CN114808485B - Disperse reactive dye digital printing ink and preparation method thereof - Google Patents
Disperse reactive dye digital printing ink and preparation method thereof Download PDFInfo
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- CN114808485B CN114808485B CN202210382097.1A CN202210382097A CN114808485B CN 114808485 B CN114808485 B CN 114808485B CN 202210382097 A CN202210382097 A CN 202210382097A CN 114808485 B CN114808485 B CN 114808485B
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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
- D06P1/38—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 reactive 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
- D06P1/60—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
- D06P1/6138—Polymerisation products of glycols, e.g. Carbowax, Pluronics
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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
- D06P1/64—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
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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
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/30—Ink jet printing
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Abstract
The invention relates to the technical field of digital printing ink preparation, and discloses a disperse reactive dye digital printing ink and a preparation method thereof. The method comprises the following steps: (1) The raw materials comprise reactive dye, associated dispersant, short chain fatty alcohol and deionized water; (2) Mixing short-chain fatty alcohol with deionized water to obtain a short-chain fatty alcohol aqueous solution; (3) Mixing reactive dye with deionized water and a short-chain fatty alcohol aqueous solution to prepare a reactive dye dilute solution; (4) Mixing the associative dispersant with deionized water and a short-chain fatty alcohol aqueous solution to prepare an associative dispersant concentrated solution; (5) And mixing the reactive dye dilute solution with the associated dispersing agent concentrated solution to prepare the dispersed reactive dye digital printing ink. The invention can form uniform and stable reactive dye oligomer dispersion liquid, can effectively reduce the requirement of digital printing on pre-applied ground paste of fabrics, and obviously improves the convenience and environmental protection of the digital printing application.
Description
Technical Field
The invention relates to the technical field of digital printing ink preparation, in particular to a disperse reactive dye digital printing ink and a preparation method thereof.
Background
The reactive dye ink is widely used for digital printing of various cotton textiles. However, the strong hydrophilicity of reactive dyes makes their aqueous inks very prone to "bleed" on the print substrate, resulting in poor print definition. For this reason, it is necessary to perform a sizing pretreatment on the printed fabric to inhibit the hydrophilicity of the cotton fabric and wash out the sizing agent on the printed fabric after the printing process is finished. The result of this is complex process, increased cost, higher energy consumption and poor environmental protection. In addition, in order to endow the product with better dispersion storage stability and hydrolysis resistance, the active dye digital printing ink based on the prior art has lower effective content and complex formula, and the product has more production links, so that the wide popularization and low-cost application of the product are limited. At present, the reactive dye ink and related technical characteristics mainly comprise: a preparation method of reactive dye ink based on a moisturizing, solubilizing and dispersing system and a preparation method of reactive dye ink based on nanometer microspheres.
At present, the preparation method of the associated reactive dye ink comprises the following steps:
1. the preparation method of the reactive dye ink based on the moisturizing, solubilizing and dispersing system comprises the following raw materials of reactive dye, deionized water and an auxiliary agent, wherein: the auxiliary agent comprises diethylene glycol, ethylene glycol, glycerol, 1, 4-butanediol as humectant, urea as solubilizer, triethanolamine as pH buffer, disodium edetate and bactericide GXL, wetting agent S465 and surfactant X-100.
As disclosed in "research and preparation of reactive dye ink" by Wang Xiaomei, wu Xuefen, zheng Jiaying, etc. (application chemical engineering, volume 48, 5 th phase), the preparation method of reactive dye ink comprises sequentially adding humectant, pH buffer solution, urea and deionized water into a beaker and stirring uniformly; adding bactericide GXL and wetting agent S465, stirring, adding reactive dye, and stirring; and sealing, standing and filtering the ink to obtain the reactive dye ink.
The preparation method of the reactive dye ink is disclosed in the development of the reactive dye digital ink-jet printing ink (12 th phase of printing and dyeing 2019) such as Ma Jinliang, wen Xiao and Qiao Yaya, and the like, wherein a solubilizer urea, a humectant (diethylene glycol, ethylene glycol, glycerol, 1, 4-butanediol), a pH regulator triethanolamine and a surfactant X-100 are added into a reactive dye solution with proper concentration, deionized water is added for mixing, and a filter membrane is used for filtering after full stirring, so as to prepare the reactive dye ink.
