CN111138886A - Liquid disperse dye and preparation method and application thereof - Google Patents

Liquid disperse dye and preparation method and application thereof Download PDF

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Publication number
CN111138886A
CN111138886A CN201911365167.7A CN201911365167A CN111138886A CN 111138886 A CN111138886 A CN 111138886A CN 201911365167 A CN201911365167 A CN 201911365167A CN 111138886 A CN111138886 A CN 111138886A
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China
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disperse dye
grinding
disperse
printing
liquid
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CN111138886B (en
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蔡再生
李云峰
范追追
王梦婷
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Zhejiang Kefeng Silicone Co ltd
Donghua University
National Dong Hwa University
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Zhejiang Kefeng Silicone Co ltd
Donghua University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0001Post-treatment of organic pigments or dyes
    • C09B67/0002Grinding; Milling with solid grinding or milling assistants
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0071Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/008Preparations of disperse dyes or solvent dyes
    • C09B67/0082Preparations of disperse dyes or solvent dyes in liquid form
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/46General 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/52General 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
    • D06P1/5207Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • D06P1/525Polymers of unsaturated carboxylic acids or functional derivatives thereof
    • D06P1/5257(Meth)acrylic acid
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/60General 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
    • D06P1/613Polyethers without nitrogen
    • D06P1/6131Addition products of hydroxyl groups-containing compounds with oxiranes
    • D06P1/6133Addition products of hydroxyl groups-containing compounds with oxiranes from araliphatic or aliphatic alcohols
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/64General 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
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65118Compounds containing hydroxyl groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/673Inorganic compounds
    • D06P1/67383Inorganic compounds containing silicon
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/34Material containing ester groups
    • D06P3/52Polyesters
    • D06P3/54Polyesters 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

The invention relates to a liquid disperse dye and a preparation method and application thereof. The method comprises the following steps: mixing a grinding aid with deionized water to enable the grinding aid to fully swell, and adding a disperse dye, ethylene glycol and a dispersing agent for grinding; adding dispersant, grinding and filtering. The method is simple to operate, and the prepared liquid disperse dye has 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 powdery disperse dyes, the liquid disperse dyes have many incomparable advantages that ① liquid disperse dyes can achieve good dispersion effect by using less dispersant, the cost is saved, the dye utilization rate is improved, ② omits a spray drying process, simplifies a process, saves energy, ③ facilitates automatic material taking, accords with the automatic development trend of the printing and dyeing industry, ④ eliminates dust pollution and the like from the source, which leads the liquid disperse dyes to be gradually valued in recent years as a commercial preparation of the disperse dyes.
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:
① particle size test, diluting a small amount of liquid ultra-fine disperse dye, and measuring the particle size of the dye in the disperse system at 25 deg.C with a Nano-ZS90 type nanometer particle size analyzer.
② stability test the prepared liquid disperse dye was stored at rest (20 ℃ C.) for 60 days to see if any 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 (10)

1. A preparation method of liquid disperse dye 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.
2. The method according to claim 1, wherein the grinding aid in step (1) is at least one of silica, titania, alumina, bentonite.
3. The method according to claim 1, wherein the disperse dye in the step (1) is at least one of disperse blue 79, disperse orange 30 and disperse red 54; the dispersant is an anionic dispersant and a nonionic dispersant with the mass ratio of 1:1-3: 1.
4. The method of claim 3, wherein the anionic dispersant is at least one of sodium lignosulfonate, sodium cellulose sulfonate, sodium methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonate formaldehyde condensate; the nonionic dispersant is at least one of alkylphenol polyoxyethylene, fatty alcohol polyoxyethylene and fatty acid polyol ester polyoxyethylene.
5. The method according to claim 1, wherein the grinding in step (1) comprises the following process parameters: the rotating speed is 400-600r/min, the ball-material ratio is 8-12:1, and the grinding time is 1-3 h.
6. The method according to claim 1, wherein the dispersant in the step (2) is at least one of sodium polyacrylate, styrene-methacrylic acid copolymer and styrene-maleic anhydride copolymer.
7. The method of claim 1, wherein the process parameters for the continuous grinding in step (2) are: the rotating speed is 400-600r/min, the ball-material ratio is 8-12:1, and the grinding time is 9-11 h.
8. A liquid disperse dye prepared according to the method of claim 1.
9. Use of a liquid disperse dye prepared according to the process of claim 1 in printing.
10. The use according to claim 9, wherein the printing process is: 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.
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CN114196232A (en) * 2021-12-27 2022-03-18 浙江博澳新材料股份有限公司 Disperse dye and preparation method thereof
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CN111675925A (en) * 2020-06-12 2020-09-18 大连工业大学 Mixed dye and supercritical CO using same2Waterless color matching method
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CN115197585A (en) * 2021-04-12 2022-10-18 福建莱得化工科技有限公司 Preparation method of environment-friendly low-emission liquid disperse dye
CN113462195A (en) * 2021-07-06 2021-10-01 浙江捷发科技股份有限公司 Preparation method of modified sodium lignosulfonate dye dispersing agent
CN113831759A (en) * 2021-09-16 2021-12-24 浙江理工大学 Liquid disperse dye for high-temperature dip dyeing and preparation method thereof
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CN115449348A (en) * 2022-10-12 2022-12-09 江西广源化工有限责任公司 Grinding aid and preparation method and application thereof
CN116285414A (en) * 2022-12-29 2023-06-23 晋江市新胜星化工科技有限公司 Preparation process of high-stability liquid disperse dye
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