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Method for synthesizing DSD (4, 4'-diaminostilbene-2, 2'-disulfonic) acid-triazine fluorescent brightening agents

A technology of fluorescent whitening agent and acid triazine, applied in the field of fluorescent whitening agent, can solve problems such as increasing production cost, and achieve the effects of reducing production cost, eliminating cost increase and pollution problems, and improving utilization rate

Active Publication Date: 2013-07-17
ZHEJIANG TRANSFAR WHYYON CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the biggest disadvantage is the introduction of the reaction solvent, which greatly increases the production cost of the product
In addition, the introduction of organic solvents inevitably has the problem of disposal and pollution of organic solvents
[0020] All of the above have improved the reaction system of the DSD acid triazine fluorescent whitening agent to a certain extent. Based on the comprehensive consideration of the reaction cost and other aspects, people can only expand the reproduction by simply expanding the reaction equipment.

Method used

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  • Method for synthesizing DSD (4, 4'-diaminostilbene-2, 2'-disulfonic) acid-triazine fluorescent brightening agents
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  • Method for synthesizing DSD (4, 4'-diaminostilbene-2, 2'-disulfonic) acid-triazine fluorescent brightening agents

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Prepare 0.015mol of DSD acid with 0.03mol of ethanolamine to make a solution of about 30g for later use.

[0047] Suspend 0.0305mol of cyanuric chloride in a 250ml four-necked bottle in 110g of ice water, and add 3 drops of concentrated hydrochloric acid. Under stirring, slowly add DSD acid ethanolamine solution dropwise, keeping pH value = 2-3, temperature 0-5°C. Use 15% sodium hydroxide solution to adjust the pH value to about 2.5, and use an amino reagent to detect the disappearance of the amino group, and the shrinkage reaction is completed.

[0048] The temperature of the reaction material is raised to 20°C, about 0.295mol of aniline is added, and 15% sodium hydroxide solution is added dropwise to keep the pH value at about 5, and the reaction temperature is 20-25°C. In the later stage of the reaction, gradually increase the pH value to 6-6.5 until the two-shrinkage reaction is completed.

[0049] Keeping the reaction temperature, slowly add 0.3 mol of sodium hyd...

Embodiment 2

[0052] Prepare 0.015 mol of DSD acid with 0.03 mol of diethanolamine to make a solution of about 30 g for later use.

[0053] Suspend 0.0305mol cyanuric chloride in 250ml four-necked bottle in 110g ice water, slowly add DSD acid diethanolamine solution dropwise under stirring, keep pH=2-3, temperature 0-5℃. Use 15% sodium hydroxide solution to adjust the pH value to about 2.5, and keep warm at 6-8°C for reaction. The disappearance of the amino group is detected by the amino reagent, and the shrinkage reaction is completed.

[0054] The temperature of the reaction material was raised to 20°C, about 0.295 mol of aniline was added, and 15% sodium hydroxide solution was added dropwise to keep the pH value at 5-6.5 until the bicondensation reaction was completed.

[0055] Keeping the reaction temperature, 0.3 mol of sodium hydroxide solution was added dropwise to the reaction liquid for about 0.5 hr, and then 0.003 mol of diethanolamine was added to the reaction liquid, and the te...

Embodiment 3-16

[0058] The experimental operation is the same as before. The experimental data are as follows:

[0059]

[0060]

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Abstract

The invention discloses a method for synthesizing DSD (4, 4'-diaminostilbene-2, 2'-disulfonic) acid-triazine fluorescent brightening agents. A DSD acid-triazine fluorescent brightening agent reaction system is improved to a certain degree by an existing method, and on the basis of comprehensive consideration in various aspects such as the reaction cost, expanded production is carried out but only can be implemented by means of simply expanding reaction equipment. The method is characterized by comprising salifying all organic amine NH<2>R<2> and DSD acid of raw materials for tertiary condensation reaction or parts of the organic amine NH<2>R<2> and DSD acid to obtain DSD acid organic ammonium salt aqueous solution; and sequentially enabling the DSD acid organic ammonium salt aqueous solution to perform primary condensation reaction, secondary condensation reaction and tertiary condensation reaction to obtain the DSD acid-triazine fluorescent brightening agents. The method has the advantages that optional compounds or auxiliaries except for reactants are omitted in reaction procedures; the burden of desalination in an aftertreatment procedure caused by addition of extra salt in an existing method for manufacturing DSD acid-triazine fluorescent brightening agents is relieved, and the problem of foaming due to additional surfactants is solved; the COD (chemical oxygen demand) of waste liquor and the total quantity of the waste liquor are reduced; and problems of increase of cost and pollution due to organic solvents utilized in primary condensation reaction in the existing method are solved.

Description

technical field [0001] The invention relates to the field of fluorescent whitening agents, in particular to a method for synthesizing DSD acid triazine fluorescent whitening agents. Background technique [0002] With the improvement of living standards, people's requirements for color are getting stronger. Because the fluorescent whitening agent has the effects of whitening, brightening and brightening, it meets people's visual requirements. Due to the strong whitening effect of DSD acid triazines, its series of products are basically low-toxic or non-toxic, and have good affinity with fibers. DSD acid triazine fluorescent whitening agents are used in textiles, detergents, and paper industries. has been widely applied. Therefore, it is of practical significance to improve the synthesis process of such fluorescent whitening agents. [0003] DSD acid triazine series fluorescent whitening agent, its general chemical structure is as follows: [0004] [0005] In the formu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B23/14C09K11/06
Inventor 李文胜蔡定汉王晓英范约明王小林王景国
Owner ZHEJIANG TRANSFAR WHYYON CHEM
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