A method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur doped carbon dots
By using citric acid and thiourea as raw materials, combined with dialysis removal and hydrazine hydrate reduction protection methods, nitrogen-sulfur-doped carbon dots with stable emission and a full range of colors were prepared, which solved the problems of complexity and low efficiency of traditional methods and realized the application of anti-counterfeiting textiles with high fluorescence quantum yield and significant spectral characteristics.
Patent Information
- Application Number
- CN202311423394.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-31
- Publication Date
- 2025-09-23
- Estimated Expiration
- 2043-10-31
AI Technical Summary
Existing technologies make it difficult to efficiently prepare stable and reliable full-color carbon dots, especially green, yellow and red carbon dots. Traditional methods are complex to operate, have low separation efficiency, and low fluorescence quantum yield, making them difficult to apply to anti-counterfeiting textiles.
Citric acid and thiourea are used as raw materials, combined with solvents of different polarities to prepare nitrogen-sulfur doped carbon dot mother liquor. Through dialysis to remove impurities and hydrazine hydrate reduction protection, a full-color carbon dot solution emitting blue, green, yellow and red light is obtained, and anti-counterfeiting textiles are prepared with adhesives.
A simple and efficient full-color carbon dot preparation was achieved with uniform particle size, high fluorescence quantum yield, suitable for a variety of textiles, significant spectral characteristics and good dispersibility, and applied to anti-counterfeiting textiles.
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Abstract
Description
Technical Field
[0001] The invention relates to a method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur doped carbon dots, belonging to the technical field of functional textiles. Background Art
[0002] With the development of society and the advancement of science and technology, the general public has put forward higher requirements for the functionality of textiles, requiring textile fabrics to be not only beautiful in appearance and comfortable to wear, but also to have specific functionality. At present, anti-counterfeiting labels for textiles refer to auxiliary materials that have information encryption and anti-counterfeiting effects under specific conditions, specifically including anti-counterfeiting trademarks, anti-counterfeiting tags and other series of products. Most of the above-mentioned anti-counterfeiting labels are connected to textiles by sewing or nailing, and there is a problem of easy falling off during transportation or use. In recent years, with the development of anti-counterfeiting technology for identification patterns, the use of various new anti-counterfeiting materials including luminous particles and carbon quantum dots (abbreviated as: carbon dots) has gained attention. By preparing high-efficiency anti-counterfeiting nanomaterials and combining modern weaving technology and functional finishing processes, it is possible to achieve encryption of pattern or text information in specific parts of textiles, and construct new anti-counterfeiting textiles based on sunlight invisibility, excitation color change or interference color change effects.
[0003] As a new type of luminescent nanomaterials, carbon dots contain abundant polar groups on their surface and have many characteristics such as good optical stability, high brightness and adjustable emission wavelength. In addition, they have excellent biocompatibility and have potential application prospects in many fields such as information anti-counterfeiting and material sensing. In recent years, great progress has been made in the synthesis and luminescence mechanism research of carbon dots with fluorescence emission function, and their application in the field of anti-counterfeiting materials has gradually been realized. Among the many preparation methods, the hydrothermal solvent method has many advantages such as high carbon dot yield and stable performance, making it the first choice for researchers to prepare full-color carbon dots. By adjusting the process conditions such as different precursor compositions, synthesis temperature and time, carbon dots with multi-color emission effects can be obtained.
[0004] Although the hydrothermal method is relatively easy to synthesize carbon dots, the light emitted by the carbon dots produced by this method after excitation is mostly concentrated in the short-wavelength blue light region, making it difficult to obtain carbon dots that emit green, yellow, and red light with high intensity and wavelengths between 500-700nm. To obtain carbon dots that emit green, yellow, and red spectra, some researchers have used citric acid and urea as carbon and nitrogen sources, and organic solvents (such as N,N-dimethylformamide) instead of water as the medium for high-temperature synthesis. The synthesized carbon dots can emit a blue / green mixed light or a blue / green / yellow / red four-color mixed light after excitation. However, when stable monochromatic green, yellow, or red carbon dots are required, the carbon dot solution must be separated by silica column chromatography or anion exchange column. This process is not only complex and time-consuming, but also has low efficiency and extremely low fluorescence quantum yield. If the eluent type is not properly selected or the elution time is not accurately controlled, it is even more difficult to obtain monochromatic carbon dots with characteristic wavelengths of blue, green, yellow, and red light.
