CN114775312A - Washable cotton fabric dye and preparation method thereof - Google Patents
Washable cotton fabric dye and preparation method thereof Download PDFInfo
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- CN114775312A CN114775312A CN202210455968.8A CN202210455968A CN114775312A CN 114775312 A CN114775312 A CN 114775312A CN 202210455968 A CN202210455968 A CN 202210455968A CN 114775312 A CN114775312 A CN 114775312A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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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
- D06P1/0056—Dyeing with polymeric dyes involving building the polymeric dyes on the fibres
- D06P1/0064—Dyeing with polymeric dyes involving building the polymeric dyes on the fibres by using reactive polyfunctional compounds, e.g. crosslinkers
- D06P1/0072—Heterocyclic compounds
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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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
The invention relates to a washable cotton fabric dye and a preparation method thereof, belonging to the technical field of printing and dyeing and comprising the following raw materials in percentage by mass: 2-4% of cross-linkable pigment, 521-2% of quaternary ammonium salt, 30-40% of polyisocyanate, 18-27% of polyol, 0.3-0.5% of dibutyltin dilaurate, 8-14% of chain extender, 6-10% of acrylate monomer and 0.06-0.1% of initiator; the preparation process comprises the following steps: mixing polyol, isocyanate and dibutyltin dilaurate, stirring for reacting for 2 hours, cooling to 60 ℃, adding a solvent, quaternary ammonium salt-52, a crosslinkable pigment and a chain extender, stirring for reacting for 2 hours at 80 ℃, cooling to 70-75 ℃, adding an acrylate monomer and an initiator, stirring for reacting for 5-6 hours at 70-80 ℃, and removing the solvent in vacuum to obtain the washable cotton fabric dye, wherein the fastness of the dye prepared by the method is 5-level, and the dye has excellent washable characteristics.
Description
Technical Field
The invention belongs to the technical field of printing and dyeing, and particularly relates to a washable cotton fabric dye and a preparation method thereof.
Background
The cotton fabric is prepared from cotton fibers, has the advantages of good water absorption, hygroscopicity, easy dyeing, soft hand feeling, moderate strength, comfortable wearing and the like, and is widely applied to production and life.
The traditional cotton fabric dyeing adopts reactive dye or direct dye, the surface of cotton fiber is electronegative in the dyeing process, additives such as neutral electrolyte and the like are required to be added to dye the fiber, the existing dye modification generally reduces the use of the additives in the dyeing process by endowing the dye with positive charge or increasing the substantivity of the dye and improving the electrostatic attraction or coulomb force between the dye and the fiber, Chinese patent CN101187175A discloses a natural dye dyeing method of the cotton fiber, a modifier containing cationic groups is used for preparing a modifier solution, the cotton fiber is firstly modified, the natural dye is used for dyeing, and the natural dye dyeing of the cotton fiber is completed after cleaning. The patent is complex in process, cotton fibers need to be modified by cationic modification liquid and then dyed, and the patent uses micromolecular dyes which are easy to cause environmental pollution in the dyeing process and easy to migrate, discolor and not resistant to washing, so that the technical problem to be solved at present is to provide the washing-resistant cotton fabric dye.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a washable cotton fabric dye and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the dye for the washable cotton fabric comprises the following raw materials in percentage by mass: 2-4% of cross-linkable pigment, 521-2% of quaternary ammonium salt, 30-40% of polyisocyanate, 18-27% of polyol, 0.3-0.5% of dibutyltin dilaurate, 8-14% of chain extender, 6-10% of acrylate monomer and 0.06-0.1% of initiator;
the dye for the washable cotton fabric is prepared by the following steps:
firstly, carrying out vacuum dehydration on a crosslinkable pigment, quaternary ammonium salt-52 and polyol at 110 ℃, then mixing the polyol, isocyanate and dibutyltin dilaurate, stirring and reacting at 70-80 ℃ for 2 hours under the protection of nitrogen, then cooling to 60 ℃, adding a solvent, the quaternary ammonium salt-52, the crosslinkable pigment and a chain extender, heating to 80 ℃, and stirring and reacting for 2 hours to obtain a first composition;
and secondly, cooling the first composition to 70-75 ℃, preserving heat, adding an acrylate monomer and an initiator, controlling the reaction temperature to 70-80 ℃, stirring for reaction for 5-6h, after the reaction is finished, heating to 110 ℃, removing the solvent in vacuum, and naturally cooling to room temperature to obtain the washable cotton fabric dye.
