Preparation method of multi-color variable and luminous multifunctional polyester fabric of variable blue tone fabric

By combining spiropyran-naphthalimide fluorescent compounds with B-354 disperse dyes, a multifunctional polyester fabric was prepared, which solved the problems of single color and insufficient fluorescence of photochromic fabrics, achieved multi-color color-changing and excellent luminous performance of polyester fabrics, and broadened its application range.

CN120683734APending Publication Date: 2025-09-23JIAXING XINGCHANG DYEING & PRINTING CO LTD
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Patent Information

Application Number
CN202511030668.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-25
Publication Date
2025-09-23

AI Technical Summary

Technical Problem

Existing photochromic fabrics have a single color change, insufficient fluorescence performance, and it is difficult to combine functional molecules with commercial dyes.

Method used

Spiropyran-naphthalimide fluorescent compound was combined with B-354 disperse dye to prepare liquid disperse dye through emulsification-solvent evaporation technology. The dye was then impregnated into polyester fabric under high temperature and high pressure under weak acidic conditions, and a reduction cleaning step was combined to prepare multifunctional polyester fabric.

Benefits of technology

A multifunctional polyester fabric with variable blue tones, multi-color discoloration and luminescence was prepared. It has a blue tone composite color change effect, excellent luminescence performance, multiple response functions and good stability, which broadens the application of high-end textiles and smart materials.

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Abstract

The invention discloses a preparation method of a multi-color variable and luminous multifunctional polyester fabric of a variable blue tone fabric. The method comprises the following core steps: (1) forming a composition from a spiropyrane-naphthalimide functional fluorescent compound and a B-354 disperse dye by adopting an emulsification-solvent evaporation technology; (2) applying the prepared liquid disperse dye composition to a polyester fabric through a high-temperature and high-pressure dip dyeing process; and (3) carrying out necessary post-treatment on the treated fabric. The functional polyester fabric prepared by the method shows fluorescence color change of different backgrounds and multiple characteristics of remarkable photochromism and fluorescence discoloration under the irradiation of ultraviolet light, is quick in photoresponse, has good reversibility and excellent fatigue resistance, and keeps relatively good color fastness at the same time. The technology provides a new way for developing multifunctional multi-color intelligent luminous textiles, high-technical-content anti-counterfeiting mark textiles, personalized fashion clothes and other textiles, and has important application prospects.
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Description

Technical Field

[0001] The present invention belongs to the technical field of functional textile material preparation, and in particular relates to a method for preparing a multifunctional polyester fabric with variable blue tone, multi-color change and luminescence. Background Art

[0002] With technological advancements and improvements in quality of life, consumer demand for clothing and textiles has shifted from basic aesthetics and practicality to functionality, personalization, and intelligence. Photochromic and luminescent textiles, owing to their unique visual effects and potential for intelligent interaction, have become a hot topic for research and development. Spiropyran compounds, a classic class of photochromic materials, exhibit broad application prospects in optical sensing, biomedicine, and smart textiles due to their reversible isomerization reaction upon UV irradiation, resulting in color changes.

[0003] However, the photochromic fabrics prepared based on traditional spiropyran compounds in the prior art face many challenges: (1) Single color change: Most spiropyran photochromic fabrics mainly show a transition from colorless or light color to a single dark color (such as purple). The color types and change patterns are relatively limited, which makes it difficult to meet the demand for rich colors in fashion design.

[0004] (2) Insufficient fluorescence performance: Ordinary spiropyran compounds often have weak fluorescence or only a single fluorescent color, which limits their application in luminescent color-changing fabrics and multiple anti-counterfeiting fields. Even if some spiropyran compounds can produce fluorescence after ring opening, their intensity and stability are often unsatisfactory. Summary of the Invention

[0005] The present invention aims to solve the problems of single color, insufficient fluorescence performance, and difficulty in compounding functional molecules with commercial dyes in the prior art of photochromic fabrics. Spiropyran-naphthalimide fluorescent compounds are combined with B-354 disperse dyes to prepare color-changing and luminescent polyester fabrics with a blue-toned composite color change effect, excellent luminescence performance, multiple response functions, and good stability. At the same time, good printing and dyeing performance is guaranteed, breaking through the limitation of the single color change of existing photochromic fabrics and broadening their application in the fields of high-end textiles and smart materials.

