CN117924965B - A photochromic printing dye and its preparation method and application - Google Patents
A photochromic printing dye and its preparation method and applicationInfo
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- CN117924965B CN117924965B CN202410073008.4A CN202410073008A CN117924965B CN 117924965 B CN117924965 B CN 117924965B CN 202410073008 A CN202410073008 A CN 202410073008A CN 117924965 B CN117924965 B CN 117924965B
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- dye
- solution
- photochromic printing
- photochromic
- printing dye
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/008—Preparations of disperse dyes or solvent dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
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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
- D06P1/673—Inorganic compounds
- D06P1/67383—Inorganic compounds containing silicon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
本申请涉及印花染料技术领域，特别涉及一种光致变色印花染料及其制备方法、应用。本申请提供的光致变色印花染料由分散染料和微胶囊分散在有机连续相中得到，所述分散染料选用靛蓝染料、蒽醌染料或三芳甲烷染料，所述微胶囊的芯材为氧化剂，所述微胶囊的壳材为SiO2复合物。本申请提供的印花染料含有以氧化剂作为芯材的微胶囊，水洗过程中氧化剂从壳材中缓释释放，具有较强的氧化性，一方面可以起到杀菌作用，另一方面在晾晒过程中，可以与易发生光氧化反应的分散染料进行反应，使分散染料缓慢分解褪色。
The present application relates to the technical field of printing dyes, and in particular to a photochromic printing dye, its preparation method, and application. The photochromic printing dye provided in the present application is obtained by dispersing a disperse dye and microcapsules in an organic continuous phase. The disperse dye is selected from indigo dye, anthraquinone dye, or triarylmethane dye. The core material of the microcapsule is an oxidant, and the shell material of the microcapsule is a SiO2 complex. The printing dye provided in the present application contains microcapsules with an oxidant as the core material. During the washing process, the oxidant is slowly released from the shell material and has strong oxidizing properties. On the one hand, it can have a bactericidal effect. On the other hand, during the drying process, it can react with the disperse dye that is prone to photooxidation, causing the disperse dye to slowly decompose and fade.
Description
Technical Field
The application relates to the technical field of printing dyes, in particular to a photochromic printing dye, and a preparation method and application thereof.
Background
Textiles such as towels, underwear, bed sheets and the like can absorb organic matters such as skin grease, sweat, cell debris and the like in daily use, bacteria, fungi and the like are easy to grow after long-term use, and the health is affected. Therefore, the products need to be replaced periodically in the use process, but users often cannot judge the performance and the use time of the textile products through naked eyes, so that the textile products cannot be replaced in time in a reasonable time.
The color-changing label is stuck on the inner side of the towel to ensure that the label is contacted with the skin, and when the towel is used for a period of time, the label can change in color due to the absorption of moisture and sweat. When the label changes from the original color to another color, it indicates that the towel has been used for a long time and needs to be replaced. For example, patent JP7130292B1 discloses a towel in which a mark is attached to the towel, and the mark is disappeared or appears after repeated washing, thereby judging the service life. However, the color-changing label may be detached due to friction, washing, etc., thereby affecting the reminding function. In addition, long-term use of color-changing labels can result in damage to the towel fibers, affecting the service life of the towel.
Disclosure of Invention
The embodiment of the application provides a photochromic printing dye, which can be printed on textiles to form printed icons, and the printed icons fade after washing and sun-drying for a certain number of times to remind a user to replace in time so as to solve the problem that color-changing labels are adhered to the textiles and are easy to fall off in the related art.
In a first aspect, the application provides a photochromic printing dye, which is prepared by dispersing a disperse dye and a microcapsule in an organic continuous phase, wherein the disperse dye is indigo dye, anthraquinone dye or triarylmethane dye, the core material of the microcapsule is an oxidant, and the shell material of the microcapsule is a SiO 2 compound.