Further, the crosslinkable pigment is prepared by the following steps:
step A1, adding reactive bright red X-3B, tetrahydrofuran and deionized water into a three-neck flask under an ice bath condition, heating to 45 ℃, simultaneously dropwise adding an octafluoropentanol tetrahydrofuran solution and a sodium hydroxide solution with the mass fraction of 10% into the three-neck flask under the stirring condition, controlling the dropwise adding speed to be 1 drop/second, stirring and reacting for 2 hours after the dropwise adding is finished, and removing the tetrahydrofuran and the deionized water by rotary evaporation after the reaction is finished to obtain an intermediate product;
wherein the dosage ratio of the active bright red X-3B, tetrahydrofuran, deionized water, octafluoropentanol tetrahydrofuran solution and sodium hydroxide solution is 0.01 mol: 60-70 mL: 30-40 mL: 10mL of: 4.5-5.2g of octafluoropentanol tetrahydrofuran solution prepared by mixing octafluoropentanol and tetrahydrofuran in a ratio of 0.01 mol: 10mL, under the alkaline condition, leading the reactive brilliant red X-3B and the octafluoropentanol to carry out HCl elimination reaction to obtain an intermediate product, wherein the specific reaction process is as follows:
step A2, adding potassium carbonate and diethylenetriamine into DMF, controlling the reaction temperature to be 60 ℃, adding an intermediate product under the stirring condition, monitoring by TLC until the reaction raw material point disappears, and after the reaction is finished, performing rotary evaporation to remove DMF to obtain a crosslinkable pigment;
wherein the dosage ratio of the potassium carbonate, the diethylenetriamine, the DMF and the intermediate product is 0.9-1.1 g: 0.01 mol: 50-60 mL: 0.01mol, under the alkaline condition, leading the intermediate product and diethylenetriamine to carry out elimination of HCl reaction to obtain the crosslinkable pigment, wherein the specific reaction process is as follows:
furthermore, the acrylate monomer is formed by mixing one or more of acrylate, methacrylate, styrene, butyl acrylate and butyl methacrylate according to any proportion.
Further, the initiator is one or more of azobisisobutyronitrile, benzoyl peroxide and phenylacetyl peroxide which are mixed according to any proportion.
Furthermore, the polyisocyanate is one or more of toluene-2, 4-diisocyanate, 4-diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate which are mixed according to any proportion.
The polyol is one or two of polyether polyol and polyester polyol mixed according to any ratio.
Furthermore, the solvent is one or more of dioxane, N-dimethyl amide, N-methyl pyrrolidone and ethyl acetate which are mixed according to any proportion.
Further, the chain extender is one or more of diethanolamine, triethanolamine and 2, 2-dimethylolpropionic acid which are mixed according to any proportion.
The invention has the beneficial effects that:
the invention provides a washable cotton fabric dye, which is an acrylate chemically-modified polyurethane high-molecular dye, wherein acrylate and polyurethane are combined in a chemical bonding form, so that the dye has excellent performances of polyurethane and acrylate, then reactive brilliant red X-3B is used as a color body, a compound with an F-C long chain and an amino compound are grafted on the molecule of the color body, a crosslinkable pigment is obtained, and the crosslinkable pigment is-NH (hydrogen-NH) on the molecule of the crosslinkable dye2Can react with NCO-, active brilliant red X-3B is bonded in the polyurethane chain, the hydrophobic substance is represented by the low surface free energy of the long chain F-C, the high molecular dye of the invention also adds quaternary ammonium salt-52, contains a plurality of hydroxyl groups which can participate in the polymerization reaction of polyurethane, contains quaternary ammonium salt structure, on one hand, the antibacterial property is exerted, on the other hand, the static adsorption effect can be formed between the high molecular dye and the crosslinkable pigment, the dyeing is improvedThe dye-uptake, color depth and abrasion resistance of the material on cotton fiber are firm, in conclusion, the dye-uptake of the dye prepared by the invention is more than 93%, the fastness to washing is grade 5, and the dye has excellent washing resistance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example provides a crosslinkable pigment, made by the steps of:
step A1, adding 0.01mol of active bright red X-3B, 60mL of tetrahydrofuran and 30mL of deionized water into a three-neck flask under an ice bath condition, heating to 45 ℃, simultaneously dropwise adding 10mL of octafluoropentanol tetrahydrofuran solution and 4.5g of sodium hydroxide solution with the mass fraction of 10% into the three-neck flask under a stirring condition, controlling the dropwise adding speed to be 1 drop/second, stirring and reacting for 2 hours after dropwise adding, and performing rotary evaporation to remove tetrahydrofuran and deionized water after the reaction is finished to obtain an intermediate product, wherein the octafluoropentanol tetrahydrofuran solution is prepared by mixing octafluoropentanol and tetrahydrofuran according to the dosage ratio of 0.01 mol: 10mL of the mixture is mixed;
and step A2, adding 0.9g of potassium carbonate and 0.01mol of diethylenetriamine into 50mL of DMF, controlling the reaction temperature to be 60 ℃, adding 0.01mol of intermediate product under the stirring condition, monitoring by TLC until the reaction raw material point disappears, and after the reaction is finished, performing rotary evaporation to remove DMF to obtain the crosslinkable pigment.
