Fluorescent whitening agent with high dispersion stability, preparation method and application method

The particle size of the fluorescent whitening agent is reduced to the nanoscale through nano-grinding technology, and combined with high dispersion stability dispersants and polymers, the problems of large particle size and poor dispersion of existing fluorescent whitening agents are solved, achieving the effect of high whiteness and uniform whitening.

CN119913745APending Publication Date: 2025-05-02NICCA CHEM CHINA CO LTD
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Patent Information

Application Number
CN202510035488.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-09
Publication Date
2025-05-02

AI Technical Summary

Technical Problem

The existing fluorescent whitening agent has a large particle size, making it difficult to fully dye the fabric, resulting in low whiteness; at the same time, poor dispersion leads to uneven whitening, and fluorescent spots or yellow spots are prone to appear, affecting the uniform whitening effect of the fabric.

Method used

The particle size of the fluorescent whitening agent is reduced to the nanoscale by using nanogrinding technology. Combined with a high-dispersion stability dispersant and polymer, the particle size of the whitening agent reaches the nanoscale through a nanogrinder, improving its dispersion and stability.

Benefits of technology

The high dispersion stability of the whitening agent is achieved, the particle size reaches the nanometer level, and can be distributed more evenly in the fabric, improve whiteness, and avoid the appearance of fluorescent spots or macules, ensuring the uniform whitening effect of the fabric.

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Patent Text Reader

Abstract

The invention discloses a fluorescent whitening agent with high dispersion stability, a preparation method and an application method, and belongs to the technical field of textile printing and dyeing. The invention introduces a fluorescent whitening agent with the characteristics of small particle size, high stability, strong whitening ability and the like. The fluorescent whitening agent is a dispersion liquid composed of a whitening agent filter cake, a dispersing agent, a solvent, a thickening agent, water and the like. The whitening agent is applied to whitening processing of polyester and blended fabrics thereof, and can show higher whiteness under the condition of lower dosage; and even under the condition that a leveling agent is not added, a uniform whitening effect can be obtained, fluorescent spots or yellow spots are not formed, and high-quality whitened fabric can be obtained.
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Description

Technical Field

[0001] The invention relates to a fluorescent whitening agent, in particular to a fluorescent whitening agent with high dispersion stability, a preparation method and an application method, and belongs to the technical field of textile printing and dyeing. Background Art

[0002] Polyester fiber is the world's most widely used synthetic textile fiber. Polyester fiber has the advantages of high modulus, high strength, high elasticity, good shape retention and heat resistance, and has become the most widely used and consumed fiber variety. Clothes made of polyester fiber will turn yellow after wearing for a period of time because the fiber molecules and dye molecules on the fabric are destroyed under the action of ultraviolet rays, resulting in aging and yellowing. In addition, some fabrics themselves are not white enough and need to be made whiter and brighter.

[0003] Fluorescent whitening agents solve these problems. Because fluorescent whitening agents have the characteristics of absorbing ultraviolet light, absorbing ultraviolet light with a wavelength of about 350nm, and then emitting blue light fluorescence with a wavelength of about 450nm, it can correct the yellow color of yellowed fabrics and make the fabrics appear white. At the same time, fluorescent whitening agents can also effectively protect textiles from damage by ultraviolet rays and extend the service life of textiles.

[0004] Fluorescent whitening agent raw materials are non-water-soluble substances with large particles. They cannot be used directly in the whitening process. They need to be mechanically ground into at least micron-level particles. At the same time, water-soluble products with a certain degree of dispersibility are convenient for use in printing and dyeing factories. The particle size of fluorescent whitening agents on the market is generally between 1-2 microns. The particle size of the whitening agent is relatively large, making it difficult to fully dye the fabric to form a high-whiteness fabric; and it is easy to stratify and agglomerate at the bottom after long-term storage, resulting in differences in the concentration of the whitening agent above and below, resulting in uneven whitening effects between batches, and the processing quality cannot be guaranteed, affecting the normal use of the product. In addition, some whitening agents have poor dispersibility and are easy to aggregate during the whitening agent processing, forming fluorescent spots or yellow spots, and it is impossible to obtain a uniformly whitened fabric. Summary of the invention

[0005] The present invention mainly solves the deficiencies in the prior art and provides a high-dispersion stability fluorescent whitening agent, a preparation method and an application method for solving the problems described in the background technology.