In some embodiments, the oxidizing agent is selected from any one of sodium ferrate, ferrous sulfate, polymeric ferric sulfate, sodium hypochlorite, aluminum trifluoride, or periodic acid.
In some embodiments, the organic continuous phase is selected from any of ethylene glycol, 1, 2-propanediol, and glycerol.
In a second aspect, the present application also provides a preparation method of the photochromic printing dye, which comprises the following steps:
S101, using a high-speed shearing dispersion disc to fully disperse dye in an organic continuous phase at room temperature to obtain a disperse dye solution;
S102, adding an anti-settling agent into the disperse dye solution at room temperature, fully dissolving, then adding microcapsules, and uniformly dispersing to obtain the photochromic printing dye.
In some embodiments, the microcapsules are prepared by the following process:
Adding hydrophilic mesoporous nano SiO 2 into an oxidant solution, and vacuumizing to completely adsorb the oxidant solution onto nano SiO 2 particles;
adding an organic solvent into an emulsifier for full dissolution to obtain an oil phase solution;
Adding nano SiO 2 particles for adsorbing an oxidant solution into the oil phase solution, and stirring at a rotating speed of 500-2000 rpm to obtain emulsion with uniform particle size;
and adding the shell material solution into the emulsion, adding an alkali solution to adjust the pH value to 7-10, reacting for 5-12 hours at the temperature of 30-60 ℃, and filtering, washing and drying after the reaction is finished to obtain the microcapsule.
In some embodiments, the organic solvent is selected from one or more of n-hexane, cyclohexane, toluene, xylene, and diethyl ether.
In some embodiments, the emulsifier is selected from one or more of Tween-80, polyvinyl alcohol, OP-10, styrene-maleic anhydride copolymer, sodium dodecylbenzene sulfonate, and sodium dodecylsulfate.
In some embodiments, the shell material is a mixture of one or more of ethyl orthosilicate, tetrabutyl titanate, KH550, KH560, KH 570.
In some embodiments, the alkali solution is any one of sodium hydroxide, potassium hydroxide, calcium hydroxide and triethanolamine.
In some embodiments, the mass ratio of the oxidizing agent to the deionized water in the oxidizing agent solution is 0.5-3.
In some embodiments, the emulsifier is added in an amount of 1% -5% by mass of the oxidant solution.
In some embodiments, the addition amount of the shell material is 0.5-2 times of the mass of the oxidant solution.
In some embodiments, the weight ratio of the disperse dye to the organic continuous phase is 1:5-1:15.
In some embodiments, the anti-settling agent is a mixture of one or more of an organo montmorillonite, a polyethylene wax, and a nonionic surfactant.
In some embodiments, the mass concentration of the anti-settling agent in the photochromic printing dye is 1 per mill to 1 percent.
In some embodiments, the mass concentration of the microcapsules in the photochromic printing dye is 2 per mill to 2 percent.
In a third aspect, the application also provides a method for printing textiles by adding the photochromic printing dye into screen printing paste, screen thermal transfer paste or inkjet thermal transfer paste.
The technical scheme provided by the application has the beneficial effects that:
1. The printing dye provided by the application contains the microcapsule taking the oxidant as the core material, the shell material of the microcapsule is a double-layer composite structure of the inner SiO 2 layer, the outer SiO 2 layer or the TiO 2 layer, and the oxidant is slowly released from the shell material in the water washing process, so that the printing dye has stronger oxidability, can play a bactericidal role on one hand, and can react with the disperse dye which is easy to undergo photooxidation reaction in the air drying process on the other hand, so that the disperse dye is slowly decomposed and faded;
2. The printing dye is printed on textiles to be used as a printing icon, after a certain number of washing and sun-drying cycles, the printing icon is slowly faded from the primary color A to be colorless or the target color B, when the printing icon is faded or reaches the target color, the life cycle of the textiles can be changed, and the problem of health and health caused by long-time use is avoided;
3. according to the application, the period of fading/color change is controlled by matching microcapsules with different concentrations and different shell material mechanical properties with different disperse dyes, and the color of the printed dye is obviously changed after 30 times of water washing and sun-drying cycles as a printed icon.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of microcapsules prepared according to an embodiment of the present application.