[0005] Therefore, it is urgent to develop a stable and reliable method for preparing carbon dots with high fluorescence quantum yield and covering four stable emission colors of blue, green, yellow and red, which can be used to process a series of materials that require information encryption, including anti-counterfeiting textiles. Summary of the Invention
[0006] Purpose of the invention: In view of the problems that carbon dots synthesized by the traditional hydrothermal solvent method have low fluorescence quantum yield, unremarkable emission light chromatographic characteristics, and poor effect when applied to anti-counterfeiting textiles, the purpose of the present invention is to provide a method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur doped carbon dots. The present invention uses citric acid as the carbon source, combines small molecule doping containing nitrogen and sulfur elements, and adopts solvents of different polarities as the synthesis medium to prepare nitrogen-sulfur doped full-color carbon dots with high fluorescence quantum yield and remarkable emission light chromatographic characteristics; on this basis, the luminescent carbon dots are further applied to the preparation of anti-counterfeiting textiles.
[0007] The technical solution of the present invention is a method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur-doped carbon dots, which is characterized by: first, using citric acid and thiourea as raw materials, dissolving them in solvents of different polarities to prepare full-color nitrogen-sulfur-doped carbon dot mother liquors that emit blue, green, yellow and red light after excitation; then, dialyzing the prepared carbon dot mother liquors to remove impurities, and adding hydrazine hydrate aqueous solution for reduction protection to obtain full-color nitrogen-sulfur-doped carbon dot solutions that emit blue, green, yellow and red light; finally, adding adhesives to the carbon dot solutions to prepare aqueous fluids to prepare anti-counterfeiting textiles.
[0008] The above-mentioned method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur doped carbon dots specifically comprises the following steps:
[0009] (1) Preparation of nitrogen-sulfur doped carbon dot mother liquor: Citric acid and thiourea are used as raw materials, a solvent is added to obtain a reaction solution, and high temperature treatment is performed to prepare a carbon dot mother liquor;
[0010] (2) Preparation of nitrogen-sulfur doped carbon dot solution: The carbon dot mother solution prepared in step (1) is dialyzed to remove impurities and then freeze-dried to obtain a lyophilized powder, the lyophilized powder is added to a hydrazine hydrate aqueous solution to obtain a mixed solution, and a reduction protection treatment is performed to prepare a full-color nitrogen-sulfur doped carbon dot solution;
[0011] (3) Preparation of full-color anti-counterfeiting textiles: The full-color nitrogen-sulfur doped carbon dot solution prepared in step (2) is added to an adhesive and / or a thickener to prepare a fluid, and then the fluid is attached to the textile by dipping or scraping to prepare a full-color anti-counterfeiting textile.
[0012] Furthermore, in step (1), the solvent includes one or more of water, glycerol, and N,N-dimethylformamide.
[0013] Specifically, there are four optional solvents in step (1), namely water, glycerol, a mixture of glycerol and N,N-dimethylformamide, and N,N-dimethylformamide.
[0014] Furthermore, the mass ratio of glycerol to N,N-dimethylformamide in the mixed solution is 7:1-5.
[0015] Furthermore, in step (1), the carbon dot mother solution is a nitrogen-sulfur-doped carbon dot mother solution that emits four full-color colors of blue, green, yellow and red after excitation.
[0016] Furthermore, when the solvent in step (1) is water, a full-color nitrogen-sulfur-doped carbon dot mother solution is obtained, which emits blue light after excitation.
[0017] Furthermore, when the solvent in step (1) is glycerol, a full-color nitrogen-sulfur-doped carbon dot mother solution is obtained, which emits green light after excitation.
[0018] Furthermore, when the solvent in step (1) is a mixture of glycerol and N,N-dimethylformamide, a full-color nitrogen-sulfur-doped carbon dot mother solution is obtained, which emits yellow light after excitation.
[0019] Furthermore, when the solvent in step (1) is N,N-dimethylformamide, a full-color nitrogen-sulfur-doped carbon dot mother solution is obtained, which emits red light after excitation.
[0020] Furthermore, in step (1), the concentration of citric acid in the reaction solution is 0.05-0.1 g / L.
[0021] Furthermore, in the reaction solution of step (1), the molar ratio of citric acid to thiourea is 1:3-7.
[0022] Furthermore, the high temperature treatment in step (1) is carried out at 140-160° C. for 4-6 hours.