[0006] The above technical problems of the present invention are mainly solved by the following technical solutions:

[0007] A highly dispersed and stable fluorescent brightener, calculated by weight:

[0008]

[0009] Preferably, the brightener filter cake is at least one compound represented by the following general formula (1) or (2) or (3),

[0010]

[0011] In formula (1), R 1 Indicates H, OH, CN, CH3, NO2, NH2, R 2 Indicates H, OH, CN, CH3, NO2, NH2;

[0012]

[0013] In formula (2), R 3 Indicates H, OH, CN, CH3, NO2, NH2, R 4 Indicates H, OH, CN, CH3, NO2, NH2;

[0014]

[0015] In formula (3), R 5 Indicates H, OH, CN, CH3, NO2, NH2, R 6 Represents H, OH, CN, CH3, NO2, and NH2.

[0016] Preferably, the dispersant is composed of at least two of the following dispersants 4-6,

[0017]

[0018] In the formula (dispersant 4), R 7 represents an alkylene group having 2 to 3 carbon atoms, p represents an integer of 1 to 50, X represents a hydrogen atom or -SO3Na, -OSO3Na, -COONa, -SO3NH4, -OSO3NH4, -COONH4, -SO3K, -OSO3K, -COOK, R 8 represents H or styryl or distyryl or tristyryl;

[0019]

[0020] In the formula (dispersant 5), R 9 express

[0021] Where n = 5-20, m = 5-20, R 10 represents at least one of a hydrogen atom, -SO3Na, -OSO3Na, -COONa, -SO3NH4, -OSO3NH4, -COONH4, -SO3K, -OSO3K, and -COOK;

[0022] Dispersant 6 is a polymer of polystyrene maleic anhydride and methoxy-PEG-acrylate, wherein the molecular weight of polystyrene maleic anhydride is 1000-30000, and the molecular weight of PEG in methoxy-PEG-acrylate is 200-20000.

[0023] Preferably, the solvent is at least one of ethylene glycol, propylene glycol, tripropylene glycol, glycerol, polyethylene glycol 600, benzyl alcohol, diethylene glycol butyl ether, and ethylene glycol butyl ether.

[0024] Preferably, the thickener is at least one of guar gum, sodium alginate, xanthan gum, sodium carboxymethyl cellulose, hydroxymethyl cellulose, sodium hydroxypropyl cellulose, sodium polyacrylate and polyacrylamide.

[0025] A method for preparing a fluorescent whitening agent with high dispersion stability is carried out according to the following steps:

[0026] ① Preparation of whitening agent pre-dispersion:

[0027] Put the brightener filter cake, dispersant and defoamer according to the proportion and appropriate amount of water into the reactor, stir well at a stirring speed of 20-200rpm;

[0028] ② Preparation of whitening agent stock solution:

[0029] The dispersion is introduced into a nano-grinding device and ground to a particle size of D50≤400nm and D90≤800nm. The grinding is completed after filtering through a black cotton cloth until there is no residue.

[0030] ③ Preparation of paste:

[0031] Mix the thickener and solvent evenly according to the proportion, add them into an appropriate amount of hot water at 80℃, stir at high speed for 30 minutes, stir thoroughly and place in an 80℃ drying room to mature overnight for later use;

[0032] ④ Preparation of brightener products:

[0033] Mix the above-mentioned brightener stock solution, paste solution, preservative and remaining water, totaling 100 parts; stir thoroughly for 4 hours, filter through black cotton cloth, filtration level 1-2, and filter and package after meeting the requirements.

[0034] Preferably, the grinding equipment in step ② is a horizontal sander, and the abrasive is zirconium oxide; the specifications of the black cotton cloth are: 30*36, 30 warp yarns and 36 weft yarns; the specifications of the black cotton cloth in step ④ are: 30*36, 30 warp yarns and 36 weft yarns; the filter bag is a 180 mesh polyester silk bag.

[0035] A method for applying a fluorescent brightener with high dispersion stability: the fluorescent brightener is applied to the whitening process of polyester and its blended fabrics, and a uniform whitened fabric is obtained in the process without a leveling agent.