FIG. 2 is an electron micrograph of a microcapsule prepared in example 1 of the present application.
FIG. 3 is a cross-sectional SEM image of printed icons made from the printing dye of example 1 of the present application.
FIG. 4 is a schematic diagram of the print dye of example 1 of the present application after 30 water wash sun cycles are simulated.
FIG. 5 is a schematic diagram showing the discoloration process of the print dye of example 1 of the present application after being formed into print icons, which simulates 30 water-washing sun-drying cycles.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The embodiment of the application provides a photochromic printing dye, which can solve the problem that a color-changing label is easy to fall off when being stuck on a textile in the prior art.
The embodiment of the application provides a preparation method of a photochromic printing dye, which comprises the following steps:
S101, fully dispersing disperse dye in an organic continuous phase by using a high-speed shearing dispersing disc under the condition of room temperature to obtain a disperse dye solution, wherein the disperse dye is indigo dye, anthraquinone dye or triarylmethane dye, the organic continuous phase is any one of ethylene glycol, 1, 2-propylene glycol and glycerol, and the weight ratio of the disperse dye to the organic continuous phase is 1:5-1:15;
And step S102, adding an anti-settling agent into the disperse dye solution at room temperature, fully dissolving, adding microcapsules, and uniformly dispersing to obtain the photochromic printing dye, wherein the mass concentration of the microcapsules in the photochromic printing dye is 2-2%, the anti-settling agent is one or more of organic montmorillonite, polyethylene wax and nonionic surfactant, and the mass concentration of the anti-settling agent in the photochromic printing dye is 1-1%.
In the step S102, the microcapsule is prepared by adding hydrophilic mesoporous nano SiO 2 into an oxidant solution, vacuumizing to completely adsorb the oxidant solution onto nano SiO 2 particles, adding an organic solvent into an emulsifier to fully dissolve the hydrophilic mesoporous nano SiO 2 to obtain an oil phase solution, adding nano SiO 2 particles adsorbing the oxidant solution into the oil phase solution, stirring at a rotating speed of 500-2000 rpm to obtain an emulsion with uniform particle size, adding a shell material solution into the emulsion, adding an alkali solution to adjust the pH value to 7-10, reacting for 5-12 hours at 30-60 ℃, and filtering, washing and drying after the reaction is finished to obtain the microcapsule. The microcapsule has a structure shown in fig. 1, 10 represents a core material oxidizer solution, 20 represents an inner SiO 2 shell material, and 30 represents an outer shell material.
The oxidant is selected from one or more of sodium ferrate, ferrous sulfate, polymeric ferric sulfate, sodium hypochlorite, aluminum trifluoride or periodic acid, the organic solvent is selected from one or more of normal hexane, cyclohexane, toluene, dimethylbenzene and diethyl ether, the emulsifier is selected from one or more of tween-80, polyvinyl alcohol, OP-10, styrene-maleic anhydride copolymer, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate, the shell material is selected from one or more of ethyl orthosilicate, tetrabutyl titanate, KH550, KH560 and KH570, the alkali solution is selected from one of sodium hydroxide, potassium hydroxide, calcium hydroxide and triethanolamine, the mass ratio of the oxidant to deionized water is 0.5-3, the addition amount of the emulsifier is 1-5% of the mass of the oxidant solution, and the addition amount of the shell material is 0.5-2 times of the mass of the oxidant solution.
