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CN111138886B - A kind of liquid disperse dye and its preparation method and application - Google Patents

A kind of liquid disperse dye and its preparation method and application Download PDF

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Publication number
CN111138886B
CN111138886B CN201911365167.7A CN201911365167A CN111138886B CN 111138886 B CN111138886 B CN 111138886B CN 201911365167 A CN201911365167 A CN 201911365167A CN 111138886 B CN111138886 B CN 111138886B
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China
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grinding
disperse dye
disperse
dye
printing
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CN111138886A (en
Inventor
蔡再生
李云峰
范追追
王梦婷
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Zhejiang Kefeng Silicone Co ltd
Donghua University
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Zhejiang Kefeng Silicone Co ltd
Donghua University
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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
    • C09B67/0001—Post-treatment of organic pigments or dyes
    • C09B67/0002—Grinding; Milling with solid grinding or milling assistants
    • 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
    • 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
    • D06P1/46—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 natural macromolecular substances or derivatives thereof
    • 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
    • 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
    • D06P1/613—Polyethers without nitrogen
    • D06P1/6131—Addition products of hydroxyl groups-containing compounds with oxiranes
    • D06P1/6133—Addition products of hydroxyl groups-containing compounds with oxiranes from araliphatic or aliphatic alcohols
    • 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
    • D06P1/64—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 low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651—Compounds without nitrogen
    • D06P1/65106—Oxygen-containing compounds
    • D06P1/65118—Compounds containing hydroxyl groups
    • 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
    • D06P1/673—Inorganic compounds
    • D06P1/67383—Inorganic compounds containing silicon
    • 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)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Coloring (AREA)

Abstract

本发明涉及一种液体分散染料及其制备方法和应用。该方法包括：将研磨助剂与去离子水混合，使研磨助剂充分溶胀，加入分散染料、乙二醇和分散剂进行研磨；再加入分散剂继续研磨，过滤。该方法操作简单，制备得到的液体分散染料分散性和稳定性均很好。The present invention relates to a liquid disperse dye and its preparation method and application. The method includes: mixing a grinding aid with deionized water to fully swell the grinding aid, adding disperse dye, ethylene glycol and a dispersant for grinding; adding a dispersant to continue grinding and filtering. The method is simple to operate, and the prepared liquid disperse dyes have good dispersibility and stability.

Description

Liquid disperse dye and preparation method and application thereof
Technical Field
The invention belongs to the field of disperse dyes and preparation and application thereof, and particularly relates to a liquid disperse dye and a preparation method and application thereof.
Background
The disperse dye is the main colorant for dyeing and printing the polyester fabric. Because the disperse dye is insoluble in water, a uniform dispersion can be formed in water by the action of a dispersant. The water solubility of the disperse dye is very low, and the disperse dye is mainly in a micro particle dispersion state during dyeing. The dyeing mechanism of the dye is completely different from that of a water-soluble dye, no chemical bond reaction exists between the dye and the fiber, the fiber expands under the high-temperature condition and enters the fiber in a pore channel deposition mode, and the attraction and hydrogen bond fixation generated between molecules are utilized to finish the dyeing process. The dyeing methods adopted at present mainly comprise a carrier method, a high-temperature high-pressure method and a hot melting method. After the traditional disperse dye is used for dyeing, dyeing residual liquid contains a small amount of undyed dye, the undyed dye is easily adsorbed on the surface of polyester fiber to form loose color, the loose color cannot be removed by simple washing, and liquid alkali, sodium hydrosulfite, an acid reduction cleaning agent and the like are added to achieve the purpose of improving the color fastness.
Compared with the powdery disperse dye, the liquid disperse dye has a plurality of incomparable advantages: firstly, the liquid disperse dye can achieve good dispersion effect by using less dispersant, thereby saving the cost and improving the utilization rate of the dye; the spray drying process is omitted, the process is simplified, and energy is saved; the automatic material taking is convenient, and the automatic development trend of the printing and dyeing industry is met; fourthly, dust pollution and the like are eliminated from the source, which makes the disperse dye as a commercial preparation form of the disperse dye gradually receive attention in recent years. Although liquid disperse dyes have many advantages, the liquid disperse dyes also have obvious defects, such as poor storage stability, easy precipitation, upper and lower layering, and uneven dye concentration of the upper and lower layers; the dye particles are easy to generate secondary agglomeration after being stored for a long time, so that the particle size is increased, and the performance of the dye is influenced. This fatal disadvantage of the liquid disperse dye seriously affects the popularization and use thereof, so that the production and application of the liquid disperse dye are not popularized.