The active dye ink prepared by the method has low effective content, and solves the problems of poor storage stability and poor hydrolysis resistance stability of the active dye by a large amount of auxiliary agents, so that the active dye ink has poor environmental protection; meanwhile, the reactive dye ink contains a higher proportion of amine substances, and long-term corrosion risk to the spray head exists. In addition, the reactive dye ink formulation does not take into account the "bleed" problem that may occur in digital printing applications at all, and has no significant advantages over conventional, conventional reactive dye inks.
2. The preparation method of the active dye ink based on the nano microspheres comprises the following raw materials of active dye, nano microspheres, deionized water and an auxiliary agent, wherein: the nanometer microsphere is anion polystyrene/methacrylic acid nanometer microsphere and cellulose nanometer microsphere, and the auxiliary agent comprises glycerin, polyethylene oxide, polyvinylpyrrolidone, pH regulator, humectant, bactericide and surfactant.
As the preparation method of the reactive dye ink disclosed by Li Hui, chen Yang, liu Guojin and the like of the monochloro-s-triazine reactive dye/nano microsphere composite structural color ink (12 th phase of 55 volume of silk in 2018), a certain amount of monochloro-s-triazine reactive dye and deionized water are taken and placed in a beaker to be stirred to prepare dye liquor; adding anionic polystyrene/methacrylic acid nanometer microsphere emulsion into dye liquor, respectively adding proper amount of glycerol, polyoxyethylene and polyvinylpyrrolidone, performing ultrasonic dispersion, standing, and filtering to obtain the reactive dye ink.
The preparation method of the reactive dye ink is disclosed in the preparation of digital printing ink based on cellulose nanosphere dispersing agent and the performance research thereof (3 rd phase of 27 volume of modern textile technology in 2019) as Shen Jing, zhang Meifei, ma Tingfang and the like, wherein the reactive dye is taken as a main body, the cellulose nanospheres are taken as dispersing agents, and the reactive dye ink is prepared by mixing and fully and uniformly stirring the reactive dye ink with humectant glycol, bactericide CIT/MIT-14 and surfactant sodium dodecyl sulfonate according to a certain proportion.
The reactive dye ink prepared by the method is actually a dispersion liquid of reactive dye molecules and active dye aggregates, and the ratio of the active dye aggregates in the reactive dye ink is generally not low (otherwise, the dye content in the ink is low), so that the reactive dye ink is unfavorable for adsorption and diffusion of dye to fibers when printed fabrics are steamed. In particular, the former is not a single-molecule dye for dyeing cotton textiles, but the nano microspheres are piled up in fiber gaps and subjected to effective self-assembly, so that a three-dimensional ordered photonic crystal structure is obtained to endow the textiles with color. Therefore, the content of the nano microspheres in the ink is high, the particle size is large, and polyvinylpyrrolidone is required to maintain the dispersion stability of the nano microspheres, so that the performance of the ink passing through a spray head is poor; meanwhile, the depolymerization performance of the dye and the microspheres is poor, which is unfavorable for the reactive dye to adsorb, diffuse and color the textile in a single molecule form.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: a digital printing ink of disperse reactive dye and its preparing process are disclosed. The disperse reactive dye digital printing ink prepared by the method can be used for digital printing of various cotton textiles. In the invention, the associative dispersant can be respectively associated with the anionic structure and the hydrophobic structure of the dye through the cationic structure and the long-chain hydrophobic chain links on the associative dispersant, and the associative dispersants can be moderately associated through the long-chain hydrophobic chain links on the associative dispersant, meanwhile, the long-chain polyether chain links on the associative dispersant can endow the associative body with good dispersibility, so that uniform and stable reactive dye oligomer dispersion liquid is ensured to be formed, the requirement of digital printing on pre-applied sizing of fabrics can be effectively reduced, and the convenience and environmental friendliness of the digital printing application are remarkably improved. In addition, dye 'oligomers' formed in a hydrophobic association manner are easy to be dissociated when being steamed at high temperature, and are favorable for fully dyeing fibers by the dye.
