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A kind of synthetic method of the stilbene biphenyl fluorescent whitening agent of slight blue tone

A technology of stilbene biphenyls and fluorescent whitening agents, which is applied in the field of fluorescent whitening agents to achieve the effects of improving purity, reducing potential safety hazards and high product yield

Active Publication Date: 2021-08-24
沈阳中化新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, fluorescent whitening agents with bluish light are in great demand in liquid detergents and PVC sheets. At present, the research at home and abroad is still in a blank state.

Method used

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  • A kind of synthetic method of the stilbene biphenyl fluorescent whitening agent of slight blue tone
  • A kind of synthetic method of the stilbene biphenyl fluorescent whitening agent of slight blue tone
  • A kind of synthetic method of the stilbene biphenyl fluorescent whitening agent of slight blue tone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a dry 500ml four-necked flask, sequentially add 130g of dimethylformamide, 34g of 4,4'-bis(diethoxyphosphonomethyl)biphenyl and 31.96g of sodium benzaldehyde o-sulfonate; then start stirring Keep warm at room temperature for 0.5h; under stirring at 30°C, add 9.2g of solid potassium hydroxide in 4 times on average for a total of 2 hours; after the addition, raise the temperature to 50°C and keep warm for 8h; The solvent was distilled off at ℃; after the distillation, 136g of 3% sodium chloride aqueous solution was added, cooled to 5°C, filtered, and dried at 100°C to obtain the target product 4,4-bis(2-disulfonate sodium styryl- ) biphenyl 42.08g. The percentage of target product determined by liquid chromatography is: 98.7%.

[0024] The whiteness and shade data are identified in Table 1 with an infrared dyeing machine (model DL-6000P) and a desktop expert spectrophotometer (X_Rite CE 7000A):

[0025]

Embodiment 2

[0027] In a dry 500ml four-necked flask, sequentially add 130g of dimethylformamide, 34g of 4,4'-bis(diethoxyphosphonomethyl)biphenyl and 31.96g of sodium benzaldehyde o-sulfonate; then start stirring Insulate at room temperature for 0.5h; stir at 15°C, add 9.2g of solid potassium hydroxide in 4 times on average, and the total addition time is 2 hours; Evaporate the solvent; after the distillation, add 136g of 3% sodium chloride aqueous solution, cool to 5°C, filter, and dry at 100°C to obtain the target product 4,4-bis(2-disulfonate sodium styryl-) Benzene 42.01g. The percentage of target product determined by liquid chromatography is: 98.8%.

[0028] The whiteness and shade data are identified in Table 2 with an infrared dyeing machine (model DL-6000P) and a desktop expert spectrophotometer (X_Rite CE 7000A):

[0029]

Embodiment 3

[0031] In a dry 500ml four-necked flask, sequentially add 130g of dimethylformamide, 34g of 4,4'-bis(diethoxyphosphonomethyl)biphenyl and 31.96g of sodium benzaldehyde o-sulfonate; then start stirring Incubate at room temperature for 0.5h; under stirring at 50°C, add 9.2g of solid potassium hydroxide in 4 times on average, and the addition time is 2 hours in total; after the addition, continue to keep warm for 8h; after the reaction is over, evaporate the solvent at 150-160°C After the distillation, add 136g concentration of 3% sodium chloride aqueous solution, filter after cooling to 5°C, and dry to obtain the target product 4,4-bis(2-disulfonate sodium styryl-)biphenyl 42.12g. The percentage of target product determined by liquid chromatography is: 98.5%.

[0032] The whiteness and shade data are identified in Table 3 with an infrared dyeing machine (model DL-6000P) and a desktop expert spectrophotometer (X_Rite CE 7000A):

[0033]

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Abstract

The invention discloses a method for synthesizing a stilbene biphenyl fluorescent whitening agent with a slight blue hue. Firstly, sodium sulfonate benzaldehyde and 4,4'-bis(diethoxyphosphonomethyl) are mixed with a solvent. ) biphenyl stirring and mixing, then add solid potassium hydroxide several times, keep warm for reaction, then evaporate the solvent under reduced pressure, quickly add sodium chloride aqueous solution, filter after cooling, and dry the filter cake to obtain a light yellow-green solid, which is slightly blue Tinted stilbene biphenyl optical brightener. The synthesis method of the present invention is simple, safe in operation, and the yield of the synthesized product is high and of good quality. Compared with the traditional process of using sodium methoxide, the yield of the product prepared by the present invention is increased by 4.5%, the purity is increased by 2%, and the Cost savings.

Description

technical field [0001] The invention belongs to the technical field of fluorescent whitening agents, and in particular relates to a method for synthesizing a stilbene biphenyl fluorescent whitening agent with a slight blue tone. Background technique [0002] 4,4-bis(2-disulfonate sodium styryl-)biphenyl (referred to as fluorescent whitening agent CBS-X) is one of the important fluorescent whitening agents in the structure of distyryl derivatives, the main application Used in textile, paper, detergent and other industries, it is an ideal additive for light industry and daily chemical industry, especially suitable for low temperature washing and whitening. It has blue fluorescence with a slight cyan hue, good whitening effect, and has the advantages of high temperature resistance, alkali resistance, chlorine bleaching resistance, and light resistance. It is currently the best fluorescent whitening agent used in the washing industry in the world. [0003] Patents CN 103755601B...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/32C07C309/32C09K11/06
Inventor 王振元弓玮张迪王红昆侯霞刘爽郭小龙于逢杰王金友王蓓盛洪波夏田
Owner 沈阳中化新材料科技有限公司
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