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The preparation method of p-nitrophenol

A technology for p-nitrophenol and p-nitroaniline, which is applied in the field of preparation of p-nitrophenol, can solve problems such as high temperature, pressurization, waste water discharge, etc., and achieves the effects of reducing discharge, simple treatment method and safe process route

Active Publication Date: 2017-01-04
QUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has a high yield, problems such as pressurization, high temperature, and serious wastewater discharge are involved in the reaction process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Salt-forming reaction: add 40g of water to a 250ml four-neck flask equipped with a thermometer, a spherical condenser, and mechanical stirring, and slowly add 40g of concentrated sulfuric acid under the condition of rapid stirring and air bath cooling, observe the temperature, and change the temperature of the oil bath. At 120°C, add 13.8g of p-nitroaniline three times, heat up to reflux after addition, react for 10 minutes until the solution is clear, remove the oil bath, air cool to below 50°C, change the water bath to cool to room temperature, a large amount of white solids precipitate out.

[0026] (2) Diazotization reaction: Transfer the reaction solution from the previous step to a low-temperature constant temperature bath, control the temperature to 0-5°C, slowly add a saturated aqueous solution containing 7g of sodium nitrite dropwise, and keep warm for 2 hours after the dropwise addition is completed. Add an appropriate amount of urea to the reaction solutio...

Embodiment 2

[0033] (1) Salt-forming reaction: add 40g of water to a 250ml four-neck flask equipped with a thermometer, a spherical condenser, and mechanical stirring, and slowly add 40g of concentrated sulfuric acid under the condition of rapid stirring and air bath cooling, observe the temperature, and change the temperature of the oil bath. At 120°C, add 13.8g of p-nitroaniline three times, heat up to reflux after addition, react for 10 minutes until the solution is clear, remove the oil bath, air cool to below 50°C, change the water bath to cool to room temperature, a large amount of white solids precipitate out.

[0034] (2) Diazotization reaction: transfer the reaction solution from the previous step to a low-temperature constant temperature bath, and control the temperature to 0-5°C. Slowly add a saturated aqueous solution containing 7g of sodium nitrite dropwise, and keep warm for 2 hours after the dropwise addition. After the warming is over, add an appropriate amount of urea to th...

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PUM

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Abstract

The invention discloses a preparation method of p-nitrophenol. The method comprises the following steps: mixing a raw material, namely paranitroaniline, with a sulfuric acid aqueous solution and carrying out salt-forming reaction; carrying out diazotization reaction on the reaction product with a saturated sodium nitrite solution; hydrolyzing the obtained heavy nitride to obtain a p-nitrophenol crude product and a mother liquid; and recrystallizing the p-nitrophenol crude product to obtain a product, namely the pure p-nitrophenol product, wherein the mother liquid is recycled and reused. The preparation method is safe in process route; the operation steps are simple and convenient; the technological design is environment-friendly; most of mother liquid basically can be repeatedly recycled and reused; and the recycling and reusing treatment method is simple.

Description

[0001] (1) Technical field [0002] The invention belongs to the technical field of chemical product preparation, and in particular relates to a preparation method of p-nitrophenol. [0003] (2) Background technology [0004] p-nitrophenol, colorless to pale yellow crystalline powder, stable in structure, soluble in hot water, alcohol, ether, etc., is an important fine chemical raw material and intermediate, and one of the key raw materials for the production of paracetamol. Manufacturing, dyes and other fields are widely used, so p-nitrophenol, as a traditional fine chemical raw material, has a large demand. [0005] At present, p-nitrophenol is mostly prepared by high-temperature pressurized hydrolysis in industry. It is prepared by reacting p-chloronitrobenzene with caustic soda at 150-173°C and a pressure of about 1 MPa for 2-4 hours. Although this method has a higher yield, problems such as pressurization, high temperature, and serious waste water discharge are involved i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/22C07C201/12
Inventor 李杰金懿吕延文李月李亚拿金耀来
Owner QUZHOU UNIV
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