Example 2
This example provides a crosslinkable pigment, which is prepared by the following steps:
step A1, adding 0.01mol of active bright red X-3B, 65mL of tetrahydrofuran and 35mL of deionized water into a three-neck flask under an ice bath condition, heating to 45 ℃, simultaneously dropwise adding 10mL of octafluoropentanol tetrahydrofuran solution and 4.8g of sodium hydroxide solution with the mass fraction of 10% into the three-neck flask under a stirring condition, controlling the dropwise adding speed to be 1 drop/second, stirring and reacting for 2 hours after dropwise adding, and performing rotary evaporation to remove the tetrahydrofuran and the deionized water after the reaction is finished to obtain an intermediate product, wherein the octafluoropentanol tetrahydrofuran solution is prepared by mixing octafluoropentanol and tetrahydrofuran according to the dosage ratio of 0.01 mol: 10mL of the mixture is mixed;
step A2, adding 1.0g of sodium hydroxide and 0.01mol of diethylenetriamine into 55mL of deionized water, controlling the reaction temperature to 60 ℃, adding 0.01mol of intermediate product under the stirring condition, monitoring by TLC until the reaction raw material point disappears, and after the reaction is finished, removing DMF by rotary evaporation to obtain the crosslinkable pigment.
Example 3
This example provides a crosslinkable pigment, which is prepared by the following steps:
step A1, adding 0.01mol of active bright red X-3B, 70mL of tetrahydrofuran and 40mL of deionized water into a three-neck flask under an ice bath condition, heating to 45 ℃, simultaneously dropwise adding 10mL of octafluoropentanol tetrahydrofuran solution and 5.2g of sodium hydroxide solution with the mass fraction of 10% into the three-neck flask under a stirring condition, controlling the dropwise adding speed to be 1 drop/second, stirring and reacting for 2h after the dropwise adding is finished, and performing rotary evaporation to remove tetrahydrofuran and deionized water after the reaction is finished to obtain an intermediate product, wherein the octafluoropentanol tetrahydrofuran solution is prepared by mixing octafluoropentanol and tetrahydrofuran according to the dosage ratio of 0.01 mol: 10mL of the mixture is obtained;
and A2, adding 1.1g of sodium hydroxide and 0.01mol of diethylenetriamine into 60mL of deionized water, controlling the reaction temperature to be 60 ℃, adding 0.01mol of intermediate product under the stirring condition, monitoring by using TLC (thin layer chromatography) until the reaction raw material point disappears, and after the reaction is finished, performing rotary evaporation to remove DMF (dimethyl formamide) to obtain the crosslinkable pigment.
Comparative example 1
This example provides a crosslinkable pigment, made by the steps of:
step A1, adding 1.1g of sodium hydroxide and 0.01mol of diethylenetriamine into 60mL of deionized water, controlling the reaction temperature to 20 ℃, adding 0.01mol of active bright red X-3B under stirring, monitoring by TLC until the point of the reaction raw material (active bright red X-3B) disappears, after the reaction is finished, transferring the reaction product into acetone with four times of volume, precipitating solids, filtering, and drying the filter cake in vacuum at 60 ℃ to constant weight to obtain the crosslinkable pigment.
Comparative example 2
This comparative example is reactive bright red X-3B.
Example 4
The dye for the washable cotton fabric comprises the following raw materials in percentage by mass: 2% of the crosslinkable pigment of example 1, quaternary ammonium salt-522%, polyisocyanate 30%, polyol 27%, dibutyltin dilaurate 0.3%, chain extender 14%, acrylate monomer 6%, initiator 0.1%;
the washable cotton fabric dye is prepared by the following steps:
firstly, carrying out vacuum dehydration on a crosslinkable pigment, quaternary ammonium salt-52 and polyol at 110 ℃, then mixing the polyol, isocyanate and dibutyltin dilaurate, stirring and reacting at 70 ℃ for 2h under the protection of nitrogen, then cooling to 60 ℃, adding a solvent, quaternary ammonium salt-52, the crosslinkable pigment and a chain extender, heating to 80 ℃, and stirring and reacting for 2h to obtain a first composition;
and secondly, cooling the first composition to 70 ℃, preserving heat, adding an acrylate monomer and an initiator, controlling the reaction temperature to 70 ℃, stirring for reaction for 5 hours, after the reaction is finished, heating to 110 ℃, removing the solvent in vacuum, and naturally cooling to room temperature to obtain the washable cotton fabric dye.