In order to achieve the above object, a first aspect of the present invention provides a method for preparing a digital printing ink of a disperse reactive dye, the method comprising the steps of:
(1) Raw material preparation: the raw materials comprise reactive dye, associated dispersant, short-chain fatty alcohol and deionized water;
the associative dispersant is one of a cationic associative dispersant and a weak cationic associative dispersant and is combined with a nonionic associative dispersant;
the structural general formula of the cationic association type dispersing agent is (R 1 )R(R 2 )(R 3 )(R 4 ) Wherein R is a tertiary amine structure having a molecular weight of not more than 300, R 1 Is polysiloxane chain unit with molecular weight of 1500-2500, R 2 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 3 Is polyethylene glycol chain unit with molecular weight of 1500-2500, R 4 A fatty chain 3 to 5 carbons long;
the structural general formula of the weak cation association type dispersing agent is (R 6 )R 5 (R 7 )(R 8 ) Wherein R is 5 Is a tertiary amine structure with molecular weight not higher than 300, R 6 Is polysiloxane chain unit with molecular weight of 1500-2500, R 7 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 8 Polyethylene glycol chain links with molecular weight of 1500-2500;
the structural general formula of the nonionic associative dispersant is (R) 10 )R 9 (R 11 )(R 12 ) Wherein R is 9 Is hydroxyl-terminated polyether triol with molecular weight of 2000-3000, R 10 Is polysiloxane chain unit with molecular weight of 1500-2500, R 11 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 12 Polyethylene glycol chain links with molecular weight of 1500-2500;
the total weight of the reactive dye, the associative dispersant, the short-chain fatty alcohol and the deionized water is 100%, the consumption of the reactive dye is 5-10% by weight, the consumption of the associative dispersant is 3-6% by weight, the consumption of the short-chain fatty alcohol is 5-10% by weight, and the balance is the deionized water;
(2) Mixing short-chain fatty alcohol with part of deionized water to obtain a short-chain fatty alcohol aqueous solution;
(3) Mixing the reactive dye with part of deionized water and part of short-chain fatty alcohol aqueous solution to prepare a reactive dye dilute solution;
(4) Mixing the associative dispersant with the rest deionized water and the rest short-chain fatty alcohol aqueous solution to prepare an associative dispersant concentrated solution;
(5) And mixing the reactive dye dilute solution with the associated dispersing agent concentrated solution to obtain the disperse reactive dye digital printing ink.
Preferably, the nonionic associative dispersant is present in the associative dispersant in an amount of 20 to 40 wt%.
Preferably, the short chain fatty alcohol is a combination of one or two of ethanol, propanol, butanol, diethylene glycol, ethylene glycol, glycerol and 1, 4-butanediol with one of amyl alcohol and hexyl alcohol.
Preferably, the proportion of amyl alcohol or hexyl alcohol in the short-chain fatty alcohol is 5-10 wt%.
Preferably, the specific process of step (2) comprises:
adding deionized water accounting for 20-30 wt% of the total amount into the short-chain fatty alcohol fully, and stirring to obtain the short-chain fatty alcohol aqueous solution.
Preferably, the specific process of step (3) includes:
mixing the reactive dye with the short-chain fatty alcohol aqueous solution with the total amount of 70-90 wt% obtained in the step (2), adding deionized water with the total amount of 50-60 wt% and mixing and dissolving to obtain the reactive dye dilute solution.
Preferably, the specific process of step (5) comprises:
(5.1) adding the association type dispersing agent concentrated solution prepared in the step (4) into the reactive dye dilute solution prepared in the step (3) in 30-50 min under stirring, and then maintaining stirring for 15-30 min;
(5.2) carrying out ultrasonic treatment for 15-30 min under stirring;
(5.3) standing, defoaming and filling to obtain the disperse reactive dye digital printing ink.
Preferably, the reactive dye is one or two of medium-temperature double-reactive-group reactive dyes.
