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Mixed toluylene biphenyl type fluorescent whitening agent and preparation method thereof

A technology of stilbene biphenyls and fluorescent whitening agents, which is applied in the field of fluorescent whitening agents, can solve the problems of easy stratification and easy precipitation of liquids, and achieves the effects of high solubility and stable storage.

Inactive Publication Date: 2013-02-13
山西青山化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention is aimed at CBS as a disulfonic 4,4'-stilbene biphenyl fluorescent whitening agent, and makes a CBS slurry and a high-scoring liquid. After a period of time, the slurry is easy to stratify. The liquid is prone to the problem of precipitation, and a mixed type stilbene biphenyl fluorescent whitening agent and its preparation method are provided

Method used

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  • Mixed toluylene biphenyl type fluorescent whitening agent and preparation method thereof
  • Mixed toluylene biphenyl type fluorescent whitening agent and preparation method thereof
  • Mixed toluylene biphenyl type fluorescent whitening agent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment １

[0021] (1) Synthesis of 4,4′-bis(dimethoxyphosphonomethyl)biphenyl:

[0022] Add 25.1 grams of 4,4′-dichloromethylbiphenyl and 7.4 grams of triethyl phosphonite into a 250ML four-neck flask, raise the temperature to 105~115°C, and keep it warm for 20 minutes. After all of them are dissolved, raise the temperature to 120~ 130°C, and evenly add the remaining 34 grams of triethyl phosphonite dropwise within 1 hour. After the addition, raise the temperature to 155~165°C within 1 hour, keep it warm for 8~10 hours, take a sample test, the content is >95%, Distill under reduced pressure to recover unreacted triethyl phosphonite, then cool down to 110°C, discharge the material, cool to room temperature and crystallize, and the precipitated white solid is 4,4'-bis(dimethoxyphosphonoform Base) 41 grams of biphenyl, the yield is 90.3%.

[0023] (2) Synthesis of mixed stilbene biphenyl fluorescent whitening agent:

[0024] In a 250ML three-neck flask, add 30 grams of 4,4'-diethoxyp...

Embodiment 2

[0039] A preparation method of a mixed type stilbene biphenyl fluorescent whitening agent, comprising the following steps:

[0040] Dissolve 4,4′-diethoxyphosphonomethylbiphenyl, sodium benzaldehyde o-sulfonate, and benzaldehyde 2,4-sodium disulfonate with a molar ratio of 1:1.2:1.2:1.1 in the organic solvent DMF Among them, sodium methoxide was added dropwise at 43°C, and the temperature was kept at 43°C for 10 hours, then the temperature was raised to 95°C, the temperature was kept for 2 hours, and the temperature was raised to 120°C, the solvent DMF was evaporated under reduced pressure, and 1.5 times the weight of the filter cake was added to the filter cake The water is dissolved and filtered at 90°C to remove impurities, concentrated and filtered, and dried to obtain the finished product.

Embodiment 3

[0042] A preparation method of a mixed type stilbene biphenyl fluorescent whitening agent, comprising the following steps:

[0043]Dissolve 4,4′-diethoxyphosphonomethylbiphenyl, sodium benzaldehyde o-sulfonate, and benzaldehyde 2,4-sodium disulfonate with a molar ratio of 1:1.2:1.2:1.1 in the organic solvent DMF Among them, sodium methoxide was added dropwise at 45°C, and the temperature was kept at 45°C for 10 hours, then the temperature was raised to 95°C, the temperature was kept for 2 hours, and the temperature was raised to 125°C, the solvent DMF was evaporated under reduced pressure, and 1.5 times the weight of the filter cake was added to the filter cake The water is dissolved and filtered at 90°C to remove impurities, concentrated and filtered, and dried to obtain the finished product.

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Abstract

The invention discloses a mixed toluylene biphenyl type fluorescent whitening agent and a preparation method thereof, relates to a fluorescent whitening agent used in industries of printing and dyeing, synthetic detergent and the like, and solves the problems that the current product is easy to layer and liquid is easy to precipitate. The method comprises the following steps of dissolving 4, 4'-diethoxy phosphonic methyl diphenyl, o-sulfonic acid sodium benzaldehyde and 2, 4-disulfonic acid sodium benzaldehyde into an organic solvent DMF (Dimethyl Formamide), dropwise adding sodium methoxide at 43-47 DEG C to react, and conducting a thermal reaction for a period of time; warming, reducing pressure, and steaming out the solvent DMF; and after a filter cake is dissolved and filtered with water to remove impurities, the filter cake is concentrated and filtered and dried to obtain a finished product. The product can be stored stably and has high solubility. After the product is put for 100 days at the room temperature, the product is still clear, colorless and deposit-free. During the temperature of 25 DEG C, the solubility in water can achieve 38 g / L.

Description

technical field [0001] The invention relates to a fluorescent whitening agent used in printing and dyeing, combined washing and other industries, in particular to a mixed-type stilbene biphenyl fluorescent whitening agent and a preparation method thereof. Background technique [0002] 4,4'-Stilbene biphenyl fluorescent whitening agent contains biphenyl, parent group and styrene group in its structure, it is very stable to light, it is rarely lost in the process of washing and dyeing, and the whitening effect is remarkable. And it does not change color during storage. It is known as a super fluorescent whitening agent and has developed rapidly in recent years. With the accelerated development of light textile industry, detergent and plastic industry, the domestic demand for optical brighteners will further increase. [0003] Fluorescent whitening agent CBS is a kind of 4,4′-stilbene biphenyl fluorescent whitening agent. It has excellent chlorine bleaching resistance, aci...

Claims

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Application Information

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IPC IPC(8): C09B67/22C09B23/14
Inventor 王雪亮杨晓波季东峰
Owner 山西青山化工有限公司
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