Wherein the acrylate monomer is acrylate, the initiator is azobisisobutyronitrile, the polyisocyanate is toluene-2, 4-diisocyanate, the polyol is polyether polyol, the chain extender is diethanolamine, and the solvent is dioxane.
Example 5
A washable cotton fabric dye comprises the following raw materials in percentage by mass: 4% of the crosslinkable pigment of example 2, quaternary ammonium salt-521%, 40% of polyisocyanate, 18% of polyol, 0.5% of dibutyltin dilaurate, 8% of chain extender, 10% of acrylate monomer and 0.06% of initiator;
the washable cotton fabric dye is prepared by the following steps:
firstly, carrying out vacuum dehydration on a crosslinkable pigment, quaternary ammonium salt-52 and polyol at 110 ℃, then mixing the polyol, isocyanate and dibutyltin dilaurate, stirring and reacting at 70 ℃ for 2 hours under the protection of nitrogen, then cooling to 60 ℃, adding a solvent, quaternary ammonium salt-52, the crosslinkable pigment and a chain extender, heating to 80 ℃, and stirring and reacting for 2 hours to obtain a first composition;
and secondly, cooling the first composition to 70 ℃, preserving heat, adding an acrylate monomer and an initiator, controlling the reaction temperature to 80 ℃, stirring for reaction for 5 hours, after the reaction is finished, heating to 110 ℃, removing the solvent in vacuum, and naturally cooling to room temperature to obtain the washable cotton fabric dye.
Wherein the acrylate monomer is acrylate, the initiator is benzoyl peroxide, the polyisocyanate is 4, 4-diphenylmethane diisocyanate, the polyol is polyester polyol, the chain extender is triethanolamine, and the solvent is dioxane.
Example 6
The dye for the washable cotton fabric comprises the following raw materials in percentage by mass: 3% of the crosslinkable pigment of example 3, quaternary ammonium salt-521.5%, 35% of polyisocyanate, 22% of polyol, 0.4% of dibutyltin dilaurate, 10% of chain extender, 8% of acrylate monomer and 0.08% of initiator;
the dye for the washable cotton fabric is prepared by the following steps:
firstly, carrying out vacuum dehydration on a crosslinkable pigment, quaternary ammonium salt-52 and polyol at 110 ℃, then mixing the polyol, isocyanate and dibutyltin dilaurate, stirring and reacting for 2h at 75 ℃ under the protection of nitrogen, then cooling to 60 ℃, adding a solvent, quaternary ammonium salt-52, the crosslinkable pigment and a chain extender, heating to 80 ℃, and stirring and reacting for 2h to obtain a first composition;
and secondly, cooling the first composition to 72 ℃, preserving heat, adding an acrylate monomer and an initiator, controlling the reaction temperature to be 75 ℃, stirring for reaction for 5.5 hours, after the reaction is finished, heating to 110 ℃, removing the solvent in vacuum, and naturally cooling to room temperature to obtain the washable cotton fabric dye.
Wherein the acrylate monomer is butyl acrylate, the initiator is benzoyl peroxide, the polyisocyanate is toluene-2, 4-diisocyanate, the polyol is polyether polyol, the chain extender is 2, 2-dimethylolpropionic acid, and the solvent is N, N-dimethylamide.
Comparative example 3
The crosslinkable pigment of example 4 was replaced by the substance of comparative example 1, the remaining starting materials and the preparation process being unchanged.
Comparative example 4
The crosslinkable pigment from example 5 was replaced by the substance from comparative example 2, and the remaining starting materials and preparation were unchanged.
Comparative example 5
The quaternary ammonium salt-52 in example 6 was removed, and the remaining raw materials and preparation process were unchanged.
The dyes prepared in the examples 4-6 and the comparative examples 3-5 are used for printing and dyeing cotton fabric coatings, and the specific process comprises the following steps: the dye solution of each group is added into hot water at 60 ℃, and the weight ratio of the dye to the water is 1: 10, stirring uniformly, standing for 3 hours, directly scraping and coating the fabric by a scraper, then drying in a 60 ℃ oven, and then testing the performance;
dye uptake: and measuring the absorbance of the dyeing stock solution and the dyeing residual solution at the maximum absorption wavelength of the dye by using an ultraviolet spectrophotometer, and obtaining the concentration of the dye solution according to a standard curve so as to obtain the dye uptake of the dye on different fibers. The dye uptake E and the fixation degree F of the dye are calculated according to the formulas (1) and (2).