[0023] Furthermore, in step (2), the dialysis impurity removal refers to using a dialysis bag with a molecular weight cut-off of 1000 Da until the conductivity of the dialysate is less than 4 μS / cm.
[0024] Furthermore, in step (2), the freeze drying is performed at -40 to -30°C for 12 to 14 hours.
[0025] Furthermore, the concentration of the lyophilized powder in the mixed solution in step (2) is 0.5 to 1 g / L.
[0026] Furthermore, in step (2), the concentration of hydrazine hydrate in the mixed solution is 18 to 22 mL / L.
[0027] Furthermore, the treatment temperature of the reduction protection treatment in step (2) is 15-25°C.
[0028] Furthermore, the treatment time of the reduction protection treatment in step (2) is 10 to 14 hours.
[0029] Furthermore, the concentration of nitrogen-sulfur-doped carbon dots in the fluid in step (3) is 0.5-1 g / L.
[0030] Furthermore, the adhesive in the fluid in step (3) is a polyacrylate adhesive.
[0031] Furthermore, the concentration of the binder in the fluid in step (3) is 2-4 g / L.
[0032] Furthermore, the thickener in the fluid in step (3) is a sodium alginate paste with a mass concentration of 3 to 7%.
[0033] Furthermore, the concentration of the thickener in the fluid in step (3) is 1-2 g / L.
[0034] Furthermore, in step (3), the textiles include woven fabrics, knitted fabrics and non-woven fabrics made of cotton, linen, silk, flax, polyester, nylon and viscose.
[0035] Furthermore, in step (3), when the dipping method is used, no thickener is added to the fluid, and the preparation operation is to dip at 50-60°C for 15-20 minutes and then bake at 120-130°C for 1-2 minutes.
[0036] Furthermore, in step (3), when using the scraping method, a thickener is added to the fluid, and the preparation operation is to use a screen scraping method and then bake at 120-130° C. for 1 to 3 minutes.
[0037] The present invention provides full-color anti-counterfeiting textiles prepared by the method.
[0038] The full-color anti-counterfeiting textile provided by the present invention is used in the fields of security encryption and special protective clothing.
[0039] Beneficial effects of the present invention:
[0040] The present invention first uses citric acid and thiourea as raw materials, dissolving them in solvents of different polarities to prepare a full range of nitrogen-sulfur-doped carbon dot mother liquors that emit blue, green, yellow, and red light upon excitation. The prepared carbon dot mother liquors are then dialyzed to remove impurities and reduced with hydrazine hydrate aqueous solution to obtain a full range of nitrogen-sulfur-doped carbon dot solutions. Finally, a binder is added to the carbon dot solutions to prepare fluids, and full-color anti-counterfeiting textiles are prepared by dipping or doctoring. Compared to the traditional hydrothermal method, which first synthesizes a multi-color carbon dot mixture and then elutes and separates the mixture using column separation technology to obtain blue, green, yellow, and red carbon dots, the present invention has the following advantages:
[0041] (1) The preparation method of carbon dots is simple: under the conditions of citric acid and thiourea as precursors, by adjusting the solvent polarity of the dissolving medium system, nitrogen-sulfur-doped carbon dots emitting a full range of blue, green, yellow and red light can be obtained, eliminating the defect of low efficiency of elution and separation of traditional multi-color luminescent carbon dot mixed liquid columns, and having the advantages of simple and efficient method.
[0042] (2) Significant characteristic spectra: The prepared carbon dots have small particle size and uniform distribution (average 2-4 nm) and have excellent dispersibility in aqueous phase; after the nitrogen-sulfur doped carbon dot mother liquor is dialyzed, freeze-dried and reduced to protect, four types of luminescent carbon dots with emission wavelengths between 453 and 626 nm, namely blue, green, yellow and red, are obtained, which avoids the problem of incomplete chromatograms or unclear characteristic colors of the blue, green, yellow and red carbon dots obtained by column elution separation of traditional multi-color luminescent carbon dot mixtures.
[0043] (3) High fluorescence quantum yield: The carbon dots prepared under nitrogen and sulfur co-doping not only have high fluorescence emission intensity, but also high fluorescence quantum yield. The fluorescence quantum yield of the four colors of carbon dots is between 21% and 38%, which is higher than the yield of carbon dots prepared by other synthetic methods reported previously.
