the defects of the existing black disperse dye and provide a black liquid disperse dye with high dye utilization rate, high color depth, low wastewater discharge, high color fastness and low lightness and a preparation method thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a black liquid disperse dye with high color fastness and low lightness comprises the following components in percentage by mass:
10-40% of the crude dye compound
2-4% of anionic surfactant
0.5 to 1 percent of nonionic surfactant
3-8% of polyacrylic acid copolymer
0.5-1% of amino silicone oil
0.02-0.05% of benzisothiazolinone
The balance of water.
In the technical scheme, the anionic surfactant is one or more of a formaldehyde condensate of sodium methyl naphthalene sulfonate and fatty amine polyoxyethylene ether sulfate; the nonionic surfactant is fatty amine polyoxyethylene ether.
In the technical scheme, the fatty amine polyoxyethylene ether sulfate is a modified product of fatty amine polyoxyethylene ether and dimethyl sulfate; the fatty amine polyoxyethylene ether has the following structure:
in the formula, R is C16H33Or C18H37And p is 15 to 30.
In the technical scheme, the polyacrylic acid copolymer is prepared by using acrylic acid, acrylonitrile, ethyl acrylate and vinyl pyridine as raw materials, preparing a prepolymer by an emulsion polymerization method, and oxidizing the prepolymer in hydrogen peroxide solution to obtain the polyacrylic acid copolymer; in the emulsion polymerized by the emulsion, the mass fraction of acrylic acid is 6-8%, the mass fraction of acrylonitrile is 4-5%, the mass fraction of ethyl acrylate is 2-3%, and the mass fraction of vinyl pyridine is 15-20%.
The invention also discloses a preparation method of the black liquid disperse dye with high color fastness and low lightness, which comprises the following steps:
(1) acrylic acid, acrylonitrile, ethyl acrylate and vinylpyridine nitrogen are subjected to emulsion polymerization and oxidation reaction to prepare a polyacrylic acid copolymer;
(2) mixing the original dye compound, an anionic surfactant, a nonionic surfactant, a polyacrylic acid copolymer, benzisothiazolinone and water, and grinding for 6-8 hours to prepare the black liquid disperse dye with high color fastness and low lightness.
The preparation method of the polyacrylic copolymer comprises the following steps:
1) mixing acrylic acid, acrylonitrile, ethyl acrylate and vinyl pyridine nitrogen with water in the presence of an emulsifier, and fully stirring to form emulsion; in the emulsion, the mass fraction of acrylic acid is 6-8%, the mass fraction of acrylonitrile is 4-5%, the mass fraction of ethyl acrylate is 2-3%, and the mass fraction of vinyl pyridine is 15-20%;
2) taking 1/2-1/3 of the emulsion, heating to 80 ℃ in the presence of ammonium persulfate, reacting for 10min, adding the rest of the emulsion within 60min, and reacting for 1h at 85 ℃ to obtain a prepolymer;
3) at 85 ℃, hydrogen peroxide and ferrous sulfate are added into the prepolymer to react for 2 hours, thus obtaining the polyacrylic copolymer.
The polyacrylic acid copolymer of the present invention has the following chemical structure:
in the technical scheme, the crude dye compound consists of red crude dye, orange crude dye and blue dye or consists of orange crude dye, purple crude dye and blue crude dye; the red dye is a compound shown as A1; the orange dye is a compound shown as A2, a compound shown as B1 or a compound shown as C1; the purple dye is a compound shown as B2 or a compound shown as C2; the blue dye is a compound shown as A3, a compound shown as A4, a compound shown as B3 or a compound shown as C3;
preferably, the crude dye complex consists of a compound represented by A1, a compound represented by A2, a compound represented by A3 and a compound represented by A4; or the crude dye complex is a compound represented by B1, a compound represented by B2, or a compound represented by B3; or the original dye complex consists of a compound shown as C1, a compound shown as C2 and a compound shown as C3.
The invention also discloses a textile printing method, which comprises the following steps:
(1) mixing the black liquid disperse dye with high color fastness and low lightness, a thickening agent and an anti-migration agent to obtain printing paste;
(2) and in the presence of the printing color paste, printing the fabric by using a screen, drying, baking at a high temperature, reducing, cleaning and drying to finish the printing of the fabric.
