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Preparation method of environment-friendly zinc-free cationic dye

A zinc cation, environment-friendly technology, applied in azo dyes, organic dyes, onium-based azo dyes, etc., can solve the problems of excessive zinc concentration, harsh dye production environment, and increased raw material costs, and achieve low zinc content in products , the production process is environmentally friendly, and the effect of industrial application prospects is good

Active Publication Date: 2010-06-09
杭州璟江瑞华科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In the existing technology, the acid binding agent (zinc oxide) used in the methylation reaction and the precipitation agent (zinc chloride) used in the salting out are all zinc salts, which causes the zinc concentration in the existing cationic dyes to exceed the standard greatly. key
At the same time, halogenated hydrocarbons such as dichloroethane are generally used as solvents in the methylation reaction. This type of solvent is a toxic and harmful solvent, which is the main reason for the poor production environment of the dye and increases the cost of raw materials.

Method used

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  • Preparation method of environment-friendly zinc-free cationic dye
  • Preparation method of environment-friendly zinc-free cationic dye
  • Preparation method of environment-friendly zinc-free cationic dye

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0028] 35.6 kilograms (0.1mol) that have been converted into raw material A shown in formula (II) are stirred with 534 kilograms of water in the enamel reactor, add 8.1 kilograms (0.2mol) of magnesium oxide that have been reduced and continue stirring, heating and Keep the temperature at 35°C, slowly add 19.3 kilograms (0.15mol) of 98% dimethyl sulfate, keep warm and stir for 5 hours after adding, monitor the reaction solution with TLC without Compound A as the end of the reaction, slowly add 160.2 kilograms of chlorine Sodium chloride, stirred for 6 hours, filtered, and the filter cake was dried to obtain 39.9 kg of environmentally friendly zinc-free cationic dyes, with a molar yield of 98.0%, moisture ≤ 7%, and zinc content ≤ 50ppm.

Embodiment 2

[0030] The preparation process is substantially the same as the method of Example 1. The difference from Example 1 is that the amount of solvent water added is 712 kilograms, and the amount of sodium chloride added is 213.6 kilograms to obtain 38.7 kilograms of environmentally friendly zinc-free cationic dyes. Yield 95.1%, moisture ≤ 7%, zinc content ≤ 40ppm.

Embodiment 3

[0032] The preparation process is substantially the same as the method of Example 1. The difference with Example 1 is that the addition of solvent water is 1068 kilograms, and the amount of sodium chloride added is 284.8 kilograms to obtain 36.6 kilograms of environmentally friendly zinc-free cationic dyes. Yield 89.9%, moisture ≤ 7%, zinc content ≤ 30ppm.

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Abstract

The invention relates to a preparation method of an environment-friendly zinc-free cationic dye. The preparation method comprises the following steps of: dissolving a compound A shown as the formula (II) in a solvent, and under the presence of an acid catcher, stirring and reacting the compound A with dimethyl sulfate at 20-50 DEG C for 1-12 hours; after the reaction ends, salting out by using metal chlorides as a separation agent; and filtering and drying a filter cake to obtain the environment-friendly zinc-free cationic dye. The zinc content of zinc in the environment-friendly zinc-free cationic dye is not more than 30-250ppm and reaches the specification that the legal limit of zinc in the dye is less than 1,500ppm of Europe ETAD (The Ecological and Toxicological Association of Dyes and Organic Pigments Manufacturers). The process replaces hazardous and noxious solvents such as dichloroethane, and the like in the traditional process with green solvents, thus compared with the prior art, the environment-friendly zinc-free cationic dye has the advantages of simple operation, safe and reliable production, high reaction yield, low production cost, environmental protection, and the like.

Description

(1) Technical field [0001] The invention relates to a preparation method of an environment-friendly zinc-free cationic dye. (2) Background technology [0002] Before the present invention, in common cationic blue X-GRL, because heavy metal zinc content is high, and zinc is a kind of poisonous to human body restricted by European ETAD (Association of Dyestuff Manufacture Industrial Ecology and Toxicology) and U.S. ADMI (American Dyestuff Manufacture Association) Heavy metals, according to ETAD regulations, the allowable limit of zinc in dyes should be <1500ppm (1500mg / kg), but in the production of cationic dyes, zinc chloride is usually added to precipitate the dyes, which results in tens of thousands of ppm of zinc in cationic dyes , which greatly exceeds the limit stipulated by ETAD, so it cannot enter the international market in large quantities. [0003] The existing cationic blue X-GRL synthesis process on the market is as follows: [0004] Diazotization reaction: ...

Claims

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Application Information

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IPC IPC(8): C09B44/02
Inventor 贾建洪俞蒙高建荣吴士敏任斌高金华
Owner 杭州璟江瑞华科技有限公司
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