Preferably, the reactive dye is one or two of reactive red, reactive blue and reactive yellow.
The second aspect of the invention provides the disperse reactive dye digital printing ink prepared by the method.
Compared with the prior art, the method has the following advantages and characteristics:
1. in the present invention, a small amount of reactive dye anions interact with the cationic/weak cationic associative dispersants by electrostatic attraction to be associated with the latter; meanwhile, more reactive dyes are mutually associated with the hydrophobic long chains on the macromolecular associated dispersing agent through hydrophobic bond force (entropy driving force) between the hydrophobic structures of the reactive dyes and the hydrophobic long chains; in addition, the associative dispersants are moderately associated with each other by hydrophobic long chains thereon. The three dye association forms lead most of reactive dye single molecules to form dye 'oligomers', and the dispersion liquid of the 'oligomers' has weak infiltration on cotton fibers, the digital printing ground paste can be very thin, even no pre-sizing treatment is needed, and the printing process is concise, energy-saving and environment-friendly;
the schematic structure of the reactive dye 'hydrophobic association oligomer' based on the association type dispersing agent is shown in figure 1, namely the reactive dye and the hydrophobic long chain on the association type dispersing agent are mutually associated through hydrophobic bond force (entropy driving force) between the two. The black chain segments in the figure represent the hydrophobic long chains (polysiloxanes) of the associative dispersants; grey chain segments represent the hydrophilic long chains (polyethylene glycol) of the associative dispersant; S-D-B-R-L represents a reactive dye molecule or ion, wherein S, D, B, R, L represents a water-soluble group, a parent structure, a bridge group, a reactive group and a hydrophobic structure of the reactive dye, respectively.
2. In the invention, the cationic associative dispersant has the capacity of resisting bacteria and resisting corrosion and is beneficial to the long-term storage of the ink; meanwhile, the hydrophobic long chain on the macromolecular association type dispersing agent also has defoaming capability, and the application performance of the ink is better.
3. In the invention, the reactive dye 'oligomer' is based on a hydrophobic association mechanism, is easy to depolymerize/de-associate, is beneficial to the adsorption and diffusion of the reactive dye 'oligomer' to the fiber, and can ensure that the reactive dye 'oligomer' can fully dye the fiber during the printing steaming period.
4. In the invention, the reactive dye is dispersed in an aqueous system in an 'oligomer' mode, and the specific surface of the dye and water is small, so that the hydrolysis reaction of the dye during long-term storage is inhibited.
5. In the invention, the high-concentration association type dispersing agent alcohol aqueous solution slowly drops into the low-concentration dye alcohol aqueous solution, so that the association between the dye and the association type dispersing agent is superior to the association between the association type dispersing agent, and the control of the association number and the association distribution of the dye is facilitated.
6. In the present invention, a small amount of pentanol or hexanol with low surface tension contributes very much to the permeability of the dye during steaming.
7. In the invention, the content of various auxiliary agents is remarkably less, and the ink has weak ionic property and excellent compatibility and compatibility.