[0006] The technical solution adopted by the present invention to solve the technical problem is: a method for preparing a multifunctional polyester fabric with variable blue tone, multi-color change and luminescence, comprising the following steps: 1) Providing a spiropyran-naphthalimide fluorescent compound, combining it with B-354 disperse dye to form a disperse dye composition, mixing it with an auxiliary agent, and preparing it into a liquid disperse dye using an emulsification-solvent evaporation technique; 2) applying the liquid disperse dye described in step 1) to the polyester fabric through a dyeing process, wherein the dyeing process is to perform high-temperature and high-pressure impregnation dyeing on the polyester fabric under weakly acidic conditions (preferably pH 4-5) at a temperature of 120-140° C. (preferably 130° C.); 3) performing post-treatment on the polyester fabric treated in step 2), wherein the post-treatment includes reduction cleaning and / or soaping steps to remove floating colors and improve color fastness.

[0007] Furthermore, the spiropyran-naphthalimide fluorescent compound in step 1) is specifically compound NA-SP, and its structural formula is as follows: .

[0008] Furthermore, when the liquid disperse dye is prepared by the emulsification-solvent evaporation technology in step 1), the oil phase contains the spiropyran-naphthalimide fluorescent compound (such as NA-SP), B-354 disperse dye, an organic solvent, and an emulsifier and / or a stabilizer; the aqueous phase contains an emulsifier and / or a protective colloid (such as sodium carboxymethyl cellulose) and water.

[0009] Furthermore, the preparation process of the liquid disperse dye comprises: a. The spiropyran - naphthalimide fluorescent compound, B-354 disperse dye, an organic solvent, and an emulsifier and / or stabilizer are uniformly mixed and dissolved by ultrasound as the oil phase; b. Mix the emulsifier and water evenly and dissolve them by ultrasonication to form the aqueous phase; c. Using an emulsifier, slowly add the oil phase dropwise to the water phase while stirring at low speed. After the addition is complete, increase the speed of the emulsifier to 10,000 r / min and emulsify at high speed in an ice bath for 20 minutes to obtain a uniform and stable oil-in-water (O / W) disperse dye pre-emulsion. d. The pre-emulsion in step c was subjected to a rotary evaporator to remove the organic solvent to obtain a liquid disperse dye mixed with a spiropyran naphthyl imide fluorescent compound and B-354 disperse dye.

[0010] Furthermore, the organic solvent is selected from one of dichloroethane, dichloromethane, toluene, ethyl acetate or a mixture thereof; the emulsifier in the oil phase includes one or two of Tween 20 and Tween 80; the emulsifier in the aqueous phase includes one or more of sodium dodecyl sulfate (SDS), Tween 20, and Tween 80; and the stabilizer can be selected from one or two of dodecanol and tetradecanol.

[0011] Furthermore, in the dyeing process, the amount of disperse dye used is 0.5% to 5.0% (owm) of the fabric weight, the dyeing bath ratio is 1:10, the dyeing temperature is 120-140°C (preferably 130°C), and the holding time is 45 to 75 minutes (preferably 60 minutes).

[0012] Furthermore, in the post-dyeing treatment process, the reduction cleaning solution contains 2.0 g / L sodium hydroxide, 2.0 g / L hydrosulfite, and 2.0 g / L soap flakes, with a bath ratio of 1:30, a reduction cleaning temperature of 85° C., a holding time of 15 minutes, and then cold water washing and drying.

[0013] In addition, the present invention also discloses a photochromic luminescent functional polyester fabric prepared by the above method.

[0014] The blue-toned photochromic luminescent fabric prepared by the above method undergoes an observable color change under irradiation with ultraviolet light of a specific wavelength (such as 365nm), and its fluorescence emission color or intensity changes; this color and fluorescence change can be reversed when the ultraviolet light source is removed and placed under visible light.

