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Method for preparing liquid fluorescent brightener combination capable of being steadily stored

A fluorescent whitening agent and storage-stable technology, applied in the field of preparation of liquid fluorescent whitening agent compositions, can solve the problems of increased manpower and production costs, difficult industrialized production, and high environmental pollution of acid solution, and achieves good storage stability , The effect of increasing product yield and reducing raw material consumption

Active Publication Date: 2014-08-13
山西晋光化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the following problems usually occur when this type of compound is used: first, their molecular weight is relatively large, but only two sulfonic acid groups are contained in the structure, and the water solubility is poor; Post-treatment generally adopts acid analysis, filtration, drying, crushing and other processes, the operation is complicated, and the discharged acid solution will pollute the environment; thirdly, disulfonic acid fluorescent whitening agents are generally powder products, and the cold water dispersibility is not high , there is dust and other pollution in the process of production and use, which brings great harm to the environment and the health of operators; finally, it is not easy to realize automatic addition operation of powder products in application, which increases manpower and production costs
Although the disulfonic acid fluorescent whitening agent has the advantages of higher whitening performance, but because of its poor water solubility, there are few reports of patents for the liquid dosage form of this type of whitening agent. Therefore, it is necessary to synthesize a liquid with stable quality. Type disulfonic acid liquid fluorescent whitening agent has very important practical significance
[0004] CN102477227A reports a disulfonic acid fluorescent whitening agent that does not add additional dissolution aids for stable storage, and the method needs to carry out 1-R 1 -2-R 2 -Synthesis of acrylamide and monoethanolamine, and its addition product replaces a single fatty amine, which improves the stability of the product, but this method has higher requirements for the synthesis product of acrylamide and monoethanolamine, and is not easy for industrial production
[0005] CN1303424A has reported a water-soluble complex of an optical brightener substantially free of inorganic salts and a quaternary ammonium salt compound, and the complex is selected from a sulfonated optical brightener and a quaternary ammonium salt to carry out a complex reaction, and subsequently removes the Almost all excess salts are formed, but the purification techniques used include solvent extraction, phase separation, high-pressure ultrafiltration, etc. The methods are relatively complicated and costly, which is not conducive to industrial production
[0010] At present, the output of high-grade paper in the market is increasing day by day, and disulfonic acid liquid fluorescent whitening agent is more and more popular due to its good whitening performance, and there is an urgent need for a liquid dosage form that is practical and convenient, easy to add automatically, and stable for a long storage time products, but disulfonic acid brighteners have poor solubility and are prone to precipitation when they are made into liquid products due to structural limitations.

Method used

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  • Method for preparing liquid fluorescent brightener combination capable of being steadily stored
  • Method for preparing liquid fluorescent brightener combination capable of being steadily stored
  • Method for preparing liquid fluorescent brightener combination capable of being steadily stored

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step (1): Add 300g of crushed ice, 300g of water, and 0.5g of PEG-400 to a 2000ml beaker, cool in an ice bath, adjust the pH to 1.5-2.0 with hydrochloric acid, add 30g of cyanuric chloride, and stir for 1.5 hours. Prepare 27g of DSD acid (100%) into an aqueous solution, add it to the above solution at a uniform speed within 1.5-2.0 hours, and use 30% NaHCO 3 Adjust PH=3.5-4.0, keep this PH value for 1.5 hours, then adjust PH=4.5-5.0, react until the amino value disappears;

[0039] Step (2): Add 2g of p-aminobenzenesulfonic acid, heat up to 30°C, and react for 0.5 hours;

[0040] Step (3): add 15g aniline, use 30%Na 2 CO 3 Adjust PH=6-7, heat up to 40°C, and react until the amino value disappears;

[0041] Step (4): Add 20g of diethanolamine, raise the temperature to 95-100°C, adjust the pH to 8-9 with 30% NaOH, and react for 3 hours;

[0042] Step (5): Stir the reaction solution to cool down to below 55°C, filter it with a Buchner funnel to remove water-insoluble i...

Embodiment 2

[0045] Step (2): Add 4g of p-aminobenzenesulfonic acid, raise the temperature to 30°C, and react for 0.5 hours.

[0046] All the other steps are the same as in Example 1. The ratio of each component of the mixture is determined by high performance liquid chromatography, and the ratio of the three components is (I): (II): (III) = 35:3:3.

Embodiment 3

[0048] Step (2): Add 6g of p-aminobenzenesulfonic acid, raise the temperature to 30°C, and react for 0.5 hours.

[0049] All the other steps are the same as in Example 1. The ratio of each component of the mixture is determined by high performance liquid chromatography, and the ratio of the three components is (I): (II): (III) = 17:3:3.

[0050] The application data of single component and mixed component to pulp whitening are as follows (equivalent to the same fluorescence intensity E=130):

[0051]

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Abstract

The invention discloses a method for preparing liquid fluorescent brightener combination capable of being steadily stored, which belongs to the technical field of culture paper special-purpose additives, and comprises the steps that 4, 4-2 amino 2 styrene-2, 2-disulfonic acid, sulfanilic acid and cyanuric chloride are subjected to the first step of condensation reaction under the condition that acid-binding agent exists, the second step of condensation reaction is subjected by continuously adding aniline, then the third step of condensation reaction is subjected by adding diethanol amine to obtain symmetrical and asymmetrical mixtures of two triazine styrene type liquid fluorescent brightener I, II and III, and the mixtures are desalted and concentrated through sand filter and carbon filter to obtain an end product. The method for preparing liquid fluorescent brightener combination capable of being steadily stored has the advantages of high whitening performance, less usage, excellent storage stability, low raw material consumption and low environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of special additives for cultural paper, and relates to a preparation method of a storage-stable liquid fluorescent whitening agent composition. Background technique [0002] Stilbene bistriazine fluorescent whitening agents can be divided into two, four, and six sulfonate groups according to the number of sulfonic acid groups. Among them, the disulfonic acid fluorescent whitening agent has high whitening performance, and is mainly used for whitening of pulp, surface sizing, coating and whitening of cotton, hemp, and cellulose fiber fabrics, and whitening of light-colored fiber fabrics. Among them, excellent fluorescent whitening agents include VBL, BA, CXT, etc., which are widely used because of their strong affinity with fibers and good whitening effect. However, the following problems usually occur when this type of compound is used: first, their molecular weight is relatively large, but only two sulfoni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21H21/30
Inventor 高飞卢英微谌孟晴
Owner 山西晋光化工有限公司