There are many methods for producing an ultra-fine liquid disperse dye, and the method can be roughly classified into a chemical processing method and a physical processing method. Wherein the chemical processing method comprises emulsion polymerization, solvent method, etc.; the physical processing method comprises high-pressure homogenization, ultrasonic preparation, and mechanical grinding. Different from a chemical processing method which needs to use a large amount of organic solvent, the physical processing method takes water as a medium, the process operation is simple and efficient, the technology is more mature, and the method is a processing mode which is widely used at present. Although the chemical method for preparing nano-powder has been studied in great numbers, the production cost is relatively high and the particle size distribution is wide. So, the industry is mainly using the physical mechanical grinding method to prepare the nanometer powder. The physical mechanical method is easy to prepare the nano powder with narrower particle size distribution, and meanwhile, the production cost is relatively low, the parameters are easy to control, and the batch production can be realized. Chinese patent CN110330810A prepares a superfine nano liquid dispersion color paste by a grinding method, wherein, a disperse dye is firstly dissolved by an organic solvent, then is added into a grinding system containing a hyper-dispersant, a wetting agent and water, the organic solvent is recovered, and then a stabilizer, a solvent and a bactericide are added for continuous grinding.
Disclosure of Invention
The invention aims to solve the technical problem of providing a liquid disperse dye, a preparation method and application thereof, so as to overcome the defects of poor dispersibility and stability of the liquid disperse dye in the prior art.
The invention provides a preparation method of a liquid disperse dye, which comprises the following steps:
(1) mixing 0.2-5% of grinding aid with deionized water to fully swell the grinding aid, adding disperse dye, 5-10% of glycol and 5-15% of dispersing agent for grinding, wherein the mass ratio of the deionized water to the disperse dye is 60-90: 30-50 parts of;
(2) adding 0.2-0.6% of dispersing agent into the system ground in the step (1), continuing grinding, and filtering to obtain liquid disperse dye;
the percentage in the steps (1) and (2) is mass percentage, and the total mass of the deionized water and the disperse dye is taken as reference.
The grinding aid in the step (1) is at least one of silicon dioxide, titanium dioxide, aluminum oxide and bentonite.
The disperse dye in the step (1) is at least one of disperse blue 79, disperse orange 30 and disperse red 54.
The dispersing agent in the step (1) is an anionic dispersing agent and a nonionic dispersing agent in a mass ratio of 1:1-3: 1.
The anionic dispersant is at least one of sodium lignosulfonate, sodium cellulose sulfonate, a sodium methyl naphthalene sulfonate formaldehyde condensate and a benzyl naphthalene sulfonate formaldehyde condensate.
The nonionic dispersing agent is at least one of alkylphenol polyoxyethylene, fatty alcohol polyoxyethylene and fatty acid polyol ester polyoxyethylene.
The grinding process parameters in the step (1) are as follows: the rotating speed is 400-600r/min, the diameter is 1mm, the ball-material ratio is 8-12:1, grinding for 1-3 h.
And (2) grinding in the step (1) adopts a ball mill.
The dispersing agent in the step (2) is at least one of sodium polyacrylate, styrene-methacrylic acid copolymer and styrene-maleic anhydride copolymer.
The process parameters of the continuous grinding in the step (2) are as follows: the rotating speed is 400-600r/min, the ball-material ratio is 8-12:1, and the grinding time is 9-11 h.
In the step (2), a double-layer 200-mesh screen is adopted for filtering.
The invention also provides the liquid disperse dye prepared by the method.
The invention also provides application of the liquid disperse dye prepared by the method in printing.
The printing process comprises the following steps: preparing printing paste from 0.5-2.5% of liquid disperse dye, 1-5.0% of adhesive, 0.5-2.5% of thickening agent and the balance of water, printing, drying and baking, wherein the percentage is mass percentage and is based on the total mass of the liquid disperse dye, the adhesive, the thickening agent and the water.
The adhesive is RUCO-COAT FX 8011.
The thickening agent is TH 5000.
The drying temperature is 80-100 ℃, and the drying time is 5-10 min.
The baking temperature is 170-190 ℃, and the baking time is 60-120 s.
The performance tests involved in the present invention are as follows:
testing the particle size: after a small amount of liquid ultra-fine disperse dye is diluted, the particle size of the dye in a disperse system is measured at 25 ℃ by a Nano-ZS90 type nanometer particle size analyzer.