[0015] The beneficial effects of the present invention are as follows: compared with the prior art, the preparation method of a multifunctional polyester fabric with variable blue tone fabric, multi-color change and luminescence provided by the present invention has the following advantages: (1) A technology was developed to combine spiropyran-naphthalimide color-changing fluorescent functional molecules with B-354 disperse dye to prepare liquid disperse dye, ensuring that the dye has good particle size distribution, dispersion stability and storage stability.

[0016] (2) A multifunctional polyester fabric with variable blue tones, multi-color discoloration and luminescence was prepared. It has the advantages of blue tones, composite color change effect, excellent luminescence performance, multiple response functions, and good stability. Under ultraviolet light irradiation, it obtains a blue appearance gradient color and a red fluorescent gradient color, and the appearance color and fluorescent color change every moment. A variable blue multi-color fluorescent color-changing functional textile fabric was obtained, which has a fast light response, good reversibility and excellent fatigue resistance, while maintaining good color fastness. It overcomes the defects of traditional photochromic fabrics with large color and single response signal, and gives polyester fabrics dual light response characteristics that can be dynamically adjusted, broadening its application in the fields of high-end textiles and smart materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 The apparent color and fluorescence changes of NA-SP / B-354 dyed polyester fabric under UV and visible light.

[0018] Figure 2CIE 1931 chromaticity diagram of apparent color and fluorescence changes of NA-SP / B-354 dyed polyester fabric.

[0019] Figure 3 Changes in (a) K / S value and (b) maximum fluorescence emission wavelength of NA-SP / B-354 dyed polyester fabric under cyclic irradiation of UV and visible light. DETAILED DESCRIPTION

[0020] The present invention will be further described below by way of specific examples, which are only intended to illustrate the present invention and are not intended to limit the scope of the present invention.

[0021] Example 1 Dissolve 2.0 g of NA-SP, 0.5 g of B-354 disperse dye, 0.5 g of dodecanol, 0.5 g of tetradecanol, and 0.2 g of Tween-20 in 15 g of ethylene dichloride. Ultrasonicate until the dye and auxiliaries are completely dissolved, which serves as the oil phase. Weigh 0.1 g of sodium lauryl sulfate, 0.15 g of Tween 80, and 0.1 g of CMC in 20 g of deionized water and ultrasonicate until fully dissolved, which serves as the aqueous phase. Using an emulsifier, slowly add the oil phase dropwise to the aqueous phase under low-speed stirring. After the addition is complete, increase the speed of the emulsifier to 10,000 rpm and emulsify at high speed in an ice bath for 20 min to obtain a uniform and stable oil-in-water (O / W) disperse dye pre-emulsion. Add 0.1 g of defoamer to the pre-emulsion, shake well, and then remove the ethylene dichloride from the pre-emulsion on a rotary evaporator to obtain a liquid disperse dye. DLS analysis showed an average particle size of 424.1 nm, a PDI value of 0.313, and a uniform particle size distribution. After stable storage for one month, the particle size showed no significant change.

[0022] Example 2 2.0 g of NA-SP, 0.3 g of commercial disperse dye B-354, 0.5 g of dodecanol, 0.5 g of tetradecanol, and 0.1 g of Tween-20 were dissolved in 15 g of ethylene dichloride and sonicated until the dye and auxiliaries were completely dissolved, which served as the oil phase. 0.1 g of sodium lauryl sulfate, 0.3 g of Tween 80, and 0.1 g of CMC were weighed and dissolved in 20 g of deionized water and sonicated until fully dissolved, which served as the aqueous phase. Using an emulsifier, the oil phase was slowly added dropwise to the aqueous phase under low-speed stirring. After the addition was complete, the speed of the emulsifier was increased to 10,000 rpm and high-speed emulsification was performed in an ice bath for 20 min to obtain a uniform and stable oil-in-water (O / W) disperse dye pre-emulsion. 0.1 g of defoamer was added to the pre-emulsion and shaken to mix well. The pre-emulsion was then subjected to a rotary evaporator to remove the ethylene dichloride, yielding the NA-SP / B-354 liquid disperse dye. DLS analysis showed an average particle size of 358.2 nm, a PDI value of 0.268, and a uniform particle size distribution. After stable storage for one month, the particle size showed no significant change.