The invention also discloses a printed fabric, and the preparation method of the printed fabric comprises the following steps:
(1) mixing the black liquid disperse dye with high color fastness and low lightness, a thickening agent and an anti-migration agent according to claim 1 to obtain printing paste;
(2) and in the presence of the printing color paste, the fabric is subjected to screen printing, drying, high-temperature baking, hot water washing and drying to obtain the printed fabric.
The grinding aid agent is a mixture of an anionic surfactant and a nonionic surfactant, and can obtain the same grinding effect as that of singly adopting methylene bis (methylnaphthalene) sulfonate, methylene dinaphthalene sulfonate and the like. Under the same condition, the grinding efficiency of the grinding aid consisting of the mixture of the anionic surfactant and the nonionic surfactant is higher than that of the grinding aids such as methylene bis (methylnaphthalene) sulfonate, methylene bis (naphthalene) sulfonate and the like which are used independently, and the dosage of the grinding aid consisting of the mixture can be obviously reduced. In a test of grinding the disperse dyes, the fact that a special polyacrylic copolymer is added into a mixture based on black disperse dyes is surprisingly found, the utilization rate of the dyes can be obviously improved, the color fastness of polyester printed products is improved, high color depth or low color brightness is obtained by combining amino silicone oil, and the preparation method is a preparation technology of high-quality liquid disperse dyes.
The invention also discloses a coloring composition, which comprises the black liquid disperse dye with high color fastness and low lightness, a thickening agent and an anti-migration agent; and the application of the coloring composition in printing of polyester fabrics or polyester spandex fabrics. In the invention, the black liquid disperse dye with high color fastness and low lightness, the thickening agent and the anti-migration agent are mixed to obtain the printing paste.
Due to the application of the technical scheme, compared with the existing commercially available black disperse dye, the black disperse dye has the following advantages:
1) the black disperse dye has high color fastness, soaping color fastness is 4-5 grade, and wet rubbing color fastness is 4-5 grade; the color fastness of the existing black disperse dye is low, the soaping color fastness is level 4, and the wet rubbing color fastness is level 4.
2) The black disperse dye has higher color depth and lower color brightness value with the same dye consumption, and the same color depth of dyed fabrics or printed fabrics can reduce the consumption of the black dye.
3) The black disperse dye based on the invention has high dye utilization rate, little dye flooding of the polyester printed product, improved soaping color fastness and wet rubbing color fastness, and obviously reduced post-treatment task of the polyester printed product; the post-treatment wastewater is less and has the advantage of low chromaticity, and the cost of wastewater treatment is reduced.
4) The black liquid disperse dye with high color fastness and low lightness disclosed by the invention improves the color fastness of the polyester printed product, the color fastness to soaping reaches 4-5 grades, and the color fastness to rubbing (dry state and wet state) reaches 4-5 grades; and the treated fabric has soft hand feeling.
Drawings
FIG. 1 is a K/S value graph of a partially printed fabric.
Detailed Description
The invention is further described below with reference to the examples, in which synthetic thickener PTF-3, synthetic thickener PTF-S and anti-migration agent MP are all commercially available products.
Example 1
1) Mixing 8.0g of acrylic acid, 4.0g of acrylonitrile, 2.0g of ethyl acrylate, 16.0g of vinyl pyridine, a proper amount of emulsifier (1.0 g of fatty alcohol (C12-18) polyoxyethylene ether (15) sodium sulfonate, 0.5g of emulsifier SP-80) and 68.5g of water, and fully stirring to obtain emulsion A;
2) 1/3 of the emulsion A in mass is taken, 0.9g of ammonium persulfate is added, the temperature is slowly raised to 80 ℃, the reaction is carried out for 10min at the temperature, then the rest 2/3 emulsion A is slowly added within 60min, and after the dropwise addition is finished, the constant temperature of 85 ℃ is kept for reaction for 1h, so that prepolymer A is prepared;
3) and (3) adding a proper amount of hydrogen peroxide and ferrous sulfate into the prepolymer at a constant temperature of 85 ℃, and continuously reacting for 2 hours to obtain the polyacrylic copolymer A.