Example 1:
The microcapsule is prepared by fully dissolving ferrous sulfate in deionized water to obtain a ferrous sulfate solution, wherein the mass ratio of the ferrous sulfate to the deionized water is 1:1, adding hydrophilic mesoporous nano SiO 2 into the ferrous sulfate solution, vacuumizing to fully adsorb the ferrous sulfate solution onto nano SiO 2 particles, wherein the dosage of the hydrophilic mesoporous nano SiO 2 is 20% of the mass of the ferrous sulfate solution, adding an emulsifier OP-10 into n-hexane to fully dissolve the emulsifier OP-10 and obtain an oil phase solution, wherein the dosage of the emulsifier OP-10 is 3% of the mass of the ferrous sulfate solution, adding nano SiO 2 particles adsorbing the ferrous sulfate solution into the oil phase to obtain emulsion with uniform particle size at a rotating speed of 1000rpm, then adding ethyl orthosilicate and KH560 into the emulsion, wherein the mass ratio of the ethyl orthosilicate to KH560 is 3:1, the dosage of the ethyl orthosilicate and KH560 is 1 times of the mass of the ferrous sulfate solution, adding sodium hydroxide to adjust the pH value of the solution to 9, reacting for 8h at 40 ℃, filtering, washing and drying to obtain the microcapsule with uniform particle size, and obtaining the microcapsule with uniform size as shown in a figure 2 of a microcapsule, and a compact size is shown in a figure 2.
The preparation method of the photochromic printing dye comprises the steps of dispersing alkaline violet of the dye in glycerol by adopting a high-speed dispersing machine at room temperature, wherein the mass ratio of the alkaline violet to the glycerol is 1:10, adding organic montmorillonite into a dispersion liquid at room temperature, adding the dispersion liquid into a kneader, adding microcapsules into the dispersion liquid at room temperature, and uniformly dispersing to obtain the photochromic printing dye, wherein the mass concentration of the organic montmorillonite in the photochromic printing dye is 0.3%, and the mass concentration of the microcapsules in the photochromic printing dye is 2%.
The photochromic printing dye prepared in the embodiment 1 is uniformly mixed with the screen printing paste according to the mass ratio of 1:20, screen printing is carried out, the mixture is transferred onto cloth, a sample is obtained by drying, an electron microscope spectrogram of the screen printing sample is shown in fig. 3, and as can be seen from fig. 3, the microcapsules are uniformly dispersed in the paste and have good compatibility with the paste.
The comparative graph of the screen printed sample prepared in example 1 before and after 30 water wash sun cycles is shown in fig. 4 and the color change process is shown in fig. 5. As can be seen from fig. 4 and 5, the screen printed sample changed in color from purple to pale purple after the water washing and sun-drying.
Example 2:
Preparing microcapsules, namely fully dissolving sodium ferrate in deionized water to obtain sodium ferrate solution, wherein the mass ratio of the sodium ferrate to the deionized water is 2:1, adding hydrophilic mesoporous nano SiO 2 into the sodium ferrate solution, vacuumizing to fully adsorb the sodium ferrate solution onto nano SiO 2 particles, wherein the dosage of the hydrophilic mesoporous nano SiO 2 is 25 times of the mass of the sodium ferrate solution, adding Tween-80 into cyclohexane, fully dissolving the Tween-80 as oil phase solution, wherein the dosage of the Tween-80 is 2% of the mass of the sodium ferrate solution, adding nano SiO 2 particles adsorbing the sodium ferrate solution into the oil phase at a rotating speed of 1000rpm to obtain emulsion with uniform particle size, then adding tetrabutyl titanate and KH560 into the emulsion, wherein the mass ratio of the tetrabutyl titanate to the KH560 is 3:1, and the dosage of the tetrabutyl titanate to the KH560 is 0.8 times of the mass of the sodium ferrate solution;
The preparation method of the photochromic printing dye comprises the steps of dispersing the indigo dye in glycerol by adopting a high-speed dispersing machine at room temperature, wherein the mass ratio of the indigo dye to the glycerol is 1:8, adding polyethylene wax into the dispersion liquid at room temperature, adding the dispersion liquid into a kneader, adding microcapsules into the dispersion liquid at room temperature, and uniformly dispersing to obtain the photochromic printing dye, wherein the mass concentration of the polyethylene wax in the photochromic printing dye is 0.5%, and the mass concentration of the microcapsules in the photochromic printing dye is 1%.