[0044] (4) Strong universal application: The full-color nitrogen-sulfur doped fluorescent carbon dots prepared by the method of the present invention have good dispersibility in aqueous solution, can be applied to the preparation of a variety of anti-counterfeiting textiles, and have stable application performance. DETAILED DESCRIPTION
[0045] The technical solutions of the present invention are further described in detail below through specific examples. However, it is necessary to point out that the following examples are only used to describe the content of the invention and do not constitute a limitation on the scope of protection of the present invention.
[0046] Source of raw materials
[0047] The adhesive is a polyacrylate adhesive purchased from Zhejiang Satellite Petrochemical; the thickener is a paste prepared from commercially available sodium alginate, the preparation process of which is to dissolve sodium alginate in water and stir it at high speed, with a mass concentration of 5%; hydrazine hydrate was purchased from Aladdin Reagent Co., Ltd.
[0048] Example 1
[0049] A method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur doped carbon dots, the specific steps are as follows:
[0050] (1) Preparation of nitrogen-sulfur doped carbon dot mother liquor: citric acid and thiourea were used as raw materials, and water, glycerol, glycerol and N,N-dimethylformamide mixture, and N,N-dimethylformamide were used as solvent media for treatment at high temperature to prepare four groups of nitrogen-sulfur doped carbon dot mother liquors with blue, green, yellow and red emission colors after excitation; treatment process and conditions: 0.05 g / L citric acid, citric acid: thiourea molar ratio of 1:5, reaction at 160 °C for 6 hours, wherein the mass ratio of glycerol and N,N-dimethylformamide in the mixture was 7:3;
[0051] (2) Preparation of nitrogen-sulfur-doped carbon dot solutions: The four groups of carbon dot mother liquors prepared in step (1) were dialyzed to remove impurities and then freeze-dried to obtain four groups of freeze-dried powders. The four groups of freeze-dried powders were then added to a hydrazine hydrate aqueous solution for reduction protection treatment to prepare a full-color nitrogen-sulfur-doped carbon dot solution that emits blue, green, yellow and red light after excitation, and named B, G, Y and R in sequence; treatment process and conditions: When dialyzing with deionized water to remove impurities, a dialysis bag with a molecular weight cutoff of 1000 Da was used until the dialyzate conductivity was less than 4 μS / cm, and then freeze-dried at -40°C for 12 hours; in the reduction protection treatment, 0.5 g / L of nitrogen-sulfur-doped carbon dots, 20 mL / L of a hydrazine hydrate aqueous solution, a treatment temperature of 20°C, and a treatment time of 12 hours were used;
[0052] (3) Preparation of full-color anti-counterfeiting textiles: The four nitrogen-sulfur-doped carbon dot solutions prepared in step (2) were added to an adhesive to prepare a fluid, and anti-counterfeiting textiles capable of emitting blue light, green light, yellow light, and red light were prepared by immersion, respectively; treatment process and conditions: 0.5 g / L nitrogen-sulfur-doped carbon dots, 2 g / L adhesive, immersion at 60°C for 20 minutes, and then baking at 120°C for 2 minutes; the textiles were cotton woven fabrics.
[0053] Example 2
[0054] The above-mentioned method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur doped carbon dots specifically comprises the following steps:
[0055] (1) Preparation of nitrogen-sulfur doped carbon dot mother liquor: Citric acid and thiourea were used as raw materials, and water, glycerol, glycerol and N,N-dimethylformamide mixture, and N,N-dimethylformamide were used as solvent media for treatment at high temperature to prepare nitrogen-sulfur doped carbon dot mother liquors with a full range of color emission colors of blue, green, yellow and red after excitation; treatment process and conditions: 0.1 g / L citric acid, citric acid: thiourea molar ratio of 1:5, reaction at 160 ° C for 6 hours, wherein the amount ratio of glycerol and N,N-dimethylformamide in the mixture was 7:3;
[0056] (2) Preparation of nitrogen-sulfur-doped carbon dot solution: The carbon dot mother solution prepared in step (1) was dialyzed to remove impurities and then freeze-dried, and then hydrazine hydrate aqueous solution was added for reduction protection treatment to prepare a full-color series of nitrogen-sulfur-doped carbon dot solutions that emit blue light, green light, yellow light and red light after excitation, and named them B, G, Y and R in sequence; treatment process and conditions: when dialyzing with deionized water to remove impurities, a dialysis bag with a molecular weight cutoff of 1000 Da was used until the dialyzate conductivity was less than 4 μS / cm, and then freeze-dried at -40°C; in the reduction protection treatment, 0.5 g / L of nitrogen-sulfur-doped carbon dots, 80 mL / L of hydrazine hydrate aqueous solution, treatment temperature 30°C, and treatment time 24 hours;
[0057] (3) Preparation of full-color anti-counterfeiting textiles: The four nitrogen-sulfur-doped carbon dot solutions prepared in step (2) were added to an adhesive and a thickener to prepare a fluid, and full-color anti-counterfeiting textiles were prepared by scraping; processing process and conditions: 1 g / L nitrogen-sulfur-doped carbon dots, 4 g / L adhesive, 2 g / L thickener, screen scraping and baking at 130°C for 3 minutes; the textile was a silk knitted fabric.