[0036] Preferably, the whitening process for polyester and its blended fabrics is carried out according to the following steps:

[0037] (1) Using a bath ratio of 1:3 to 1:20, adding polyester and its blended fabrics into a dyeing machine at 20 to 50° C., and adding a whitening processing liquid prepared in proportion into the dyeing machine;

[0038] Wherein, the whitening processing liquid, wherein the whitening agent dosage is 0.01-1.5g / L;

[0039] (2) Set the parameters, raise the temperature to 110-140°C at 0.5-4°C / min, and keep warm for 20-60 minutes;

[0040] (3) then washing with hot water, washing with cold water, and drying to obtain the whitened fabric.

[0041] Preferably, the dyeing machine in step (1) is an overflow dyeing machine.

[0042] Beneficial Effects

[0043] 1. The present invention adopts a high molecular polymer containing a whitening agent affinity group and having hydrophilicity and a polyether dispersant to disperse the whitening agent filter cake, and uses a nano grinder to make the particle size of the whitening agent reach the nano level, making it easier to enter the interior of the polyester fiber, thereby obtaining a processed fabric with high whiteness and no fluorescent spots and yellow spots.

[0044] 2. The dispersant used in the present invention has an excellent dispersing effect on the brightener filter cake, which can prevent the brightener from agglomerating during the brightening process. Even in the absence of a leveling agent, a uniformly brightened processed fabric can be obtained.

[0045] 3. The particle size of the brightener prepared by the present invention reaches the nanometer level, and the dispersion stability is good. The storage stability of the product is further improved by combining with a solvent and a thickener, so that the product can be placed at room temperature for 6 months without stratification, thereby ensuring the stability of the processing quality. DETAILED DESCRIPTION

[0046] The technical solution of the present invention is further specifically described below through embodiments.

[0047] Example 1: The preparation process of a fluorescent whitening agent with high dispersion stability is as follows:

[0048]

[0049]

[0050] The molecular structure formula of the fluorescent brightener filter cake is:

[0051]

[0052] A method for preparing the fluorescent whitening agent of this embodiment comprises the following steps:

[0053] 1) Dissolve 3 parts of sodium styrylphenol polyoxyethylene ether sulfonate and 3 parts of sodium ethylenediamine polyoxyethylene-polyoxypropylene copolymer sulfonate in 61.35 parts of water and stir well.

[0054] 2) Add 10 parts of fluorescent brightener filter cake ER-I to the mixture in step 1) and stir to make it evenly dispersed, and then add 0.2 parts of defoaming agent.

[0055] 3) The mixture in step 2) is put into a laboratory small grinding machine for grinding until the particle size D 50 ≤400nm, D 90 ≤800nm. After completion, filter with a 100-mesh filter bag to obtain the brightener filtrate.

[0056] 4) Mix 0.3 parts of thickener and 2 parts of tripropylene glycol evenly, add to 20 parts of hot water, shear at high speed to make it swell completely, cool down after dissolution, add 0.15 parts of preservative for later use.

[0057] 5) Add the mixture obtained in step 3) and step 4) into a 500 ml beaker, stir thoroughly, and filter to remove impurities to obtain the product.

[0058] Example 2: The preparation process of a fluorescent whitening agent with high dispersion stability is as follows:

[0059]

[0060]

[0061] The molecular structure formula of the fluorescent brightener filter cake is:

[0062]

[0063] A method for preparing the fluorescent whitening agent of this embodiment comprises the following steps:

[0064] 1) Dissolve 3 parts of sodium styrylphenol polyoxyethylene ether sulfonate and 3 parts of sodium ethylenediamine polyoxyethylene-polyoxypropylene copolymer sulfonate in 61.35 parts of water and stir well.

[0065] 2) Add 10 parts of fluorescent brightener filter cake ER-II to the mixture in step 1) and stir to make it evenly dispersed, and then add 0.2 parts of defoaming agent.

[0066] 3) The mixture in step 2) is put into a laboratory small grinding machine for grinding until the particle size D 50 ≤400nm, D 90 ≤800nm. After completion, filter with a 100-mesh filter bag to obtain the brightener filtrate.

[0067] 4) Mix 0.3 parts of thickener and 2 parts of tripropylene glycol evenly, add to 20 parts of hot water, shear at high speed to make it swell completely, cool down after dissolution, add 0.15 parts of preservative for later use.

[0068] 5) Add the mixture obtained in step 3) and step 4) into a 500 ml beaker, stir thoroughly, and filter to remove impurities to obtain the product.