Drawings
FIG. 1 is a schematic representation of the structure of a reactive dye "hydrophobically associating oligomer" based on an associative dispersant.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides a preparation method of disperse reactive dye digital printing ink, which comprises the following steps:
(1) Raw material preparation: the raw materials comprise reactive dye, associated dispersant, short-chain fatty alcohol and deionized water;
the associative dispersant is one of a cationic associative dispersant and a weak cationic associative dispersant and is combined with a nonionic associative dispersant;
the cation associated type fractionThe structural general formula of the powder is (R) 1 )R(R 2 )(R 3 )(R 4 ) Wherein R is a tertiary amine structure having a molecular weight of not more than 300, R 1 Is polysiloxane chain unit with molecular weight of 1500-2500, R 2 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 3 Is polyethylene glycol chain unit with molecular weight of 1500-2500, R 4 A fatty chain 3 to 5 carbons long;
the structural general formula of the weak cation association type dispersing agent is (R 6 )R 5 (R 7 )(R 8 ) Wherein R is 5 Is a tertiary amine structure with molecular weight not higher than 300, R 6 Is polysiloxane chain unit with molecular weight of 1500-2500, R 7 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 8 Polyethylene glycol chain links with molecular weight of 1500-2500;
the structural general formula of the nonionic associative dispersant is (R) 10 )R 9 (R 11 )(R 12 ) Wherein R is 9 Is hydroxyl-terminated polyether triol with molecular weight of 2000-3000, R 10 Is polysiloxane chain unit with molecular weight of 1500-2500, R 11 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 12 Polyethylene glycol chain links with molecular weight of 1500-2500;
the total weight of the reactive dye, the associative dispersant, the short-chain fatty alcohol and the deionized water is 100%, the consumption of the reactive dye is 5-10% by weight, the consumption of the associative dispersant is 3-6% by weight, the consumption of the short-chain fatty alcohol is 5-10% by weight, and the balance is the deionized water;
(2) Mixing short-chain fatty alcohol with part of deionized water to obtain a short-chain fatty alcohol aqueous solution;
(3) Mixing the reactive dye with part of deionized water and part of short-chain fatty alcohol aqueous solution to prepare a reactive dye dilute solution;
(4) Mixing the associative dispersant with the rest deionized water and the rest short-chain fatty alcohol aqueous solution to prepare an associative dispersant concentrated solution;
(5) And mixing the reactive dye dilute solution with the associated dispersing agent concentrated solution to obtain the disperse reactive dye digital printing ink.
In the present invention, the cationic associative dispersant has a structural formula (R) 1 )R(R 2 )(R 3 )(R 4 ) Representing that there is R on the structure R 1 、R 2 、R 3 、R 4 Four branch structures.
In particular embodiments, R may be a tertiary amine structure having a molecular weight of 100, 200, or 300; r is R 1 Polysiloxane units which may be 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400 or 2500 in molecular weight; r is R 2 Can be polysiloxane units with molecular weights of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500 or polyethylene glycol units with molecular weights of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500; r is R 3 Polyethylene glycol chain links with molecular weights of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400 or 2500 are possible; r is R 4 May be 3, 4 or 5 carbon long fatty chains.
In the present invention, the weak cation associative dispersant has a structural formula (R 6 )R 5 (R 7 )(R 8 ) Represented by structure R 5 With R thereon 6 、R 7 、R 8 Three branch structures.
In particular embodiments, R5 may be a tertiary amine structure having a molecular weight of 100, 200, or 300; r is R 6 Polysiloxane units which may be 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400 or 2500 in molecular weight; r is R 7 Can be polysiloxane units with molecular weights of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500 or polyethylene glycol units with molecular weights of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500; r is R 8 May be polyethylene glycol units having a molecular weight of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400 or 2500.
At the bookIn the invention, the structural general formula of the nonionic associative dispersant is (R 10 )R 9 (R 11 )(R 12 ) Represented by structure R 9 With R thereon 10 、R 11 、R 12 Three branch structures.
In a specific embodiment, R 9 Hydroxyl-terminated polyether triols having molecular weights of 2000, 2100, 2200, 2300, 2400, 2500, 2600, 2700, 2800, 2900 or 3000; r is R 10 Polysiloxane units which may be 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400 or 2500 in molecular weight; r is R 11 Can be polysiloxane units with molecular weights of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500 or polyethylene glycol units with molecular weights of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500; r is R 12 May be polyethylene glycol units having a molecular weight of 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400 or 2500.
In particular embodiments, the reactive dye may be used in an amount of 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt% or 10 wt%, the associative dispersant may be used in an amount of 3 wt%, 4 wt%, 5 wt% or 6 wt%, and the short chain fatty alcohol may be used in an amount of 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt% or 10 wt%, based on the total weight of the reactive dye, associative dispersant, short chain fatty alcohol and deionized water taken as 100%, with the balance being deionized water.
In a preferred embodiment, the nonionic associative dispersant is present in the associative dispersant in an amount of from 20 to 40 weight percent. Specifically, the nonionic associative dispersant may be present in the associative dispersant in an amount of 20 wt%, 25 wt%, 30 wt%, 35 wt%, or 40 wt%.
