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Synthesis method for 3-nitryl-4-hydroxyl phenylarsonic acid

A technology of hydroxyphenylarsinic acid and a synthesis method, applied in the chemical field, can solve the problems of inability to recycle the reaction solution, troublesome waste water treatment, large consumption of raw materials, etc., and achieve the effects of low cost, high utilization rate of raw materials and less pollution

Active Publication Date: 2013-04-17
ZHEJIANG RONGYAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a 3-nitro-4-hydroxyphenylarsonic acid synthesis process in view of the large consumption of raw materials, low utilization rate, the reaction solution can not be recycled, and troublesome waste water treatment, etc., to provide a 3-nitro- 4-Hydroxyphenylarsine Synthetic Method

Method used

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  • Synthesis method for 3-nitryl-4-hydroxyl phenylarsonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 500kg of arsenic acid aqueous solution (mass concentration 85%), 100kg of o-nitroaniline, 10kg of chloroform, and 0.5kg of β-cyclodextrin into a 2000L enamel pot. When ready, start stirring and heat up, and the reaction temperature is controlled at 135~ 160°C, start the reaction timer, and the reaction time is about 5.5 hours. After the reaction, turn off the steam, concentrate and recover the dehydrating agent under normal pressure, and obtain the concentrated liquid. Filter after cooling to obtain filter cake A and filtrate A. The filter cake A is 3-nitro-4-aminophenylarsine acid condensation material, and the filtrate A is recycled. Add water to the filter cake A and raise the temperature to 70 ° C. Add liquid alkali to adjust the pH value to 4 After dissolving, adsorbed by an adsorbent, cool to 55°C and filter to obtain filter cake B and filtrate B filtrate, add alkali to hydrolyze the B filtrate, react for a certain time and temperature, and obtain 3-nitro-4-hyd...

Embodiment 2

[0024] Add 1200kg of arsenic acid aqueous solution (mass concentration 85%), 100kg of o-nitroaniline, 10kg of polyacrylamide, 0.5kg of β-cyclodextrin into a 2000L enamel pot. When ready, start stirring and heat up, and the reaction temperature is controlled at 135- 160°C, start the reaction timing, the reaction time is about 5.0 hours, after the reaction is over, turn off the steam, concentrate and recover the dehydrating agent under normal pressure, and obtain the concentrated liquid, add water to the condensed liquid for analysis and release, and stir for 0.5 h to obtain the reaction liquid, the reaction liquid Filter after cooling to obtain filter cake A and filtrate A. The filter cake A is 3-nitro-4-aminophenylarsine acid condensation material, and the filtrate A is recycled. Add water to the filter cake A and raise the temperature to 70 ° C. Add liquid alkali to adjust the pH value to 12 After dissolving, adsorbed by an adsorbent, cool to 55°C and filter to obtain filter c...

Embodiment 3

[0026] Add 900kg of arsenic acid aqueous solution (mass concentration 85%), 100kg of o-nitroaniline, 10kg of tetrachloroethylene, 0.5kg of n-octanoic acid into a 2000L enamel pot. When ready, stir and heat up. The reaction temperature is controlled at 135-160°C. Start the reaction timing, and the reaction time is about 5.5 hours. After the reaction is over, turn off the steam, concentrate and recover the dehydrating agent under normal pressure, and obtain the concentrated liquid. Add water to the condensed liquid for analysis and release, and stir for 1 hour to obtain the reaction liquid. The reaction liquid is cooled and filtered. Filter cake A and filtrate A are obtained, filter cake A is 3-nitro-4-aminophenylarsine acid condensation material, filtrate A is recycled, filter cake A is heated to 70°C by adding liquid alkali to adjust the pH value to 14 after being dissolved and then adsorbed After absorbing the agent, cool to 55°C and filter to obtain the filter cake B and filt...

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Abstract

The invention discloses a synthesis method for 3-nitryl-4-hydroxyl phenylarsonic acid. The synthesis method for the 3-nitryl-4-hydroxyl phenylarsonic acid comprises the steps of performing condensation reaction, recovering a dehydrating agent, obtaining condensation liquid, cooling and filtering, recycling, hydrolyzing, acidifying, filtering, adjusting the pH, cooling and crystallizing, centrifugally dehydrating, drying and the like. The synthesis method for the 3-nitryl-4-hydroxyl phenylarsonic acid is simple to operate; the utilization ratio of raw materials is high; the cost is low; and environmental friendliness is achieved.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for synthesizing 3-nitro-4-hydroxyphenylarsine. Background technique [0002] Roxarsine (chemical name: 3-nitro-4-hydroxyphenylarsine acid), is light yellow, odorless, tasteless crystalline powder, belongs to organic arsine preparations feed additive, mainly used in chicken and pig feed , as a feed additive for livestock and poultry, it not only plays the nutritional role of supplementing the essential trace element arsenic, but also has an important medicinal effect, which can promote protein synthesis, change the metabolism of intestinal cells, and inhibit the growth of harmful bacteria in the intestinal tract , which plays the role of growth promoter and antibacterial agent, is a highly safe multifunctional feed additive, and has been widely used in many countries and regions such as the United States, Canada, Latin America, and Southeast Asia. According to the repor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/76
Inventor 陈仁尔陈建华吴凤洁陈建平
Owner ZHEJIANG RONGYAO CHEM
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