[0069] Example 3: The preparation process of a fluorescent whitening agent with high dispersion stability is as follows:

[0070]

[0071]

[0072] The molecular structure of the fluorescent brightener filter cake 135 is:

[0073]

[0074] A method for preparing the fluorescent whitening agent of this embodiment comprises the following steps:

[0075] 1) Dissolve 3 parts of sodium styrene phenol polyoxyethylene ether sulfonate, 3 parts of sodium ethylenediamine polyoxyethylene-polyoxypropylene copolymer sulfonate and 3 parts of styrene-maltoacrylate copolymer in 45.35 parts of water and stir well.

[0076] 2) Add 16 parts of fluorescent brightener filter cake 135 and 4 parts of fluorescent brightener filter cake ER-I to the mixture of step 1) and stir to make them evenly dispersed, and then add 0.2 parts of defoaming agent.

[0077] 3) The mixture in step 2) is put into a laboratory small grinding machine for grinding until the particle size D 50 ≤400nm, D 90 ≤800nm. After completion, filter with a 100-mesh filter bag to obtain the brightener filtrate.

[0078] 4) Mix 0.3 parts of thickener and 5 parts of tripropylene glycol evenly, add to 20 parts of hot water, shear at high speed to make it swell completely, cool down after dissolution, add 0.15 parts of preservative for later use.

[0079] 5) Add the mixture obtained in step 3) and step 4) into a 500 ml beaker, stir thoroughly, and filter to remove impurities to obtain the product.

[0080] Example 4: The preparation process of a fluorescent whitening agent with high dispersion stability is as follows:

[0081]

[0082]

[0083] The molecular structure formula of the fluorescent brightener filter cake is:

[0084]

[0085] A method for preparing the fluorescent whitening agent of this embodiment comprises the following steps:

[0086] 1) Dissolve 3 parts of sodium styrylphenol polyoxyethylene ether sulfonate, 2 parts of sodium ethylenediamine polyoxyethylene-polyoxypropylene copolymer sulfonate and 2 parts of styrene-maltoacrylate copolymer in 52.35 parts of water and stir well.

[0087] 2) Add 15 parts of fluorescent brightener filter cake 185 to the mixture of step 1) and stir to make it evenly dispersed, and then add 0.2 parts of defoaming agent.

[0088] 3) The mixture in step 2) is put into a laboratory small grinding machine for grinding until the particle size D 50 ≤400nm, D 90 ≤800nm. After completion, filter with a 100-mesh filter bag to obtain the brightener filtrate.

[0089] 4) Mix 0.3 parts of thickener and 5 parts of tripropylene glycol evenly, add to 20 parts of hot water, shear at high speed to make it swell thoroughly, cool after dissolution, add 0.15 parts of preservative for later use.

[0090] 5) Add the mixture obtained in step 3) and step 4) into a 500 ml beaker, stir well, filter to remove impurities, and obtain a fluorescent brightener for polyester fiber.

[0091] High temperature and high pressure dyeing process embodiment:

[0092] Add 0.02g of brightener into a high-temperature and high-pressure dyeing tank, add 100ml of deionized water, add 0.1g of glacial acetic acid, add 10g of polyester white fabric, dye (135℃×30min, bath ratio 1:10) - wash - dehydrate - 120℃×2min drying - 170℃×90S setting. After the end, use a colorimeter to test the CIE whiteness value of the fabric.

[0093] Beneficial effects:

[0094]

Claims

1. A high dispersion stability fluorescent brightener, characterized in that According to weight parts:

2. A fluorescent whitening agent with high dispersion stability according to claim 1, characterized in that: The brightener filter cake is at least one compound represented by the following general formula (1) or (2) or (3), In formula (1), R 1 Indicates H, OH, CN, CH3, NO2, NH2, R 2 Indicates H, OH, CN, CH3, NO2, NH2; In formula (2), R 3 Indicates H, OH, CN, CH3, NO2, NH2, R 4 Indicates H, OH, CN, CH3, NO2, NH2; In formula (3), R 5 Indicates H, OH, CN, CH3, NO2, NH2, R 6 Represents H, OH, CN, CH3, NO2, and NH2.