Example 2
1) Mixing 6.0g of acrylic acid, 5.0g of acrylonitrile, 3.0g of ethyl acrylate, 19.0g of vinyl pyridine, a proper amount of emulsifier (1.0 g of sodium dodecyl sulfate, 0.5g of emulsifier SP-80) and 65.5 g of water, and fully stirring to obtain emulsion B;
2) 1/3 of the emulsion A in mass is taken, 1.0g of ammonium persulfate is added, the temperature is slowly raised to 80 ℃, the reaction is carried out for 1min at the temperature, then the rest 2/3 emulsion A is slowly added within 60min, and after the dropwise addition is finished, the reaction is carried out for 1h at the constant temperature of 85 ℃ to prepare a prepolymer B;
3) and (3) adding a proper amount of hydrogen peroxide and ferrous sulfate into the prepolymer at a constant temperature of 85 ℃, and continuously reacting for 2 hours to obtain the polyacrylic copolymer B.
Example 3
0.77g of the red dye of the formula A1, 11.46g of the orange dye of the formula A2, 6.18g of the blue dye of the formula A3, 6.65g of the blue dye of the formula A4, 2.0g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.5g of fatty amine polyoxyethylene ether (EO = 15), 5.0g of polyacrylic copolymer A, 0.5g of aminosilicone, 0.02g of benzisothiazolinone and 66.92g of water are mixed and ground on a zirconia sand mill for 2.5 hours to give the liquid disperse dye AA-1.
Example 4
0.77g of the red dye of the formula A1, 11.46g of the orange dye of the formula A2, 6.18g of the blue dye of the formula A3, 6.65g of the blue dye of the formula A4, 3.0g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.5g of fatty amine polyoxyethylene ether (EO = 20), 8.0g of polyacrylic copolymer A, 0.6g of aminosilicone, 0.05g of benzisothiazolinone and 62.79g of water are mixed and ground on a zirconia sand mill for 3 hours to give the liquid disperse dye AA-2.
Example 5
A liquid disperse dye AA-3 was prepared by mixing 0.77g of the red dye of formula A1, 11.46g of the orange dye of formula A2, 6.18g of the blue dye of formula A3, 6.65g of the blue dye of formula A4, 2.5g of ammonium polyoxyethylene fatty amine sulfate (EO = 15), 1.0g of polyoxyethylene fatty amine ether (EO = 30), 3.0g of polyacrylic copolymer A, 0.7g of aminosilicone, 0.03g of benzisothiazolinone and 67.71g of water, and grinding for 2 hours on a zirconia sand mill.
Example 6
5.08g of the orange dye of the formula B1, 3.59g of the violet dye of the formula B2, 3.83 of the blue dye of the formula B3, 2.0g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.5g of ammonium polyoxyethylene fatty amine sulfate (EO = 20), 0.5g of polyoxyethylene fatty amine ether (EO = 20), 7.50g of the polyacrylic copolymer B, 0.5g of aminosilicone, 0.05g of benzisothiazolinone and 76.45g of water are mixed and ground on a zirconia sand mill for 3 hours to give the liquid disperse dye BB-1.
Example 7
5.08g of an orange dye of the formula B1, 3.59g of a violet dye of the formula B2, 3.83 of a blue dye of the formula B3, 2.0g of a formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.5g of fatty amine polyoxyethylene ether (EO = 15), 5.20g of polyacrylic copolymer B, 0.6g of aminosilicone oil, 0.02g of benzisothiazolinone and 79.18g of water were mixed and ground on a zirconia sand mill for 2.5 hours to prepare a liquid disperse dye BB-2.
Example 8
5.08g of the orange dye of the formula B1, 3.59g of the violet dye of the formula B2, 3.83 of the blue dye of the formula B3, 1.5g of ammonium sulfate fatty amine polyoxyethylene ether (EO = 15), 0.5g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.8g of fatty amine polyoxyethylene ether (EO = 30), 3.0g of the polyacrylic copolymer B, 0.9g of aminosilicone oil, 0.5g of aminosilicone oil, 0.03g of benzisothiazolinone and 80.77g of water were mixed and ground on a zirconia sand mill for 2 hours to obtain the liquid disperse dye BB-3.