Testing stability: the prepared liquid disperse dye was stored at rest (20 ℃ C.) for 60 days, and it was observed whether or not a precipitate was generated.
Advantageous effects
The preparation method is simple to operate, the prepared liquid disperse dye is good in dispersity and stability, and the particle size of the liquid disperse dye is about 100 nm; no precipitate is generated after standing and storing for more than 60 days. When the prepared liquid disperse dye is used for preparing color paste for printing polyester fabrics, the color paste does not need to be reduced and cleaned after being printed, dried and baked at high temperature, so that the consumption of water resources can be reduced, the discharge amount of waste water is reduced, and the color paste has practical significance for environmental protection.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The main reagents are as follows:
the bentonite is purchased from enemy Shanfeng soil Co., Ltd in Hangzhou, and the disperse dye is purchased from Wanfeng chemical Co., Ltd in Zhejiang; the dispersing agent sodium lignosulfonate and fatty alcohol-polyoxyethylene ether are purchased from Jiangsu Yabang dye Co., Ltd; ethylene glycol was purchased from shanghai Lingfeng Chemicals, Inc.; polyacrylate was purchased from bosa chemical ltd, jiang; the adhesive RUCO-COAT FX 8011 and the thickener TH5000 are from Quanzhou Haitian materials science and technology, Inc.
The addition of the grinding aid can reduce the particle size of the dye; in the application, the two dispersing agents are added separately for grinding, and the uniform stability of the particles can be improved by adding the dispersing agent twice.
Example 1
The first step is as follows: and (3) preparing a liquid disperse dye.
0.2 percent of grinding aid bentonite is added into deionized water and mixed evenly to ensure that the bentonite is fully swelled. Then adding disperse dye disperse red 54 (the mass ratio of the disperse red 54 to the deionized water is 30:90), 5% of glycol and 5% of dispersing agent (the mass ratio of sodium lignosulfonate to fatty alcohol-polyoxyethylene ether is 2: 1), grinding glass beads with the rotation speed of 500r/min and the diameter of 1mm by using a ball mill for 2 hours, then continuously adding 0.2% of dispersing agent polyacrylate, and continuously grinding for 10 hours. And finally filtering the mixture by using a double-layer 200-mesh screen to obtain filtrate, and storing the filtrate for later use. Wherein, the percentage is mass percentage, and is based on the total mass of the disperse red 54 and the deionized water.
The second step is that: a water-washing-free printing process.
Mixing and stirring 0.5% of the prepared liquid disperse dye, 0.5% of an adhesive RUCO-COAT FX 80111%, a thickening agent TH 50000.5% and the balance of water uniformly to prepare a printing paste, and printing by using the following process: printing paste preparation → printing (400m/h) → drying (80 ℃, 10min) → baking (170 ℃, 120 s). Wherein, the percentage is mass percentage and is based on the total mass of the system.
Example 2
Adding 2% of grinding aid bentonite into deionized water, and uniformly mixing to fully swell. Then adding disperse dye disperse red 54 (the mass ratio of the disperse red 54 to the deionized water is 30:90), 8% of glycol and 10% of dispersing agent (the mass ratio of sodium lignosulfonate to fatty alcohol-polyoxyethylene ether is 2: 1), grinding glass beads with the rotation speed of 500r/min and the diameter of 1mm by using a ball mill for 2 hours, then continuously adding 0.4% of polyacrylate, and continuously grinding for 10 hours. And finally filtering the mixture by using a double-layer 200-mesh screen to obtain filtrate, and storing the filtrate for later use. Wherein, the percentage is mass percentage, and is based on the total mass of the disperse red 54 and the deionized water.
The second step is that: a water-washing-free printing process.
Mixing and stirring 0.5% of the prepared liquid disperse dye, 0.5% of an adhesive RUCO-COAT FX 80111%, a thickening agent TH 50000.5% and the balance of water uniformly to prepare a printing paste, and printing by using the following process: printing paste preparation → printing (400m/h) → drying (90 ℃, 7min) → baking (180 ℃, 90 s). Wherein, the percentage is mass percentage and is based on the total mass of the system.
Example 3
The first step is as follows: and (3) preparing a liquid disperse dye.