[0058] Comparative Example 1
[0059] In step (1) of Example 1, no thiourea is added, and the other steps and process parameters are the same as those of Example 1.
[0060] Comparative Example 2
[0061] In step (2) of Example 1, no hydrazine hydrate aqueous solution is added, and the other steps and process parameters are the same as those of Example 1.
[0062] Comparative Example 3
[0063] In step (2) of Example 1, a hydrazine hydrate aqueous solution is first added to the carbon dot mother liquor for reduction protection treatment, followed by dialysis to remove impurities and freeze-drying, and then redissolved to obtain a nitrogen-sulfur-doped carbon dot solution. The other steps and process parameters are the same as in Example 1.
[0064] The fluorescence quantum yield, maximum excitation wavelength, and maximum emission wavelength of the nitrogen-sulfur-doped carbon dot solutions prepared in step (2) of Examples 1-2 and Comparative Examples 1-3 were measured respectively; the color appearance of the anti-counterfeiting textiles prepared in step (3) under D65 standard daylight and maximum excitation wavelength were recorded respectively.
[0065] In the calculation of fluorescence quantum yield, quinine sulfate (dissolved in 0.1 mol / L H2SO4) was used as a reference (QY at 360 nm was 54%) to calculate the fluorescence quantum yield QY of the sample: QY = QY1(F / F1)(A1 / A)(η / η1) 2 , where QY is the quantum yield of the test sample, subscript 1 denotes the parameter of known QY (quinine sulfate), F is the integrated emission intensity of the test sample, η is the refractive index of the solvent (1.33 for water), and A is the absorbance (the absorbance under 360 nm excitation is between 0 and 0.1). The maximum excitation wavelength and maximum emission wavelength were determined using an F-4600 fluorescence spectrometer (Hitachi, Japan) under the following measurement conditions: slit 5.0 nm, voltage 700 V, and excitation wavelength range 360–600 nm.
[0066] The characteristic parameters measured in Examples 1 and 2 and Comparative Examples 1 and 2 were compared, and the results are shown in Table 1:
[0067] Table 1
[0068]
[0069]
[0070] From Table 1 we can see that:
[0071] a. In Examples 1 and 2, the nitrogen-sulfur-doped carbon dots prepared by the method of the present invention exhibit blue, green, yellow, and red light at the maximum excitation wavelength; at the same time, the fluorescence quantum yield of the carbon dots increases with increasing carbon source concentration, increasing hydrazine hydrate concentration, and extending reduction protection time; after treatment in step (3), the four anti-counterfeiting textiles obtained all appear white under D65 simulated daylight, and have significant blue, green, yellow, and red light at the maximum excitation wavelength, and the prepared textiles have good anti-counterfeiting effect.
[0072] b. In Comparative Example 1, thiourea was not added during the carbon dot synthesis in step (1), and a carbon dot mother solution without nitrogen-sulfur doping structure was obtained; compared with Example 1, the measured fluorescence quantum yield was significantly reduced.
[0073] c. During the treatment in step (2) of Comparative Example 2, no hydrazine hydrate aqueous solution was added for reduction protection when preparing the carbon dot solution. The maximum excitation wavelengths and maximum emission wavelengths of the four nitrogen-sulfur doped carbon dot solutions were basically the same. The prepared anti-counterfeiting textiles only showed blue light at the excitation wavelength, and no green, yellow, or red light was observed. The reason for this is that the carbon dots are easily oxidized by dissolved oxygen in water during dialysis to remove impurities, resulting in a blue shift in the emission wavelength. It can be seen that if no hydrazine hydrate aqueous solution is added for reduction protection in step (2), it is difficult to prepare carbon dots having blue, green, yellow, and red light at the maximum excitation wavelength.