In a preferred embodiment, the short chain fatty alcohol is a combination of one or two of ethanol, propanol, butanol, diethylene glycol, ethylene glycol, glycerol and 1, 4-butanediol with one of pentanol and hexanol. For example, the short chain fatty alcohol is a combination of propanol and pentanol, a combination of butanol and hexanol, a combination of diethylene glycol and hexanol.
Further preferably, the proportion of pentanol or hexanol in the short-chain fatty alcohol is 5 to 10 wt%. Specifically, it may be 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt% or 10 wt%.
In a preferred embodiment, the specific process of step (2) comprises:
adding deionized water accounting for 20-30 wt% of the total amount into the short-chain fatty alcohol fully, and stirring to obtain the short-chain fatty alcohol aqueous solution.
In a preferred embodiment, the specific process of step (3) comprises:
mixing the reactive dye with the short-chain fatty alcohol aqueous solution with the total amount of 70-90 wt% obtained in the step (2), adding deionized water with the total amount of 50-60 wt% and mixing and dissolving to obtain the reactive dye dilute solution.
In a preferred embodiment, the specific process of step (5) comprises:
(5.1) adding the association type dispersing agent concentrated solution prepared in the step (4) into the reactive dye dilute solution prepared in the step (3) in 30-50 min under stirring, and then maintaining stirring for 15-30 min;
(5.2) carrying out ultrasonic treatment for 15-30 min under stirring;
(5.3) standing, defoaming and filling to obtain the disperse reactive dye digital printing ink.
In a preferred embodiment, the reactive dye is one or both of a medium temperature type double reactive group reactive dye.
Further preferably, the reactive dye is one or two of reactive red, reactive blue and reactive yellow.
The second aspect of the invention provides the disperse reactive dye digital printing ink prepared by the method.
The printing ink prepared by the method can be widely used for digital printing of various cotton textiles, and the finished product is required to be stored in a sealed manner at a cool and dry place.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
TABLE 1
In table 1:
the structural general formula of the cationic association type dispersing agent is (R 1 )R(R 2 )(R 3 )(R 4 ) Wherein R is triethanolamine, R 1 And R is 2 Are polysiloxane units of molecular weight 2000, R 3 Is a polyethylene glycol chain unit with molecular weight of 2000, R 4 3 butyl;
the structural general formula of the weak cation association type dispersing agent is (R 6 )R 5 (R 7 )(R 8 ) Wherein R is 5 Is triethanolamine, R 6 And R is 7 Are polysiloxane units of molecular weight 2000, R 8 Polyethylene glycol chain with molecular weight of 2000;
the structural general formula of the nonionic association type dispersing agent is (R) 10 )R 9 (R 11 )(R 12 ) Wherein R is 9 Is hydroxyl-terminated polyether triol with molecular weight of 3000, R 10 Is a polysiloxane chain unit with molecular weight of 2000, R 11 And R is 12 Polyethylene glycol chain units with molecular weight of 2000;
example 1
(1) Preparing raw materials, wherein the specific selection and the dosage of the raw materials are shown in table 1;
(2) Deionized water accounting for 20 weight percent of the total weight is added into the short-chain fatty alcohol fully, and the mixture is stirred to prepare the short-chain fatty alcohol aqueous solution.
(3) Mixing the reactive dye with the short-chain fatty alcohol aqueous solution with the total amount of 70 wt% obtained in the step (2), adding deionized water with the total amount of 50 wt% and mixing and dissolving to obtain a reactive dye dilute solution;
(4) Mixing the associative dispersant with the rest deionized water and the rest short-chain fatty alcohol aqueous solution to prepare an associative dispersant concentrated solution;
(5.1) adding the association type dispersing agent concentrated solution prepared in the step (4) into the reactive dye dilute solution prepared in the step (3) within 30min under stirring, and then maintaining stirring for 20min;
(5.2) carrying out ultrasonic treatment for 20min under stirring;
(5.3) standing, defoaming and filling to obtain the disperse reactive dye digital printing ink.
