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Process for producing fluorescent whitening agent 5BM

A fluorescent whitening agent and ice water technology, applied in chemical instruments and methods, luminescent materials, styrene-based dyes, etc., can solve the problems of low product quality, and achieve the effects of simple preparation methods, avoiding dust pollution, and easy operation

Inactive Publication Date: 2009-05-13
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

[0005] The present invention provides a preparation method of fluorescent whitening agent 5BM in order to solve the problem of low product quality obtained by processing and preparing fluorescent whitening agent 5BM in the prior art

Method used

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  • Process for producing fluorescent whitening agent 5BM
  • Process for producing fluorescent whitening agent 5BM

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: the preparation method of a kind of fluorescent whitening agent 5BM, the steps are: according to the ratio of molar ratio 2:1, get cyanuric chloride and DSD acid and put into reactor, add appropriate amount of ice water (consumption according to every 200 -250 kg of DSD acid is added corresponding to the amount of 2000-2200 liters of ice water, cyanuric chloride is insoluble in water, the purpose is ice grinding), adjust the pH value to 1-1.5, and then add sodium carbonate to neutralize the reaction generated Hydrochloric acid, adjust the pH value to 6-6.5, after the amino value of DSD acid disappears, add aniline with a molar ratio of 2, and add 2 moles of N-methylethanolamine after the aniline disappears, and make the pH value 10-12 by adding NaOH , and then cooled to 5°C with ice water to precipitate the product, then filtered, dried, and pulverized to obtain the 5BM product.

Embodiment 2

[0016] Embodiment 2: solvent method is made granular 5BM product (contrast):

[0017] Add 375g of crushed ice and 300g of butanone into a 2000mL flask equipped with stirring, pH meter, thermometer, reflux condenser and dropping funnel, mix well and cool down to -7°C. Then add 50g of cyanuric chloride, add 50g of DSD acid under vigorous stirring, (full name 4,4'-diaminostilbene-disulfonic acid) keep the temperature ≤ 5°C under ice bath for 30-40 minutes 195mL15% sodium carbonate solution was added dropwise, so that the pH value of the reaction solution was maintained at 3-4 at first, and then to 5-6. After the disappearance of the DSD acid, an easy-to-stirrable tan-yellow homogeneous slurry was obtained. Then the temperature was raised to 20°C, and 25.2g of aniline was added dropwise within 5 minutes, and at the same time, 22g of 50% NaOH solution was added dropwise at 27-30°C, so that the pH value of the reaction solution was maintained at 4-5 at first, and then to 8.0-8.5. ...

Embodiment 3

[0018] Embodiment 3: take the present invention as example non-solvent method to manufacture granular 5BM product

[0019] Add 100g of crushed ice and 100g of water into a 2000mL beaker, stir evenly, add 10% hydrochloric acid to adjust the pH to 1-1.5, add 10g of cyanuric chloride for beating for 0.5 hours, then add 9.75g of DSD acid (solution Concentration in the range of 100-120g / L), while maintaining 5°C, add 2.78g (0.026mol) 10% sodium carbonate solution dropwise in 30-40 minutes to keep the pH at 5-5.5, Then adjust it to 6-6.5. After the amino value disappears, add 5.2g of aniline, and at the same time add 2.95g (0.028mol) of 10% sodium carbonate solution dropwise at 20-35°C to keep the pH between 7-7.5. After disappearing, add 4.8g of N-methyl monoethanolamine at one time, and heat it to 80°C, keep it warm for 1.5 hours, the pH value of the reaction solution is 10 at first, and then drops rapidly,

[0020] 2.2 g (0.055 mol) of 20% NaOH solution was added dropwise to mai...

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Abstract

The invention relates to a method for preparing a synthetic detergent and a ring whitening agent for printing industry, in particular to a method for preparing a fluorescent whitening agent 5BM. The method solves the problem that the product obtained through the prior method for processing and preparing the fluorescent whitening agent 5BM has low quality. The method comprises the following steps: cyanuric chloride and DSD acid are put into a reaction kettle and are added with ice water; the PH value of the mixture of the ice water, the cyanuric chloride and the DSD acid is regulated to between 1 and 1.5; the hydrochloric acid generated in the reaction is neutralized; the PH value is regulated to between 6 and 6.5; after the amido value of the DSD acid disappears, the hydrochloric acid is added with aniline; after the aniline disappears, N-methylethanolamine is added to the mixture; the PH value is finally regulated to between 10 and 12; the mixture is cooled to the temperature of 5 DEG C through the ice water so that a target product is precipitated out; and the target product is filtered, dried and pulverized to obtain the 5BM product.

Description

technical field [0001] The invention relates to a preparation method of a synthetic detergent and a ring brightener used in the printing and dyeing industry, in particular to a preparation method of a fluorescent whitening agent 5BM. Background technique [0002] Fluorescent whitening agent 5BM belongs to the structure of stilbene bistriazine, molecular formula C 38 h 38 N 12 o 8 S 2 Na 2 , [0003] [0004] Because of its superior performance, it is widely used in papermaking, printing and dyeing, washing and other industries. At present, 5BM produced according to foreign solvent production methods has always had triazine impurities (mainly referring to 2-hydroxy-4,6-dianiline-s-triazine, 2-morpholino-4,6-dianiline- s-triazine and 2-anilino-4,6-dimorpholino-s-triazine) content and heavy metal content are high, and production and use pollution are relatively large; while triazine content is low and heavy metal content is low in environmental protection However, du...

Claims

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Application Information

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IPC IPC(8): C09B23/14C09K11/06
Inventor 张成才李钢
Owner 山西青山化工有限公司
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