[0074] d. During the treatment in step (2) of Comparative Example 3, a hydrazine hydrate aqueous solution was first added to the carbon dot mother liquor for reduction protection treatment, and then dialyzed to remove impurities and freeze-dried, and then dissolved again to obtain a nitrogen-sulfur doped carbon dot solution; the test results showed that the maximum excitation wavelength and the maximum emission wavelength of the four nitrogen-sulfur doped carbon dot solutions were basically the same, and the textile only showed blue light at the excitation wavelength, and no green light, yellow light, or red light was observed; this result shows that although the carbon dot mother liquor was reduced and protected by a hydrazine hydrate aqueous solution, the carbon dots were still oxidized by the dissolved oxygen in the water during the subsequent dialysis to remove impurities, resulting in a blue shift in the emission wavelength at the laser wavelength. Therefore, the hydrazine hydrate aqueous solution must be subjected to a reduction protection treatment after dialysis to remove impurities in order to have a better application effect.
[0075] Although the present invention has been disclosed above in terms of preferred embodiments, it is not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the definition of the claims.
Claims
1. A method for preparing anti-counterfeiting textiles based on full-color nitrogen-sulfur doped carbon dots, characterized in that: The specific steps include: (1) Preparation of nitrogen-sulfur doped carbon dot mother liquor: Citric acid and thiourea are used as raw materials, solvent is added to obtain a reaction solution, and high temperature treatment is performed to prepare carbon dot mother liquor; (2) Preparation of nitrogen-sulfur doped carbon dot solution: The carbon dot mother solution prepared in step (1) is dialyzed to remove impurities and then freeze-dried to obtain a lyophilized powder. The lyophilized powder is added to a hydrazine hydrate aqueous solution to obtain a mixed solution, which is subjected to a reduction protection treatment to prepare a full-color nitrogen-sulfur doped carbon dot solution; (3) Preparation of full-color anti-counterfeiting textiles: adding the full-color nitrogen-sulfur doped carbon dot solution prepared in step (2) to an adhesive and / or thickener to prepare a fluid, and then attaching the fluid to the textile by dipping or scraping to prepare a full-color anti-counterfeiting textile; In step (1), there are four kinds of solvents, namely water, glycerol, a mixture of glycerol and N,N-dimethylformamide, and N,N-dimethylformamide; When the solvent in step (1) is water, a full-color nitrogen-sulfur-doped carbon dot mother liquor is obtained, which emits blue light after excitation; when the solvent in step (1) is glycerol, a full-color nitrogen-sulfur-doped carbon dot mother liquor is obtained, which emits green light after excitation; when the solvent in step (1) is a mixture of glycerol and N,N-dimethylformamide, a full-color nitrogen-sulfur-doped carbon dot mother liquor is obtained, which emits yellow light after excitation; when the solvent in step (1) is N,N-dimethylformamide, a full-color nitrogen-sulfur-doped carbon dot mother liquor is obtained, which emits red light after excitation; The high temperature treatment in step (1) is carried out at 140-160° C. for 4-6 hours.
2. The method according to claim 1, wherein In step (1), the concentration of citric acid in the reaction solution is 0.05-0.1 g / L; the molar ratio of citric acid to thiourea is 1:3-7.
3. The method according to claim 1, wherein In step (2), the concentration of the lyophilized powder in the mixed solution is 0.5~1 g / L; the concentration of hydrazine hydrate in the mixed solution is 18~22 mL / L.
4. The method according to claim 1, wherein In step (2), the treatment temperature of the reduction protection treatment is 15-25° C.; and the treatment time of the reduction protection treatment is 10-14 hours.
5. The method according to claim 1, wherein In step (3), the concentration of nitrogen-sulfur-doped carbon dots in the fluid is 0.5-1 g / L; the adhesive in the fluid is a polyacrylate adhesive; the concentration of the adhesive is 2-4 g / L; the thickener in the fluid is a sodium alginate paste with a mass concentration of 3-7%; the concentration of the thickener is 1-2 g / L.
6. The method according to claim 1, wherein In step (3), the textile is selected from woven fabrics, knitted fabrics or non-woven fabrics made of cotton, linen, silk, flax, polyester, nylon or viscose.
7. A full-color anti-counterfeiting textile produced by the method according to any one of claims 1 to 6.
8. Use of the full-color anti-counterfeiting textiles described in claim 7 in the fields of security encryption or special protective clothing.
Citation Information
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