Example 2
(1) Preparing raw materials, wherein the specific selection and the dosage of the raw materials are shown in table 1;
(2) Deionized water in an amount of 25% by weight of the total amount was added to the short-chain fatty alcohol sufficiently and stirred to prepare an aqueous short-chain fatty alcohol solution.
(3) Mixing the reactive dye with the short-chain fatty alcohol aqueous solution with the total amount of 80 weight percent obtained in the step (2), adding deionized water with the total amount of 60 weight percent, mixing and dissolving to obtain a reactive dye dilute solution;
(4) Mixing the associative dispersant with the rest deionized water and the rest short-chain fatty alcohol aqueous solution to prepare an associative dispersant concentrated solution;
(5.1) adding the association type dispersing agent concentrated solution prepared in the step (4) into the reactive dye dilute solution prepared in the step (3) in 40min under stirring, and then maintaining stirring for 20min;
(5.2) carrying out ultrasonic treatment for 20min under stirring;
(5.3) standing, defoaming and filling to obtain the disperse reactive dye digital printing ink.
Example 3
(1) Preparing raw materials, wherein the specific selection and the dosage of the raw materials are shown in table 1;
(2) Deionized water in an amount of 25% by weight of the total amount was added to the short-chain fatty alcohol sufficiently and stirred to prepare an aqueous short-chain fatty alcohol solution.
(3) Mixing the reactive dye with the short-chain fatty alcohol aqueous solution with the total amount of 85 weight percent obtained in the step (2), adding deionized water with the total amount of 55 weight percent, mixing and dissolving to obtain a reactive dye dilute solution;
(4) Mixing the associative dispersant with the rest deionized water and the rest short-chain fatty alcohol aqueous solution to prepare an associative dispersant concentrated solution;
(5.1) adding the association type dispersing agent concentrated solution prepared in the step (4) into the reactive dye dilute solution prepared in the step (3) within 50min under stirring, and then maintaining stirring for 30min;
(5.2) ultrasonic treatment for 30min under stirring;
(5.3) standing, defoaming and filling to obtain the disperse reactive dye digital printing ink.
Test example 1
The average particle size, specific absorbance, zeta potential and conductivity of the printing inks prepared in the examples were measured and the results are shown in table 2.
Detection equipment: nano-particle size and Zeta potential instrument (ZS 90 type, malvern instruments inc., uk).
TABLE 2
As can be seen from table 2, the reactive dye treated with the associative dispersant realizes the design of "oligomerization" according to the change of particle size; compared with the reactive dye solution with the same concentration, the reactive dye 'oligomer' dispersion liquid has similar specific absorbance, and the Zeta potential and the conductivity of the reactive dye 'oligomer' dispersion liquid are not greatly reduced, so that the reactive dye 'oligomer' dispersion liquid has excellent thermodynamic stability.
Test example 2
Compared with the printing with the reactive dye solution with the same concentration, the color fastness of the printing ink for digital printing with the disperse reactive dye prepared by the embodiment has no obvious change, the color depth is improved by 7-12 percent (namely, the covering property of the dye on textiles is improved), and the consumption of printing ground paste (sodium alginate) is reduced by 15-20 percent.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. The preparation method of the disperse reactive dye digital printing ink is characterized by comprising the following steps of:
(1) Raw material preparation: the raw materials comprise reactive dye, associated dispersant, short-chain fatty alcohol and deionized water;
the associative dispersant is one of a cationic associative dispersant and a weak cationic associative dispersant and is combined with a nonionic associative dispersant;
the structural general formula of the cationic association type dispersing agent is (R 1 )R(R 2 )(R 3 )(R 4 ) Wherein R is a tertiary amine structure having a molecular weight of not more than 300, R 1 Is polysiloxane chain unit with molecular weight of 1500-2500, R 2 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 3 Is polyethylene glycol chain unit with molecular weight of 1500-2500, R 4 A fatty chain 3 to 5 carbons long;