E＝(C0-C1/C0)x100％ (1)
F＝(C0-C1-C2/C0)x100％ (2)
In the formula, C0 and C1 represent the dye liquor concentration before and after dyeing, and C2 represents the soaping residue concentration after soaping.
(II) color fastness: color fastness to washing in accordance with ISO105C10-2006 part C10 of the textile color fastness test: soap or soda wash fastness "; colour fastness to rubbing according to ISO105X12-2001, part X12 of the textile colour fastness test: measuring the color fastness to rubbing; color fastness to sunlight according to ISO105B02-2013 "textile color fastness test part B02: fastness to artificial color: xenon arc.
The test results are shown in table 1:
TABLE 1
As can be seen from Table 1, the dyes prepared in examples 4 to 6 have a dye uptake of 93% or more and a fastness to washing of 5, and therefore, the dyes prepared according to the present invention have higher fastness.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (6)
1. The dye for the washable cotton fabric is characterized by comprising the following raw materials in percentage by mass: 2-4% of cross-linkable pigment, 521-2% of quaternary ammonium salt, 30-40% of polyisocyanate, 18-27% of polyol, 0.3-0.5% of dibutyltin dilaurate, 8-14% of chain extender, 6-10% of acrylate monomer and 0.06-0.1% of initiator;
wherein the crosslinkable pigment is prepared by the following steps:
step A1, mixing reactive bright red X-3B, tetrahydrofuran and deionized water under an ice bath condition, heating to 45 ℃, dropwise adding an octafluoropentanol tetrahydrofuran solution and a sodium hydroxide solution with the mass fraction of 10% under stirring, and after dropwise adding, stirring and reacting for 2 hours to obtain an intermediate product;
and step A2, adding potassium carbonate and diethylenetriamine into DMF, controlling the reaction temperature to 60 ℃, adding the intermediate product under the stirring condition, monitoring by TLC until the reaction raw material point disappears, and after the reaction is finished, removing the DMF by rotary evaporation to obtain the crosslinkable pigment.
2. The cotton fabric washing resistant dye according to claim 1, wherein the amount ratio of the reactive bright red X-3B, tetrahydrofuran, deionized water, octafluoropentanol tetrahydrofuran solution and sodium hydroxide solution in step A1 is 0.01 mol: 60-70 mL: 30-40 mL: 10mL of: 4.5-5.2 g.
3. A cotton wash resistant dye according to claim 2, wherein the octafluoropentanol tetrahydrofuran solution obtained in step a1 is prepared from octafluoropentanol and tetrahydrofuran in an amount ratio of 0.01 mol: 10mL of the above-mentioned components were mixed together.
4. A cotton washing resistant fabric dye according to claim 1, wherein the ratio of the amount of potassium carbonate, diethylenetriamine, DMF and intermediate products in step a2 is 0.9-1.1 g: 0.01 mol: 50-60 mL: 0.01 mol.
5. A dye for cotton fabrics resistant to washing with water according to claim 4, characterized in that the solvent is one or more of dioxane, N-dimethyl amide, N-methyl pyrrolidone and ethyl acetate mixed in any proportion.
6. The preparation method of the washable cotton fabric dye according to claim 1, characterized by comprising the following steps:
firstly, carrying out vacuum dehydration on a crosslinkable pigment, quaternary ammonium salt-52 and polyol at 110 ℃, then mixing the polyol, isocyanate and dibutyltin dilaurate, stirring and reacting at 70-80 ℃ for 2 hours under the protection of nitrogen, then cooling to 60 ℃, adding a solvent, the quaternary ammonium salt-52, the crosslinkable pigment and a chain extender, heating to 80 ℃, and stirring and reacting for 2 hours to obtain a first composition;
and secondly, cooling the first composition to 70-75 ℃, preserving heat, adding an acrylate monomer and an initiator, controlling the reaction temperature to 70-80 ℃, stirring for reaction for 5-6h, after the reaction is finished, heating to 110 ℃, removing the solvent in vacuum, and naturally cooling to room temperature to obtain the washable cotton fabric dye.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115637590A (en) * | 2022-10-26 | 2023-01-24 | 浙江九舜纺织有限公司 | Preparation method and application of super-strong and super-wear-resistant cotton fabric |
| CN116285497A (en) * | 2023-01-28 | 2023-06-23 | 常熟市琴达针织印染有限公司 | Washing-resistant ink for printing and dyeing and preparation method thereof |
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