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Continuous production process of p-nitrophenol

A production process, p-nitrophenol technology, applied in the field of waste sulfuric acid concentration, can solve the problems of cooling crystallization process error, low automation level, low yield, etc.

Inactive Publication Date: 2020-10-23
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Because the method is easy to get raw materials and simple process, most of the downstream products do not have high requirements on its quality. Therefore, the production of p-nitrophenol mostly adopts relatively primitive pure manual operation, and the automation level is low, but manual operation leads to feeding, reaction process and There are large errors in the cooling crystallization process, resulting in poor product quality and low yield

Method used

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  • Continuous production process of p-nitrophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Such as figure 1 As shown, a continuous production process of p-nitrophenol, the continuous production process is based on a set of continuous production system, the front end of the continuous production system is set as a nitration tank, and the two ends of the nitro tank are respectively equipped with chlorobenzene spray tanks and acid spray tanks , the downstream of the nitration tank is provided with a settling tank, the downstream of the settling tank is equipped with a neutralization tank, the downstream of the neutralization tank is equipped with a first-level washing tank, the downstream of the water-washing tank is equipped with a first-level drying oven, and the downstream of the first-level drying oven is set There is a hydrolysis kettle, and the downstream of the hydrolysis kettle is equipped with a pickling kettle, the downstream of the pickling kettle is equipped with a second-level washing kettle, and the downstream of the second-level washing kettle is e...

Embodiment 2

[0046] The difference between this embodiment and embodiment 1 is:

[0047] A continuous production process of p-nitrophenol, the continuous production process comprises the following steps:

[0048] 1). Nitrification: transfer anhydrous chlorobenzene to the chlorobenzene spray tank, mix the concentrated sulfuric acid and concentrated nitric acid and transfer to the acid spray tank, and add nitrite as the nitration positioning agent, and spray the spray tank into the nitration tank at the same time Inside, control the reaction temperature inside the nitration tank to be 40°C, and the reaction pressure to be 0.15Mpa. After the spray is complete, stir at a stirring rate of 500r / min until the amount of each substance does not change;

[0049] The molar ratio of anhydrous chlorinated benzene, sulfuric acid, nitric acid and nitrite is 1:1:3:0.1;

[0050] 2). Settling: transfer the nitrochlorobenzene mixture after the nitration reaction and the waste sulfuric acid produced by nitra...

Embodiment 3

[0062] The difference between this embodiment and embodiment 1, 2 is:

[0063] A continuous production process of p-nitrophenol, the continuous production process comprises the following steps:

[0064] 1). Nitrification: transfer anhydrous chlorobenzene to the chlorobenzene spray tank, mix the concentrated sulfuric acid and concentrated nitric acid and transfer to the acid spray tank, and add nitrite as the nitration positioning agent, and spray the spray tank into the nitration tank at the same time Inside, control the reaction temperature inside the nitration tank to be 60°C, and the reaction pressure to be 0.3Mpa. After the spray is complete, stir at a stirring rate of 800r / min until the amount of each substance does not change;

[0065] The molar ratio of anhydrous chlorinated benzene, sulfuric acid, nitric acid and nitrite is 5:10:20:1;

[0066] 2). Settling: transfer the nitrochlorobenzene mixture after the nitration reaction and the waste sulfuric acid produced by nit...

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Abstract

The invention relates to a continuous production process of p-nitrophenol. The continuous production process is based on a set of continuous production system, all devices in the continuous productionsystem cooperate with one another, continuous work is achieved, production efficiency is guaranteed, and the continuous production process comprises the specific steps that chlorobenzene is used as araw material for nitration, and p-nitrophenol is obtained after a product is subjected to sedimentation, neutralization, sufficient washing, drying, hydrolysis, acid pickling, water washing and secondary drying; according to the invention, chlorobenzene is used as a substrate; first, p-nitrochlorobenzene is synthesized, hydrolyzing is performed under an alkaline condition to obtain p-nitrophenol;according to the method, continuous production is carried out by reducing high-power energy consumption steps and using conventional steps so that the energy consumption during continuous productionis reduced, the production cost is reduced, the economic benefit is further improved, waste liquid generated in each step can be repeatedly and continuously utilized, the post-treatment is relativelysimple, the pollution is reduced, and the environment is protected; the yield of the finally obtained p-nitrophenol is 90% or above, and the purity of the p-nitrophenol reaches 95% or above.

Description

technical field [0001] The invention relates to the technical field of waste acid concentration, and more precisely relates to a method for concentrating waste sulfuric acid. Background technique [0002] p-Nitrophenol, pure product is light yellow crystal, odorless, melting point 114-116°C, boiling point 279°C, flash point 169°C, relative density 1.479 (20 / 4°C), slightly soluble in water (1.6%, 25°C) at room temperature ℃), not easy to volatilize with steam, easily soluble in ethanol, chloroform and ether, when dissolved in acid solution, the light yellow gradually recedes, between PH3~4, almost colorless, when dissolved in lye, the color deepens and can sublimate. [0003] p-Nitrophenol has a wide range of uses, it can be used as dye intermediates, raw materials for medicines and pesticides, acid-base indicators, analytical reagents, leather preservatives, and also used as intermediates for dyes, medicines and pesticides in organic synthesis body. p-Nitrophenol is also a...

Claims

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Application Information

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IPC IPC(8): C07C205/22C07C201/12C07C201/16
CPCC07C201/08C07C201/12C07C201/16C07C205/12C07C205/22
Inventor 黄中桂袁晓林朱礼华杨镭王彪
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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