[0023] Example 3 The liquid disperse dye obtained in Example 1 was diluted to 5 g / L and used for dyeing polyester fabric. The liquid disperse dye was used in an amount of 2% (owm) of the fabric weight, the dye bath ratio was 1:10, the dyeing temperature was 130° C., and the heat preservation time was 60 minutes. After dyeing, a reduction cleaning solution was performed, the reduction cleaning solution comprising 2.0 g / L sodium hydroxide, 2.0 g / L hydrosulfite, and 2.0 g / L soap flakes, the bath ratio was 1:30, the reduction cleaning temperature was 85° C., the heat preservation time was 15 minutes, and the fabric was then rinsed with cold water and dried to obtain a polyester fabric dyed with the liquid disperse dye.

[0024] Example 4 The polyester fabric dyed with the liquid disperse dye in Example 3 was placed under ultraviolet light and visible light, and its color change and fluorescence change at different irradiation times were recorded. The results are as follows: Figure 1 As shown in Figure 2, under UV light, the fabric's apparent color changes from cyan, light blue, to dark blue, while its fluorescent color changes from an initial light green to orange, pink, and finally to bright red. Under visible light, both the fabric's apparent color and fluorescence return to their initial state.

[0025] Example 5 The NA-SP / B-354 liquid disperse dye obtained in Example 1 was diluted to 2 g / L and used for polyester fabric dyeing. The liquid disperse dye was used in an amount of 2% (owm) of the fabric weight, the dyeing bath ratio was 1:10, the dyeing temperature was 130°C, and the heat preservation time was 60 minutes. After dyeing, reduction cleaning was performed, the reduction cleaning solution contained 2.0 g / L sodium hydroxide, 2.0 g / L hydrosulfite, and 2.0 g / L soap flakes, the bath ratio was 1:30, the reduction cleaning temperature was 85°C, the heat preservation time was 15 minutes, and then the fabric was rinsed with cold water and dried to obtain polyester fabric dyed with NA-SP / B-354 liquid disperse dye.

[0026] Example 6 The polyester fabric dyed with NA-SP / B-354 liquid disperse dye in Example 5 was placed under ultraviolet light and visible light, and its color change and fluorescence change at different irradiation times were recorded. The results are as follows: Figure 2 As shown in Figure 2, under UV light, the fabric's apparent color changes from cyan, light blue, to dark blue, and its fluorescent color changes from light green, through orange, pink, and finally bright red. Under visible light, both the fabric's apparent color and fluorescence return to their initial state.

[0027] Example 7 In order to explore the fatigue resistance of photochromic luminescent polyester fabric, the polyester fabric in Example 3 was irradiated 10 times under ultraviolet light and visible light, and the changes in the K / S value and the maximum fluorescence emission wavelength at 560 nm before and after irradiation were tested. The results are as follows: Figure 3 The results show that after 10 cycles of alternating UV / visible light irradiation, the apparent color depth and fluorescence intensity of polyester fabric dyed with NA-SP / B-354 liquid disperse dye did not show significant fluctuations, indicating that the light-responsive color-changing and luminescent functional fabric of the present invention has excellent fatigue resistance.

[0028] A blue appearance gradient color and a red fluorescent gradient color are obtained. Under ultraviolet light, the appearance color and the fluorescent color change every moment, obtaining a variable blue multi-color fluorescent color-changing functional textile.

[0029] The above embodiments are only used to illustrate the present invention, and are not intended to limit the present invention. Ordinary technicians in the relevant technical field may make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, all equivalent technical solutions also fall within the scope of the present invention. The scope of patent protection of the present invention should be defined by the claims.

