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Treatment method of waste acid generated by synthesis of m-nitroacetophenone

A technology for the treatment of nitroacetophenone and waste acid, which is applied in the chemical industry, can solve the problems of producing a large amount, the production equipment is corrosive, and cannot meet the requirements of sustainable development, and achieves the effect of reducing pressure.

Pending Publication Date: 2019-05-24
盐城日精科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage of this process is that a large amount of waste acid containing organic matter and waste water containing organic matter will be produced during the nitrification reaction, especially the waste acid is corrosive to the production equipment and cannot meet the requirements of sustainable development

Method used

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  • Treatment method of waste acid generated by synthesis of m-nitroacetophenone
  • Treatment method of waste acid generated by synthesis of m-nitroacetophenone
  • Treatment method of waste acid generated by synthesis of m-nitroacetophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 69.6g of concentrated sulfuric acid into a 500ml beaker equipped with mechanical stirring and a thermometer, specifically mix 77.06g of concentrated sulfuric acid with a concentration of 92.04% and 19.54g of concentrated sulfuric acid with a concentration of 98%, and then pipette 15ml as a compounding acid 27g of sulfuric acid; start stirring, and slowly add 15g of acetophenone dropwise under the condition of keeping the temperature not exceeding -7°C, so that the reaction temperature is controlled below -10°C and slowly add a mixed acid nitrating reagent, specifically 10ml of fuming nitric acid Pipette and mix with 15ml of the aforementioned mixture of concentrated sulfuric acid, control the speed of dripping, and keep warm for 5 minutes after the completion of the dropwise addition. After the reaction is completed, pour the reaction solution into a beaker containing 100g of ice-water mixture, keep stirring rapidly, and wait until the ice-water mixture is filled. Co...

Embodiment 2

[0036] Add 69.6g of concentrated sulfuric acid into a 500ml beaker equipped with mechanical stirring and a thermometer, specifically mix 78.64g of concentrated sulfuric acid with a concentration of 92.55% and 17.96g of concentrated sulfuric acid with a concentration of 98%, and then pipette 15ml as a compounding acid 27g of sulfuric acid; start stirring, and slowly add 15g of acetophenone dropwise under the condition of keeping the temperature not exceeding -7°C, so that the reaction temperature is controlled below -10°C and slowly add a mixed acid nitrating reagent, specifically 10ml of fuming nitric acid Pipette and mix with 15ml of the aforementioned mixture of concentrated sulfuric acid, control the speed of dripping, and keep warm for 5 minutes after the completion of the dropwise addition. After the reaction is completed, pour the reaction solution into a beaker containing 100g of ice-water mixture, keep stirring rapidly, and wait until the ice-water mixture is filled. Co...

Embodiment 3

[0039] Add 69.6g of concentrated sulfuric acid in a 500ml beaker equipped with mechanical stirring and a thermometer, specifically after mixing 78.46g of 92.22% concentration with 18.14g of concentration 98% concentration of sulfuric acid, then pipette 15ml of sulfuric acid 27g as a compounding acid; Start stirring, and slowly add 15g of acetophenone dropwise under the condition that the temperature does not exceed -7°C, so that the reaction temperature is controlled below -10°C and slowly add a mixed acid nitration reagent, specifically 10ml of fuming nitric acid and 15ml of the above-mentioned pipette Take the mixed concentrated sulfuric acid mixture, control the dropping speed, keep warm for 5 minutes after the dropping is completed, after the reaction is completed, pour the reaction solution into a beaker containing 100g of ice-water mixture, keep stirring rapidly, until the ice is completely melted and vacuum Suction filtration, press dry the solid as much as possible, was...

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Abstract

The invention discloses a treatment method of waste acid generated by synthesis of m-nitroacetophenone. The waste acid generated by an acetophenone nitration reaction is extracted with acetophenone atthe normal temperature 1-3 times, and liquid separation is carried out to obtain waste acid A; the waste acid A is frozen and stirred at a temperature ranging from -5 to -20 DEG C, and filtration iscarried out to obtain waste acid B; the waste acid B is distilled under the conditions of negative pressure and temperature of 170-210 DEG C to obtain waste acid C, the mass concentration of sulfuricacid in the waste acid C is 92% or above, and COD is 400-1200 mg / L. The treatment method of the waste acid generated by the synthesis of the m-nitroacetophenone has the advantages that the waste acidgenerated by the synthesis of the m-nitroacetophenone is extracted, frozen and distilled to obtain the waste acid C of which the mass concentration of the sulfuric acid is 92% or above, and the wasteacid C can be used for the nitration reaction of the synthesis of the m-nitroacetophenone repeatedly to achieve recycling of the waste acid.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for treating waste acid produced by synthesizing m-nitroacetophenone. Background technique [0002] m-Nitroacetophenone is an important intermediate in organic synthesis, and has important applications in the preparation of phenylephrine, zaleplon, metal complex anticancer drugs and the synthesis of photosensitive functional polymer materials. At present, m-nitroacetophenone is generally prepared in industry by the nitration reaction process of fuming nitric acid-sulfuric acid system. The large heat capacity enables the temperature of the reaction to be effectively controlled. Because concentrated sulfuric acid can be miscible with most organic matter, the contact between organic matter and nitric acid is increased, which is beneficial to the nitrification reaction. However, the disadvantage of this process is that a large amount of waste acid con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/45
Inventor 柏洪来徐杰武
Owner 盐城日精科技有限公司
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