Adding 5% of bentonite into deionized water, and uniformly mixing to fully swell. Then adding disperse dye disperse red 54 (the mass ratio of the disperse red 54 to the deionized water is 30:90), 10% of glycol and 15% of dispersing agent (the mass ratio of sodium lignosulfonate to fatty alcohol-polyoxyethylene ether is 2: 1), grinding glass beads with the rotation speed of 500r/min and the diameter of 1mm by using a ball mill for 2 hours, then continuously adding 0.6% of polyacrylate, and continuously grinding for 10 hours. And finally filtering the mixture by using a double-layer 200-mesh screen to obtain filtrate, and storing the filtrate for later use. Wherein, the percentage is mass percentage, and is based on the total mass of the disperse red 54 and the deionized water.
The second step is that: a water-washing-free printing process.
Mixing and stirring 0.5% of the prepared liquid disperse dye, 0.5% of an adhesive RUCO-COAT FX 80111%, a thickening agent TH 50000.5% and the balance of water uniformly to prepare a printing paste, and printing by using the following process: printing paste preparation → printing (400m/h) → drying (100 ℃, 5min) → baking (210 ℃, 60 s). Wherein, the percentage is mass percentage and is based on the total mass of the system.
Example 4
The first step is as follows: and (3) preparing a liquid disperse dye.
Adding 5% of bentonite into deionized water, and uniformly mixing to fully swell. Then adding disperse dye disperse red 54 (the mass ratio of the disperse red 54 to the deionized water is 45:80), 10% of glycol and 15% of dispersing agent (a mixture of sodium lignosulfonate and fatty alcohol-polyoxyethylene ether in a mass ratio of 2: 1), grinding glass beads with the rotation speed of 500r/min and the diameter of 1mm by using a ball mill for 2 hours, then continuously adding 0.6% of polyacrylate, and continuously grinding for 10 hours. And finally filtering the mixture by using a double-layer 200-mesh screen to obtain filtrate, and storing the filtrate for later use. Wherein, the percentage is mass percentage, and is based on the total mass of the disperse red 54 and the deionized water.
The second step is that: a water-washing-free printing process.
Mixing and stirring 1.5% of the prepared liquid disperse dye, 1.5% of an adhesive RUCO-COAT FX 80113%, a thickening agent TH 50001.5% and the balance of water uniformly to prepare a printing paste, and printing by using the following process: printing paste preparation → printing (400m/h) → drying (90 ℃, 7min) → baking (180 ℃, 90 s). Wherein, the percentage is mass percentage and is based on the total mass of the system.
Example 5
The first step is as follows: and (3) preparing a liquid disperse dye.
Dissolving disperse dye disperse red 54 in deionized water (the mass ratio of the disperse red 54 to the deionized water is 30:90), adding 10% of ethylene glycol and 15% of dispersing agent (a mixture of sodium lignosulfonate and fatty alcohol-polyoxyethylene ether in a mass ratio of 2: 1), grinding glass grinding beads with the rotation speed of 500r/min and the diameter of 1mm by using a ball mill for 2 hours, then continuously adding 0.6% of polyacrylate, and continuously grinding for 10 hours. And finally filtering the mixture by using a double-layer 200-mesh screen to obtain filtrate, and storing the filtrate for later use. Wherein, the percentage is mass percentage, and is based on the total mass of the disperse red 54 and the deionized water.
The second step is that: a water-washing-free printing process.
Mixing and stirring 1.5% of the prepared liquid disperse dye, 1.5% of an adhesive RUCO-COAT FX 80113%, a thickening agent TH 50001.5% and the balance of water uniformly to prepare a printing paste, and printing by using the following process: printing paste preparation → printing (400m/h) → drying (90 ℃, 7min) → baking (180 ℃, 90 s). Wherein, the percentage is mass percentage and is based on the total mass of the system.
Example 6
The first step is as follows: and (3) preparing a liquid disperse dye.
Adding 5% of bentonite into deionized water, and uniformly mixing to fully swell. Then adding disperse dye disperse red 54 (the mass ratio of the disperse red 54 to the deionized water is 30:90), 10% of glycol and 15% of dispersing agent (the mass ratio of sodium lignosulfonate to fatty alcohol-polyoxyethylene ether is 2: 1), grinding glass beads with the diameter of 1mm at the rotating speed of 500r/min, and grinding for 12h by using a ball mill. And finally filtering the mixture by using a double-layer 200-mesh screen to obtain filtrate, and storing the filtrate for later use. Wherein, the percentage is mass percentage, and is based on the total mass of the disperse red 54 and the deionized water.
The second step is that: a water-washing-free printing process.