Example 9
0.79g of the orange dye of the formula C1, 2.94g of the violet dye of the formula C2, 6.53g of the blue dye of the formula C3, 1.5g of ammonium sulfate fatty amine polyoxyethylene ether (EO = 15), 0.5g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.8g of fatty amine polyoxyethylene ether (EO = 30), 7.0g of polyacrylic copolymer A, 0.8g of aminosilicone oil, 0.03g of benzisothiazolinone and 79.11g of water are mixed and ground on a zirconia sand mill for 2 hours to give the liquid disperse dye CC-1.
Example 10
0.79g of the orange dye of the formula C1, 2.94g of the violet dye of the formula C2, 6.53g of the blue dye of the formula C3, 1.5g of ammonium sulfate fatty amine polyoxyethylene ether (EO = 15), 0.5g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.8g of fatty amine polyoxyethylene ether (EO = 30), 7.0g of the polyacrylic copolymer A, 0.8g of aminosilicone oil and 79.14g of water are mixed and ground on a zirconia sand mill for 2 hours to give the liquid disperse dye CC-2.
Example 11
0.79g of the orange dye of the formula C1, 2.94g of the violet dye of the formula C2, 6.53g of the blue dye of the formula C3, 1.5g of ammonium sulfate fatty amine polyoxyethylene ether (EO = 15), 0.5g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.8g of fatty amine polyoxyethylene ether (EO = 30), 0.8g of aminosilicone oil, 0.03g of benzisothiazolinone and 86.11g of water are mixed and ground on a zirconia sand mill for 2 hours to give the liquid disperse dye CC-3.
Example 12
0.79g of the orange dye of the formula C1, 2.94g of the violet dye of the formula C2, 6.53g of the blue dye of the formula C3, 1.5g of ammonium sulfate fatty amine polyoxyethylene ether (EO = 15), 0.5g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.8g of the fatty amine polyoxyethylene ether (EO = 30), 7.0g of the polyacrylic copolymer A, 0.03g of benzisothiazolinone and 79.91g of water are mixed and ground on a zirconia sand mill for 2 hours to give the liquid disperse dye CC-4.
Comparative example 1
A liquid disperse dye RA-1 was prepared by mixing 0.77g of the red dye of the formula A1, 11.46g of the orange dye of the formula A2, 6.18g of the blue dye of the formula A3, 6.65g of the blue dye of the formula A4, 11.0 g of the formaldehyde condensate of sodium methylnaphthalenesulfonate and 63.94g of water, and grinding for 2 hours on a zirconia sand mill.
Comparative example 2
A liquid disperse dye RA-2 was prepared by mixing 0.77g of the red dye of the formula A1, 11.46g of the orange dye of the formula A2, 6.18g of the blue dye of the formula A3, 6.65g of the blue dye of the formula A4, 20.0 g of the formaldehyde condensate of sodium methylnaphthalenesulfonate and 54.94g of water, and grinding for 2 hours on a zirconia sand mill.
Comparative example 3
A liquid disperse dye RA-3 was prepared by mixing 0.77g of the red dye of the formula A1, 11.46g of the orange dye of the formula A2, 6.18g of the blue dye of the formula A3, 6.65g of the blue dye of the formula A4, 3.0g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.5g of the polyoxyethylene ether of an aliphatic amine (EO = 20), 0.05g of benzisothiazolinone and 71.39g of water and grinding for 3 hours on a zirconia sand mill.
Comparative example 4
5.08g of the orange dye of the formula B1, 3.59g of the violet dye of the formula B2, 3.83g of the blue dye of the formula B3, 14.50g of the formaldehyde condensate of sodium methylnaphthalenesulfonate and 73.00g of water were mixed and ground for 2 hours on a zirconia sand mill to give the liquid disperse dye RB-1.
Comparative example 5
A liquid disperse dye RB-2 was prepared by mixing 5.08g of the orange dye of formula B1, 3.59g of the violet dye of formula B2, 3.83g of the blue dye of formula B3, 2.0g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.5g of the polyoxyethylene ether of an aliphatic amine (EO = 15), 0.02g of benzisothiazolinone, and 84.98g of water, and grinding for 2 hours on a zirconia sand mill.