3. A fluorescent whitening agent with high dispersion stability according to claim 1, characterized in that The dispersant is composed of at least two of the following dispersants 4-6, In the formula (dispersant 4), R 7 represents an alkylene group having 2 to 3 carbon atoms, p represents an integer of 1 to 50, X represents a hydrogen atom or -SO3Na, -OSO3Na, -COONa, -SO3NH4, -OSO3NH4, -COONH4, -SO3K, -OSO3K, -COOK, R 8 represents H or styryl or distyryl or tristyryl; In the formula (dispersant 5), R 9 express Where n = 5-20, m = 5-20, R 10 represents at least one of a hydrogen atom, -SO3Na, -OSO3Na, -COONa, -SO3NH4, -OSO3NH4, -COONH4, -SO3K, -OSO3K, and -COOK; Dispersant 6 is a polymer of polystyrene maleic anhydride and methoxy-PEG-acrylate, wherein the molecular weight of polystyrene maleic anhydride is 1000-30000, and the molecular weight of PEG in methoxy-PEG-acrylate is 200-20000.

4. A fluorescent whitening agent with high dispersion stability according to claim 1, characterized in that: The solvent is at least one of ethylene glycol, propylene glycol, tripropylene glycol, glycerol, polyethylene glycol 600, benzyl alcohol, diethylene glycol butyl ether, and ethylene glycol butyl ether.

5. The fluorescent whitening agent with high dispersion stability according to claim 1, characterized in that: The thickener is at least one of guar gum, sodium alginate, xanthan gum, sodium carboxymethyl cellulose, hydroxymethyl cellulose, sodium hydroxypropyl cellulose, sodium polyacrylate and polyacrylamide.

6. A method for preparing a fluorescent whitening agent with high dispersion stability, the method using the fluorescent whitening agent according to any one of claims 1 to 5, characterized in that the method is carried out according to the following steps: ① Preparation of whitening agent pre-dispersion: Put the brightener filter cake, dispersant and defoamer according to the proportion and appropriate amount of water into the reactor, stir well at a speed of 20-200rpm; ② Preparation of whitening agent stock solution: The dispersion is introduced into a nano-grinding device and ground to a particle size of D50≤400nm and D90≤800nm. The grinding is completed after filtering through a black cotton cloth until there is no residue. ③ Preparation of paste: Mix the thickener and solvent evenly according to the proportion, add them into an appropriate amount of hot water at 80℃, stir at high speed for 30 minutes, stir thoroughly and place in an 80℃ drying room to mature overnight for later use; ④ Preparation of brightener products: Mix the above-mentioned brightener stock solution, paste solution, preservative and remaining water, totaling 100 parts; stir thoroughly for 4 hours, filter through black cotton cloth, filtration level 1-2, and filter and package after meeting the requirements.

7. The method for preparing a fluorescent whitening agent with high dispersion stability according to claim 1, characterized in that: The grinding equipment in step ② is a horizontal sander, and the abrasive is zirconium oxide; the specifications of the black cotton cloth are: 30*36, 30 warp yarns and 36 weft yarns; the specifications of the black cotton cloth in step ④ are: 30*36, 30 warp yarns and 36 weft yarns; the filter bag is a 180-mesh polyester silk bag.

8. An application method of a fluorescent whitening agent with high dispersion stability, the application method using the fluorescent whitening agent according to any one of claims 6 to 7, characterized in that: Fluorescent brighteners are used in the whitening process of polyester and its blended fabrics, and uniform whitened fabrics can be obtained in the process without a leveling agent.

9. The method for applying a fluorescent whitening agent with high dispersion stability according to claim 8, characterized in that The whitening process for polyester and its blended fabrics is carried out according to the following steps: (1) Using a bath ratio of 1:3 to 1:20, adding polyester and its blended fabrics into a dyeing machine at 20 to 50° C., and adding a whitening processing liquid prepared in proportion into the dyeing machine; Wherein, the whitening processing liquid, wherein the whitening agent dosage is 0.01-1.5g / L; (2) Set the parameters, raise the temperature to 110-140°C at 0.5-4°C / min, and keep warm for 20-60 minutes; (3) then washing with hot water, washing with cold water, and drying to obtain the whitened fabric.

10. The application method of a high dispersion stability fluorescent whitening agent according to claim 8, characterized in that: The dyeing machine in step (1) is an overflow dyeing machine.

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