The photochromic printing dye prepared in the example 2 and the screen printing paste are uniformly mixed according to the mass ratio of 1:20, screen printing is carried out, the mixture is transferred onto cloth, and the sample is obtained by drying.
The screen printed samples prepared in example 2 were tested by 30 water wash sun cycles and the color changed from an initial violet color to a pink color by linear fade.
Example 3:
Preparing microcapsules, namely fully dissolving sodium hypochlorite into deionized water to obtain a sodium hypochlorite solution, wherein the mass ratio of the sodium hypochlorite to the deionized water is 1.5:1, adding hydrophilic mesoporous nano SiO 2 into the sodium hypochlorite solution, vacuumizing to fully adsorb the sodium hypochlorite solution onto nano SiO 2 particles, wherein the dosage of the hydrophilic mesoporous nano SiO 2 is 20% of the mass of the sodium hypochlorite solution, adding sodium dodecyl sulfate into diethyl ether to fully dissolve the sodium dodecyl sulfate, taking the sodium dodecyl sulfate as an oil phase solution, wherein the dosage of the sodium dodecyl sulfate is 2.5% of the mass of the sodium hypochlorite solution, adding nano SiO 2 particles of the adsorbed sodium hypochlorite solution into the oil phase, obtaining emulsion with uniform particle size at a rotating speed of 1500rpm, then adding KH570 into the emulsion, wherein the dosage of KH570 is 0.5 times of the mass of the sodium hypochlorite solution, adding sodium hydroxide to adjust the pH value of the solution to 9, reacting for 8 hours at 50 ℃, and then filtering, washing and drying to obtain the microcapsules;
The preparation method of the photochromic printing dye comprises the steps of dispersing malachite green in ethylene glycol by adopting a high-speed dispersing machine at room temperature, wherein the mass ratio of the malachite green to the ethylene glycol is 1:8, adding epoxy diacetate POD into a dispersion liquid at room temperature, adding the dispersion liquid into a kneader, adding microcapsules at room temperature, and uniformly dispersing to obtain the photochromic printing dye, wherein the mass concentration of the epoxy diacetate POD in the photochromic printing dye is 0.3%, and the mass concentration of the microcapsules in the photochromic printing dye is 1.2%.
The photochromic printing dye prepared in the example 3 and the screen printing paste are uniformly mixed according to the mass ratio of 1:20, screen printing is carried out, the mixture is transferred onto cloth, and the sample is obtained by drying.
The screen printed samples prepared in example 3 were tested by 30 water wash sun cycles and the color changed from green to pale yellow by linear fade.
Example 4:
Preparing microcapsules, namely fully dissolving periodic acid in deionized water to obtain a periodic acid solution, wherein the mass ratio of periodic acid to deionized water is 1:1, adding hydrophilic mesoporous nano SiO 2 into the periodic acid solution, vacuumizing to fully adsorb the periodic acid solution onto nano SiO 2 particles, adding sodium dodecyl benzene sulfonate into n-hexane to fully dissolve the sodium dodecyl benzene sulfonate, wherein the adding amount of the sodium dodecyl benzene sulfonate is 3% of the mass of the periodic acid solution, adding nano SiO 2 particles adsorbing the periodic acid solution into the oil phase, obtaining emulsion with uniform particle size at the rotating speed of 1000rpm, then adding KH550 into the emulsion, wherein the adding amount of KH550 is 1 time of the mass of the periodic acid solution, adding potassium hydroxide to adjust the pH value of the solution to 9, reacting for 8 hours at 55 ℃, and then filtering, washing and drying to obtain the microcapsules;
The preparation method of the photochromic printing dye comprises the steps of dispersing dye fuchsin in glycerol by a high-speed dispersing machine at room temperature, wherein the mass ratio of fuchsin to glycerol is 1:12, adding organic montmorillonite into the dispersion liquid at room temperature, adding the dispersion liquid into a kneader, adding microcapsules at room temperature, and dispersing uniformly to obtain the photochromic printing dye, wherein the mass concentration of the organic montmorillonite in the photochromic printing dye is 0.6%, and the mass concentration of the microcapsules in the photochromic printing dye is 5 per mill.