Comparative example 6
0.79g of the orange dye of the formula C1, 2.94g of the violet dye of the formula C2, 6.53g of the blue dye of the formula C3, 1.5g of ammonium sulfate fatty amine ethoxylate (EO = 15), 0.5g of the formaldehyde condensate of sodium methylnaphthalenesulfonate, 0.8g of fatty amine ethoxylate (EO = 30), 0.03g of benzisothiazolinone and 86.91g of water are mixed and ground on a zirconia sand mill for 2 hours to give the liquid disperse dye RC-1.
And (3) performance testing:
1) printing process flow and process parameters
The process A comprises the following steps: polyester fabric → printing color paste (liquid disperse dye, synthetic thickener PTF-31.0%, synthetic thickener PTF-S1.0%, anti-migration agent MP 0.5%, and water in balance) → screen printing → drying (70 ℃ X2 min) → high temperature baking (180 ℃ X1 min) → hot water washing (50 ℃ X10 min) → drying → finished product.
And a process B: polyester fabric → preparation of printing color paste (liquid disperse dye, synthetic thickener PTF-31.0%, synthetic thickener PTF-S1.0%, anti-migration agent MP 0.5%, and water in balance) → screen printing → drying (70 ℃ X2 min) → high-temperature baking (180 ℃ X1 min) → reduction cleaning (sodium hydroxide 1.0g/L, sodium hydrosulfite 1.0g/L, bath ratio 1: 10, 70 ℃ X10 min) → hot water washing (50 ℃ X10 min, bath ratio 1: 10) → drying → finished product.
4) Color fastness, L × (lightness) and K/S value curves:
color fastness to rubbing: testing according to GB/T3920-;
fastness to soaping: according to GB/T3921-: method 3 testing.
L value: testing L on UltraScanXE computer color testing and matching instrument*The value is obtained. Test conditions were D65Light source, 100At viewing angle, the sample was folded into 4 layers and averaged 10 times.
Difference in L ×: and (4) calculating the difference value of the L values of the process A and the process B, and representing the removal degree of the floating color under the cleaning condition.
K/S value curve: the K/S value curve was tested on an UltraScanXE computer color tester. Test conditions were D65Light source, 100At viewing angle, the sample was folded into 4 layers, and the degree of the shade was represented by taking the average of 10 times.
The same amount of liquid disperse dyes, black dyes consisting of red dye with a structural formula A1, orange dye with a structural formula A2, blue dye with a structural formula A3 and blue dye with a structural formula A4 are adopted, the L (brightness) test results of a printing process A and a printing process B are shown in a table 1, and the color fastness test results are shown in a table 2; the K/S value curves of the printed fabrics of some of the examples and comparative examples using printing process A are shown in FIG. 1.
The results of L (lightness) tests on the liquid disperse dyes, namely the black dyes consisting of the orange dye with the structural formula B1, the purple dye with the structural formula B2 and the blue dye with the structural formula B3, by the printing process A and the printing process B are shown in Table 3, and the results of the color fastness tests are shown in Table 4.
The results of L (lightness) and color fastness tests using the printing process A are shown in Table 5, using the same amount of liquid disperse dyes, black dyes consisting of orange dye of formula C1, violet dye of formula C2 and blue dye of formula C3.
As is clear from tables 1 and 2, in examples 3 to 5, the difference in L is small and the soaping fastness and the dry/wet rubbing fastness are on the order of 4 to 5 regardless of whether the process A or the process B is used. This shows that good color fastness is achieved when examples 3 to 5 employ process A, without the need to employ reduction washing to improve the color fastness. Comparative examples 1 to 3, the L value prepared by the process a is low, the color is dark, but the soaping color fastness and the dry/wet rubbing color fastness are poor; the L value prepared by the process B is higher, the color is lighter, the soaping color fastness and the dry/wet rubbing color fastness are better, and the wet rubbing color fastness is still poorer. Examples 3 to 5 had lower L values than comparative examples 1 to 3 and had better soaping fastness and dry/wet rubbing fastness. Comparing comparative examples 1 to 3, the anionic surfactant content in comparative example 2 was the highest, and L was the highest; while comparative example 3 had the lowest level of anionic and nonionic surfactant and had the lowest L value. This visual observation of the shades of color is shown in FIG. 1, with example 4 having the highest K/S value (lowest L value, darkest color) and comparative example 2 having the lowest K/S value (highest L value, lightest color).