the structural general formula of the weak cation association type dispersing agent is (R 6 )R 5 (R 7 )(R 8 ) Wherein R is 5 Is a tertiary amine structure with molecular weight not higher than 300, R 6 Is polysiloxane chain unit with molecular weight of 1500-2500, R 7 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 8 Polyethylene glycol chain links with molecular weight of 1500-2500;
the structural general formula of the nonionic associative dispersant is (R) 10 )R 9 (R 11 )(R 12 ) Wherein R is 9 Is hydroxyl-terminated polyether triol with molecular weight of 2000-3000, R 10 Is polysiloxane chain unit with molecular weight of 1500-2500, R 11 Is polysiloxane chain unit with molecular weight of 1500-2500 or polyethylene glycol chain unit with molecular weight of 1500-2500, R 12 Polyethylene glycol chain links with molecular weight of 1500-2500;
the total weight of the reactive dye, the associative dispersant, the short-chain fatty alcohol and the deionized water is 100%, the consumption of the reactive dye is 5-10% by weight, the consumption of the associative dispersant is 3-6% by weight, the consumption of the short-chain fatty alcohol is 5-10% by weight, and the balance is the deionized water;
(2) Mixing short-chain fatty alcohol with part of deionized water to obtain a short-chain fatty alcohol aqueous solution;
(3) Mixing the reactive dye with part of deionized water and part of short-chain fatty alcohol aqueous solution to prepare a reactive dye dilute solution;
(4) Mixing the associative dispersant with the rest deionized water and the rest short-chain fatty alcohol aqueous solution to prepare an associative dispersant concentrated solution;
(5) And mixing the reactive dye dilute solution with the associated dispersing agent concentrated solution to obtain the disperse reactive dye digital printing ink.
2. The method according to claim 1, wherein the nonionic associative dispersant is present in an amount of 20 to 40 wt%.
3. The method of claim 1, wherein the short chain fatty alcohol is one or a combination of two of ethanol, propanol, butanol, diethylene glycol, ethylene glycol, glycerol, and 1, 4-butanediol, and one of pentanol and hexanol.
4. A process according to claim 3, wherein the proportion of pentanol or hexanol in the short-chain fatty alcohol is from 5 to 10% by weight.
5. The method of claim 1, wherein the specific process of step (2) comprises:
adding deionized water accounting for 20-30 wt% of the total amount into the short-chain fatty alcohol fully, and stirring to obtain the short-chain fatty alcohol aqueous solution.
6. The method according to claim 1 or 5, wherein the specific process of step (3) comprises:
mixing the reactive dye with the short-chain fatty alcohol aqueous solution with the total amount of 70-90 wt% obtained in the step (2), adding deionized water with the total amount of 50-60 wt% and mixing and dissolving to obtain the reactive dye dilute solution.
7. The method according to claim 1 or 5, wherein the specific process of step (5) comprises:
(5.1) adding the association type dispersing agent concentrated solution prepared in the step (4) into the reactive dye dilute solution prepared in the step (3) in 30-50 min under stirring, and then maintaining stirring for 15-30 min;
(5.2) carrying out ultrasonic treatment for 15-30 min under stirring;
(5.3) standing, defoaming and filling to obtain the disperse reactive dye digital printing ink.
8. The method of claim 1, wherein the reactive dye is one or both of medium temperature type double reactive group reactive dyes.
9. The method according to claim 1 or 8, wherein the reactive dye is one or two of reactive red, reactive blue and reactive yellow.
10. A disperse reactive dye digital printing ink prepared by the method of any one of claims 1-9.
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| JP2002235025A (en) * | 2001-02-13 | 2002-08-23 | Pilot Ink Co Ltd | Ink composition for ball-point pen |
| CN110306360A (en) * | 2019-07-19 | 2019-10-08 | 浙江海印数码科技有限公司 | A kind of digit printing high stable reactive dye ink and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002235025A (en) * | 2001-02-13 | 2002-08-23 | Pilot Ink Co Ltd | Ink composition for ball-point pen |
| CN110306360A (en) * | 2019-07-19 | 2019-10-08 | 浙江海印数码科技有限公司 | A kind of digit printing high stable reactive dye ink and preparation method thereof |
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