The photochromic printing dye prepared in the example 4 is uniformly mixed with the screen printing paste according to the mass ratio of 1:20, screen printing is carried out, the mixture is transferred onto cloth, and the sample is obtained by drying.
The screen printed sample prepared in example 4 was tested by 30 water wash sun cycles and the color was linearly discoloured from red to pale yellow.
Example 5:
Preparing microcapsules, namely fully dissolving polymeric ferric sulfate into deionized water to obtain a polymeric ferric sulfate solution, wherein the mass ratio of the polymeric ferric sulfate to the deionized water is 2:1, adding hydrophilic mesoporous nano SiO 2 into the polymeric ferric sulfate solution, vacuumizing to fully adsorb the polymeric ferric sulfate solution onto nano SiO 2 particles, wherein the dosage of the hydrophilic mesoporous nano SiO 2 is 15% of the mass of the polymeric ferric sulfate solution, adding an emulsifier OP-10 into n-hexane to fully dissolve the emulsifier OP-10 and obtain an oil phase solution, wherein the adding amount of the emulsifier OP-10 is 3.5% of the mass of the polymeric ferric sulfate solution, adding nano SiO 2 particles for adsorbing the polymeric ferric sulfate solution into the oil phase to obtain an emulsion with uniform particle size at 1800rpm, then adding ethyl orthosilicate and KH570 into the emulsion, wherein the mass ratio of the ethyl orthosilicate to KH570 is 3:1, the adding amount of the ethyl orthosilicate to KH570 is 1.2 times of the mass of the polymeric ferric sulfate solution, adding triethanolamine to adjust the pH value of the solution to 9, reacting at 60 ℃ for 8 hours, and then filtering, washing and drying to obtain the microcapsules;
The photochromic printing dye is prepared by dispersing dye methyl violet in 1, 2-propylene glycol by a high-speed dispersing machine at room temperature, wherein the mass ratio of the methyl violet to the 1, 2-propylene glycol is 1:15, adding polyethylene wax into a dispersion liquid at room temperature, adding the dispersion liquid into a kneader, adding microcapsules at room temperature, and uniformly dispersing to obtain the photochromic printing dye, wherein the mass concentration of the polyethylene wax in the photochromic printing dye is 8 per mill, and the mass concentration of the microcapsules in the photochromic printing dye is 1.5 percent.
The photochromic printing dye prepared in the example 5 is uniformly mixed with the screen printing paste according to the mass ratio of 1:20, screen printing is carried out, the mixture is transferred onto cloth, and the sample is obtained by drying.
The screen printed sample prepared in example 5 was tested for a linear fade from violet to light pink in color by 30 water wash sun cycles.
In the description of the present specification, reference to the terms "one embodiment/manner," "some embodiments/manner," "example," "a particular example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment/manner or example is included in at least one embodiment/manner or example of the application. In this specification, the schematic representations of the above terms are not necessarily for the same embodiment/manner or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/modes or examples described in this specification and the features of the various embodiments/modes or examples can be combined and combined by persons skilled in the art without contradiction.
It should be noted that in the present application, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises an element. In the present application, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically specified otherwise.
The foregoing is only a specific embodiment of the application to enable those skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The photochromic printing dye is characterized by being obtained by dispersing a disperse dye and a microcapsule in an organic continuous phase, wherein the disperse dye is anthraquinone dye, a core material of the microcapsule is an oxidant, the oxidant is any one of sodium ferrate, sodium hypochlorite or periodic acid, and a shell material of the microcapsule is SiO 2 compound.
