Crystal transfer method for triazinyl amino toluylene fluorescent brightening agent

A technology of triazine-aminostilbene and amino-stilbene, which is applied in the field of fluorescent whitening agents and can solve problems such as increased sewage treatment costs, environmental pollution, and large amounts of waste water

Inactive Publication Date: 2012-06-20
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

In production, the requirements for equipment are high, and a vacuum dryer is required, and a large amount of waste water is

Method used

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  • Crystal transfer method for triazinyl amino toluylene fluorescent brightening agent
  • Crystal transfer method for triazinyl amino toluylene fluorescent brightening agent
  • Crystal transfer method for triazinyl amino toluylene fluorescent brightening agent

Examples

Experimental program
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Effect test

Embodiment 1

[0021] A method for crystal transformation of a triazinylaminostilbene fluorescent whitening agent, comprising the following steps:

[0022] In a 1L glass container, add 93 grams of ice-water mixture, 10 grams of cyanuric chloride, dropwise add 9.6 grams of 4,4'-diaminostilbene-2,2'- For the sodium salt solution of disulfonic acid, adjust the pH to about 5 with soda ash solution continuously during the dropping process. After the amino value disappears, raise the temperature to 30±2°C and keep it warm for 30 minutes; add 5.0 grams of aniline to react, and adjust the PH with soda ash solution =8 or so, after the amino value disappears, heat up to 40°C and keep warm for 30 minutes; add 5.8 grams of morpholine, then add 80 grams of pre-prepared β-type CXT seed slurry with a content of 10%, react for 30 minutes, and heat up to Keep warm at 100°C, add sodium hydroxide after 5 minutes, adjust the pH to about 11, reflux for 6 hours, cool down to 60°C after the reaction, filter to obt...

Embodiment 2

[0024] A method for crystal transformation of a triazinylaminostilbene fluorescent whitening agent, comprising the following steps:

[0025] In a 1L glass container, add 95 grams of ice-water mixture, 10 grams of cyanuric chloride, dropwise add 9.8 grams of 4,4'-diaminostilbene-2,2'- For the sodium salt solution of disulfonic acid, adjust the pH to about 5 with soda ash solution continuously during the dropping process. After the amino value disappears, heat up to 50±2°C for 30 minutes; add 5.5 grams of aniline to react, and continuously use soda ash solution Adjust the pH to about 9, and after the amino value disappears, heat up to 60°C and keep warm for 30 minutes; add 5.2 grams of morpholine, and then add 31.5 grams of pre-prepared β-type AMS seed slurry with a content of 20%, and react for 20 minutes. Heat up to 100°C and keep it warm. After 5 minutes, add sodium hydroxide to adjust the pH to about 11. Reflux for 4 hours. After the reaction, cool down to 70°C and filter to...

Embodiment 3

[0027] A method for crystal transformation of a triazinylaminostilbene fluorescent whitening agent, comprising the following steps:

[0028] In a 1L glass container, add 98 grams of ice-water mixture, 10 grams of cyanuric chloride, dropwise add 9.7 grams of 4,4'-diaminostilbene-2,2'- For the sodium salt solution of disulfonic acid, adjust the pH to about 5 with soda ash solution continuously during the dropping process. After the amino value disappears, raise the temperature to 30±2°C and keep it for 30 minutes; add 5.3 grams of aniline, and constantly adjust it with soda ash solution PH=8 or so, after the amino value disappears, raise the temperature to 70°C and keep it warm for 30 minutes; add 14.5 grams of methylamine aqueous solution with a mass fraction of 40%, and then add 10 grams of pre-prepared 40% β-type fluorescent whitening agent RKH seed crystal slurry, after reacting for 15 minutes, heat up to 100°C and keep it warm, add sodium hydroxide to adjust pH=11 after 5 m...

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Abstract

The invention belongs to the technical field of fluorescent brightening agent, in particular to a crystal transfer method for triazinyl amino toluylene fluorescent brightening agent. The invention mainly provides the crystal transfer method for the triazinyl amino toluylene fluorescent brightening agent, which is used for transferring the unstable straw yellow Alpha unformed triazinyl amino toluylene fluorescent brightening agent into stable white Beta type triazinyl amino toluylene fluorescent brightening agent. The crystal transfer method comprises the steps as follows: 1, mixing water with Beta type triazinyl amino toluylene fluorescent brightening agent to obtain Beta type seed crystal slurry; 2, adding the Beta type seed crystal slurry into the third condensation reaction liquid in the manufacturing process of the triazinyl amino toluylene fluorescent brightening agent to undergo backflow reaction for 1 to 6 hours; and 3, after the reaction, reducing the temperature to 40 to 100 DEG C, filtering, and drying to obtain the Beta type triazinyl amino toluylene fluorescent brightening agent. The invention has the advantages of low cost, zero contamination, simplicity in treatment, and the like.

Description

technical field [0001] The invention belongs to the technical field of fluorescent whitening agents, and in particular relates to a crystal form transformation method of triazinylaminostilbene fluorescent whitening agents. Background technique [0002] Triazinylamino stilbene fluorescent whitening agent is a class of organic compounds obtained through three consecutive condensation reactions. The first condensation reaction is the condensation of one molecule of DSD acid (4,4'-diaminostilbene-2,2'-disulfonic acid) with two molecules of cyanuric chloride to obtain a condensation product, and at the same time produce two molecules of cyanuric chloride Hydrogen chloride; the second condensation reaction is the condensation of the first condensation product with an amino-containing aromatic compound to obtain a secondary condensation product, while producing two molecules of hydrogen chloride; the third condensation reaction is the secondary condensation product and an organic c...

Claims

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Application Information

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IPC IPC(8): C09B67/48C09B23/14C09K11/06
Inventor 季东峰张成才杨晓波
Owner 山西青山化工有限公司
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