Mixing and stirring 1.5% of the prepared liquid disperse dye, 1.5% of an adhesive RUCO-COAT FX 80113%, a thickening agent TH 50001.5% and the balance of water uniformly to prepare a printing paste, and printing by using the following process: printing paste preparation → printing (400m/h) → drying (90 ℃, 7min) → baking (180 ℃, 90 s). Wherein, the percentage is mass percentage and is based on the total mass of the system.
Example 7
The first step is as follows: and (3) preparing a liquid disperse dye.
Adding 5% of bentonite into deionized water, and uniformly mixing to fully swell. Then adding disperse dye disperse red 54 (the mass ratio of the disperse red 54 to the deionized water is 30:90), 10% of glycol, 15% of dispersing agent (a mixture of sodium lignosulfonate and fatty alcohol-polyoxyethylene ether in a mass ratio of 2: 1) and 0.6% of polyacrylate, grinding the mixture by using glass grinding beads with the rotation speed of 500r/min and the diameter of 1mm, and grinding the mixture by using a ball mill for 12 hours. And finally filtering the mixture by using a double-layer 200-mesh screen to obtain filtrate, and storing the filtrate for later use. Wherein, the percentage is mass percentage, and is based on the total mass of the disperse red 54 and the deionized water.
The second step is that: a water-washing-free printing process.
Mixing and stirring 1.5% of the prepared liquid disperse dye, 1.5% of an adhesive RUCO-COAT FX 80113%, a thickening agent TH 50001.5% and the balance of water uniformly to prepare a printing paste, and printing by using the following process: printing paste preparation → printing (400m/h) → drying (90 ℃, 7min) → baking (180 ℃, 90 s). Wherein, the percentage is mass percentage and is based on the total mass of the system.
Comparative example 1
Weighing 30g of CI.R-54 disperse red dye, and dissolving the CI.R-54 disperse red dye in 100ml of trichloroethylene to prepare a disperse dye solution; weighing 4g of styrene-maleic anhydride polymer and 0.5g of alkylphenol polyoxyethylene ether, dissolving in 100ml of water, adding grinding beads, stirring and mixing at a low speed of 100r/min for 10min, wherein the volume ratio of the grinding beads to the solution is 0.1-5:1, and obtaining a dispersed grinding system; slowly adding the disperse dye solution into a disperse grinding system, grinding and stirring, after the disperse dye solution is completely added, increasing the stirring speed to 2000r/min, heating to 90 ℃, condensing, refluxing and recovering the organic solvent, stirring and grinding for 3 hours, and keeping grinding; then adding 0.5g of thiodiglycol, 5g of diethylene glycol monobutyl ether and 0.05g of isothiazolinone bactericide, and continuing to grind for 30 min; the grinding beads were separated by filtration using a 100 mesh gauze.
The dispersion and stability results of the liquid disperse dyes in examples 1 to 7 and comparative example 1 are shown in table 1:
TABLE 1
Sample (I) Particle size Stability of
Example 1 90.3nm 60 days
Example 2 83.2nm 60 days
Example 3 78.4nm 60 days
Example 4 110.7nm 60 days
Example 5 108.2nm 60 days
Example 6 79.6nm 50 days
Example 7 78.0nm 50 days
Comparative example 1 155.5nm 50 days
As can be seen from Table 1, the particle diameters of the liquid disperse dyes in examples 1 to 7 are smaller than that of comparative example 1, which indicates that the dispersibility of the liquid disperse dyes in examples 1 to 7 is better than that of comparative example 1, wherein the particle diameters of the liquid disperse dyes in examples 1 to 3 decrease with the increase of the auxiliary agent, which indicates that the auxiliary agent plays an important role in the dispersion; the particle size increase in example 4 is probably due to the fact that the increase of the dye causes the dye to have poor flowability in the dispersion system and the collision probability is reduced; in example 5, the particle size was increased due to the absence of the grinding aid; example 6 compared with example 3, the dispersant is not added twice, the influence on the particle size is not great, but the stability is reduced; example 7 compared to example 3, the dispersant was added at one time, and the particle size was slightly reduced, but the stability was reduced. The liquid disperse dyes of examples 1 to 5 were stored at rest (20 ℃ C.) for 60 days, no precipitation occurred, whereas the liquid disperse dyes of examples 6 to 7 and comparative example 1 were significantly precipitated.