2. A photochromic printing dye according to claim 1, wherein the organic continuous phase is any one of ethylene glycol, 1, 2-propanediol, glycerol.
3. The photochromic printing dye according to claim 1, wherein the weight ratio of the disperse dye to the organic continuous phase is 1:5-1:15, and the mass concentration of the microcapsules in the photochromic printing dye is 2 per mill-2%.
4. A process for the preparation of a photochromic printing dye according to claim 1, characterized in that it comprises the following steps:
s101, fully dispersing disperse dye in an organic continuous phase under the condition of room temperature to obtain a disperse dye solution;
S102, adding an anti-settling agent into the disperse dye solution at room temperature, fully dissolving, then adding microcapsules, and uniformly dispersing to obtain the photochromic printing dye.
5. The method of preparing a photochromic printing dye according to claim 4, wherein the microcapsules are prepared by the following process:
Adding hydrophilic mesoporous nano SiO 2 into an oxidant solution, and vacuumizing to completely adsorb the oxidant solution onto nano SiO 2 particles;
adding an organic solvent into an emulsifier for full dissolution to obtain an oil phase solution;
Adding nano SiO 2 particles for adsorbing an oxidant solution into the oil phase solution, and stirring to obtain emulsion with uniform particle size;
And adding the shell material solution into the emulsion, adding an alkali solution to adjust the pH value to 7-10, reacting at 30-60 ℃, filtering, washing and drying after the reaction is finished, thus obtaining the microcapsule.
6. The method for preparing photochromic printing dye according to claim 5, wherein the organic solvent is one or more of n-hexane, cyclohexane, toluene, xylene and diethyl ether, and the emulsifier is one or more of tween-80, polyvinyl alcohol, OP-10, styrene-maleic anhydride copolymer, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
7. The method for preparing a photochromic printing dye according to claim 5, wherein the shell material solution is a mixture of one or more of tetraethoxysilane, tetrabutyl titanate, KH550, KH560 and KH570, and the alkali solution is any one of sodium hydroxide, potassium hydroxide, calcium hydroxide and triethanolamine.
8. The method for preparing photochromic printing dye according to claim 5, wherein the addition amount of the emulsifier is 1% -5% of the mass of the oxidant solution, and the addition amount of the shell material is 0.5-2 times of the mass of the oxidant solution.
9. The preparation method of the photochromic printing dye according to claim 4, wherein the anti-settling agent is one or a mixture of more of organic montmorillonite, polyethylene wax and nonionic surfactant, and the mass concentration of the anti-settling agent in the photochromic printing dye is 1-1%.
10. The photochromic printing dye prepared by the preparation method of any one of claims 4 to 9 is added into a screen printing paste, a screen thermal transfer paste or an inkjet thermal transfer paste for printing textiles.
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| CN104010825A (en) * | 2011-12-31 | 2014-08-27 | 桑福德有限合伙人公司 | Irreversible thermochromic ink compositions |
| CN104024350A (en) * | 2011-12-31 | 2014-09-03 | 桑福德有限合伙人公司 | Irreversible thermochromic ink compositions |
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| US8865621B2 (en) * | 2012-08-06 | 2014-10-21 | Sanford, L.P. | Irreversible color changing ink compositions |
| CN104624125B (en) * | 2013-11-11 | 2018-03-02 | 中国人民银行印制科学技术研究所 | A kind of Photochromic double-shell microcapsule and its preparation method and application |
| US11359137B2 (en) * | 2017-05-03 | 2022-06-14 | University Of South Florida | Microencapsulated thermochromic materials and uses thereof |
| CN111393895A (en) * | 2020-04-13 | 2020-07-10 | 探路者控股集团股份有限公司 | Long-acting optical variable powder and preparation method and application thereof |
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| CN104024350A (en) * | 2011-12-31 | 2014-09-03 | 桑福德有限合伙人公司 | Irreversible thermochromic ink compositions |
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