As is clear from tables 3 and 4, in examples 6 to 8, the difference in L is small and both the soaping fastness and the dry/wet rubbing fastness achieved 4 to 5 levels by using the process A or the process B. The printed fabrics of examples 6 to 8 were darker in color and had lower L values. Compared with the comparative examples 4 and 5, the prepared product by the process A has lower L value, darker color and poorer color fastness; the prepared product by the process B has large L value, light color and good color fastness; comparative examples 4 and 5, whether process a or process B was used, were inferior in color depth and color fastness to examples 6-8.
As is clear from Table 4, the L value, soaping fastness and dry/wet rubbing fastness of comparative example 9 and example 10 were almost the same, indicating that the dyes of the present invention are excellent in stability of printing performance on fabrics.
Comparing example 11 with example 12, example 11 has a higher L value and a smaller decrease in lightness value, whereas example 12 has a lower L value and a darker color; however, the color depth was less than that of example 9 or example 10, which indicates that when the polyacrylic copolymer and the amino silicone oil were used together, the L value was more decreased.
The technology of the invention can not only obtain deeper color depth, but also obtain excellent color fastness by adopting weak and light cleaning conditions, thus being capable of cleaning the consumption of water, saving energy and auxiliary agent and greatly reducing the burden of wastewater treatment.
Table 1L (lightness) test results
TABLE 2 color fastness test results
Table 3L (lightness) test results
TABLE 4 color fastness test results
TABLE 5L (lightness) test results (Process A)
Claims (3)
1. A printing paste is characterized in that a black liquid disperse dye with high color fastness and low lightness, a thickening agent and an anti-migration agent are mixed to obtain the printing paste; the black liquid disperse dye with high color fastness and low lightness comprises the following components in percentage by mass:
10-40% of the crude dye compound
2-4% of anionic surfactant
0.5 to 1 percent of nonionic surfactant
3-8% of polyacrylic acid copolymer
0.5-1% of amino silicone oil
0.02-0.05% of benzisothiazolinone
The balance of water;
the anionic surfactant is one or more of a formaldehyde condensate of sodium methyl naphthalene sulfonate and fatty amine polyoxyethylene ether sulfate; the nonionic surfactant is fatty amine polyoxyethylene ether; the fatty amine polyoxyethylene ether sulfate is a modified product of fatty amine polyoxyethylene ether and dimethyl sulfate; the fatty amine polyoxyethylene ether has the following chemical structure:
in the formula, R is C16H33Or C18H37P is 15-30;
the polyacrylic acid copolymer is prepared by using acrylic acid, acrylonitrile, ethyl acrylate and vinyl pyridine as raw materials, preparing a prepolymer by adopting an emulsion polymerization method, and oxidizing the prepolymer in a hydrogen peroxide solution; in the emulsion polymerized by the emulsion, the mass fraction of acrylic acid is 6-8%, the mass fraction of acrylonitrile is 4-5%, the mass fraction of ethyl acrylate is 2-3%, and the mass fraction of vinyl pyridine is 15-20%;
the crude dye compound consists of red crude dye, orange crude dye and blue dye or consists of orange crude dye, purple crude dye and blue crude dye; the red dye is a compound shown as A1; the orange dye is a compound shown as A2, a compound shown as B1 or a compound shown as C1; the purple dye is a compound shown as B2 or a compound shown as C2; the blue dye is a compound shown as A3, a compound shown as A4, a compound shown as B3 or a compound shown as C3;
2. the printing paste according to claim 1, wherein the printing paste is prepared by mixing a black liquid disperse dye having high color fastness and low lightness, a thickener, and an anti-migration agent.
3. The use of the printing paste according to claim 1 for printing on polyester or polyester spandex fabrics.
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