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Clean production process of p-aminoacetanilide

A technique for the production of aminoacetanilide, which is applied in chemical instruments and methods, organic dyes, monoazo dyes, etc., can solve the problems that aminoacetanilide production wastes cannot be effectively utilized, and reduce losses, reduce costs, Effect of Yield Improvement

Active Publication Date: 2019-08-23
SHANDONG WUYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a clean production process of p-aminoacetanilide to solve the problem that the p-aminoacetanilide production waste cannot be effectively utilized in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0014] 1. Synthesis of p-aminoacetanilide

[0015] 1. Nitration: Add 90g of concentrated sulfuric acid (98%) into a 250mL three-necked flask, stir, add 30g of acetanilide (99%) at 20~25℃ within 2~2.5 hours, and make it completely dissolved after the addition. Cool down to 7°C at 15-18°C, add mixed acid (comprised of 8.4g water; 8g 98% sulfuric acid and 14.4g 96% nitric acid) dropwise within 20 hours. After dripping, dilute in 200mL ice water and stir for 1 hour. After filtering, the filter cake is washed with 100 mL of water to neutrality, and the filtrate and washing water (about 250 mL containing about 24% sulfuric acid and a small amount of nitric acid) are recovered as PFS. The filter cake is p-nitroacetanilide.

[0016] 2. Reduction: Add 200g of water to a 1000mL three-necked flask, stir, add 40g of iron powder and 1g of acetic acid (98%), increase the temperature to 80℃, add p-nitroacetanilide in 3~3.5 hours, control the temperature at 72~75℃ . After the addition, keep for...

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Abstract

The invention discloses a clean production process for 4-aminoacetanilide. Waste sulfuric acid generated during 4-aminoacetanilide production and waste iron sludge generated from a reduction procedureare composited into PFS (polymerized ferrous sulfate). The clean production process includes putting the waste sulfuric acid and the waste iron sludge, both generated by a batch of 4-aminoacetanilide, into a reactor, wherein the molar ratio of iron in the sulfuric acid to iron in the ion sludge is (1.4-1.6):1; increasing the temperature while stirring, and keeping the temperature for two hours toform ferric salt; transferring hot filtrated stock into another reactor, and adding sodium chlorate in batches, wherein the molar ratio of ion in the sodium chlorate to the iron in the iron sludge is0.15:1; directly compositing 4-aminoacetanilide slurry from the reduction procedure into scarlet acid-proof 4BS. The clean production process has the advantages that dangerous waste from 4-aminoacetanilide production is recycled, so that costs of raw materials are reduced, and clean production is achieved; diazotization compounding is conducted directly after reduction of the 4-aminoacetanilide to obtain the scarlet acid-proof 4BS, so that procedures for the 4-aminoacetanilide are simplified, losses are reduced, the yield of the 4-aminoacetanilide can be increased to more than 15%, and energyconservation and emission reduction are realized.

Description

Technical field [0001] The invention relates to the technical field of dye intermediate production, in particular to a clean production process of p-aminoacetanilide. Background technique [0002] P-aminoacetanilide, also known as N-acetyl-p-phenylenediamine, is an important dye intermediate. It is mainly used to prepare disperse dyes, direct dyes, acid dyes and reactive dyes, such as disperse yellow G, direct acid-resistant scarlet 4BS, acid-resistant products Red 6B, reactive blue AG, etc. There are currently two methods for industrial production of p-aminoacetanilide. Method 1. Acetanilide is prepared by nitration with mixed acid and then reduction with iron powder. Method 2: p-nitroaniline reacts with acetic anhydride under the action of a catalyst to prepare p-nitroacetanilide, and then it is obtained by reduction with iron powder. The three wastes in this method are equivalent to the first method, but the raw material acetic anhydride is a precursor drug, and the country...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/01C09B29/16C01G49/14
Inventor 于文民石铭兆孙兆官刘建国李刚
Owner SHANDONG WUYANG CHEM
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