Claims (9)

1.一种液体分散染料的制备方法，包括：1. a preparation method of liquid disperse dye, comprising: （1）将0.2-5%研磨助剂与去离子水混合，使研磨助剂充分溶胀，加入分散染料、5-10%乙二醇和5-15%分散剂进行研磨，其中去离子水与分散染料的质量比为60-90：30-50，研磨助剂为二氧化硅、二氧化钛、氧化铝、膨润土中的至少一种；(1) Mix 0.2-5% grinding aid with deionized water to fully swell the grinding aid, add disperse dye, 5-10% ethylene glycol and 5-15% dispersant for grinding, in which deionized water and dispersion The mass ratio of the dye is 60-90:30-50, and the grinding aid is at least one of silica, titania, alumina and bentonite; （2）步骤（1）研磨后的体系中加入0.2%-0.6%分散剂继续研磨，过滤，得到液体分散染料；(2) Step (1) Add 0.2%-0.6% dispersant to the system after grinding and continue to grind and filter to obtain liquid disperse dye; 步骤（1）和（2）中百分数为质量百分数，是以去离子水和分散染料的总质量为基准。The percentages in steps (1) and (2) are mass percentages, based on the total mass of deionized water and disperse dyes. 2.根据权利要求1所述方法，其特征在于，所述步骤（1）中分散染料为分散蓝79、分散橙30、分散红54中的至少一种；分散剂为质量比为1:1-3:1的阴离子分散剂和非离子分散剂。2. The method according to claim 1, wherein in the step (1), the disperse dye is at least one of disperse blue 79, disperse orange 30, and disperse red 54; the dispersant is a mass ratio of 1:1 -3:1 anionic dispersant and nonionic dispersant. 3.根据权利要求2所述方法，其特征在于，所述阴离子分散剂为木质素磺酸钠、纤维素磺酸钠、甲基萘磺酸钠甲醛缩合物、苄基萘磺酸甲醛缩合物中的至少一种；非离子分散剂为烷基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、脂肪酸多元醇酯聚氧乙烯醚中的至少一种。3. method according to claim 2 is characterized in that, described anionic dispersant is sodium lignosulfonate, sodium cellulose sulfonate, sodium methylnaphthalenesulfonate formaldehyde condensate, benzylnaphthalenesulfonate formaldehyde condensate At least one of the non-ionic dispersants is at least one of alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty acid polyol ester polyoxyethylene ether. 4. 根据权利要求1所述方法，其特征在于，所述步骤（1）中研磨采用球磨机，研磨的工艺参数为：转速为400-600 r/min，球料比为8-12:1，研磨时间为1-3 h。4. method according to claim 1, is characterized in that, grinding adopts ball mill in described step (1), and the technological parameter of grinding is: rotating speed is 400-600 r/min, and the ratio of ball to material is 8-12:1, The grinding time is 1-3 h. 5.根据权利要求1所述方法，其特征在于，所述步骤（2）中分散剂为聚丙烯酸钠、聚丙烯酸酯、苯乙烯-甲基丙烯酸共聚物、苯乙烯-马来酸酐共聚物中的至少一种。5 . The method according to claim 1 , wherein the dispersing agent in the step (2) is sodium polyacrylate, polyacrylate, styrene-methacrylic acid copolymer, and styrene-maleic anhydride copolymer. 6 . at least one of. 6. 根据权利要求1所述方法，其特征在于，所述步骤（2）中继续研磨采用球磨机，继续研磨的工艺参数为：转速为400-600 r/min，球料比为8-12:1，研磨时间为9-11 h。6. method according to claim 1, is characterized in that, in described step (2), continue grinding and adopt ball mill, and the technological parameter of continuing grinding is: rotating speed is 400-600 r/min, and ball-to-material ratio is 8-12: 1. The grinding time is 9-11 h. 7.一种如权利要求1所述方法制备得到的液体分散染料。7. A liquid disperse dye prepared by the method of claim 1. 8.一种如权利要求1所述方法制备得到的液体分散染料在印花中的应用。8. the application of the liquid disperse dye prepared by the method as claimed in claim 1 in printing. 9. 根据权利要求8所述应用，其特征在于，所述印花的工艺为：将液体分散染料0.5%-2.5%、粘合剂1%-5.0%、增稠剂0.5%-2.5%和余量的水制成印花色浆，印花，烘干，焙烘，其中百分数为质量百分数，是以液体分散染料、粘合剂、增稠剂和水的总质量为基准。9. application according to claim 8, is characterized in that, the technique of described printing is: liquid disperse dye 0.5%-2.5%, adhesive 1%-5.0%, thickener 0.5%-2.5% and more Amount of water is used to make printing paste, printing, drying and baking, where the percentage is the mass percentage, which is based on the total mass of liquid disperse dyes, binders, thickeners and water.
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