Claims

1. A method for preparing a multifunctional polyester fabric with variable blue tone, multi-color change and luminescence, characterized in that: The following steps are involved: 1) Providing a spiropyran-naphthalimide fluorescent compound to form a composition with B-354 disperse dye, and preparing the liquid disperse dye using an emulsification-solvent evaporation technique; 2) applying the liquid disperse dye described in step 1) to the polyester fabric through a dyeing process, wherein the dyeing process is to perform high-temperature and high-pressure impregnation dyeing on the polyester fabric under weakly acidic conditions at a temperature of 120-140° C.; 3) performing post-treatment on the polyester fabric treated in step 2), wherein the post-treatment includes reduction cleaning and / or soaping steps to remove floating colors and improve color fastness.

2. The method for preparing a multifunctional polyester fabric with variable blue tone and multi-color color change and luminescence according to claim 1, characterized in that: In the step 1), the spiropyran-naphthalimide fluorescent compound is specifically a compound NA-SP, and its structural formula is as follows: 。 3. The method for preparing a multifunctional polyester fabric with variable blue tone and multi-color color change and luminescence according to claim 1, characterized in that: When the liquid disperse dye is prepared by the emulsification-solvent evaporation technology in step 1), the oil phase contains the spiropyran-naphthalimide fluorescent compound, the B-354 disperse dye composition, an organic solvent, and an emulsifier and / or a stabilizer; the aqueous phase contains an emulsifier and / or a protective colloid and water.

4. The method for preparing a multifunctional polyester fabric with variable blue tones and multi-color color change and luminescence according to claim 3, characterized in that: The preparation process of the liquid disperse dye comprises: a spiropyran - naphthalimide fluorescent compound, B-354, an organic solvent and an emulsifier and / or stabilizer are mixed and dissolved by ultrasound as the oil phase; b. Mix the emulsifier and water evenly and dissolve by ultrasonication as the aqueous phase; c. Using an emulsifier, slowly add the oil phase dropwise to the water phase while stirring at low speed. After the addition is complete, increase the speed of the emulsifier to 10,000 r / min and emulsify at high speed in an ice bath for 20 minutes to obtain a uniform and stable oil-in-water (O / W) disperse dye pre-emulsion. d. The organic solvent is removed from the pre-emulsion in step c to obtain a liquid disperse dye composition of a spiropyran naphthyl imide fluorescent compound mixed with B-354 disperse dye.

5. The method for preparing a multifunctional polyester fabric with variable blue tones and multi-color color change and luminescence according to claim 4, wherein in step a, the organic solvent is selected from one or a mixture of dichloroethane, dichloromethane, toluene, and ethyl acetate; the emulsifier in the oil phase includes one or both of Tween 20 and Tween 80; the emulsifier in the aqueous phase includes one or more of sodium dodecyl sulfate (SDS), Tween 20, and Tween 80; and the stabilizer is selected from one or both of dodecanol and tetradecanol.

6. The method for preparing a multifunctional polyester fabric with variable blue tones and multi-color color change and luminescence according to claim 1, characterized in that: In the step 2) dyeing process, the amount of disperse dye used is 0.5% to 5.0% (owm) of the fabric weight, the dye bath ratio is 1:10, the dyeing temperature is 120-140° C., and the holding time is 45 to 75 minutes.

7. The method for preparing a multifunctional polyester fabric with variable blue tones and multi-color color change and luminescence according to claim 1, characterized in that: In the step 3) post-dyeing treatment process, the reduction cleaning solution contains 2.0 g / L sodium hydroxide, 2.0 g / L hydrosulfite, and 2.0 g / L soap flakes, with a bath ratio of 1:

30. The reduction cleaning temperature is 85° C., the holding time is 15 minutes, and then the product is washed with cold water and dried.

8. A blue-toned photochromic luminescent polyester fabric prepared by the method according to any one of claims 1 to 7.

9. The blue-toned photochromic luminescent polyester fabric according to claim 8, characterized in that: The fabric undergoes an observable color change when irradiated with ultraviolet light of a specific wavelength, and its fluorescence emission color or intensity changes; the color and fluorescence changes can be reversed after removing the ultraviolet light source and placing it under visible light.