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Comprehensive development separation method of m-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene mixture

A chloronitrobenzene meta-oil, separation method technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of low utilization value, imperfect separation method, low economic value, etc. The effect of high utilization rate, improved reaction efficiency and product quality, and shortened reaction time

Active Publication Date: 2019-11-12
SHANGYU XIES CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is to utilize halogen derivatives containing nitro on the aromatic rings of m-chloronitrobenzene, p-chloronitrobenzene and o-chloronitrobenzene, and p-chloronitrobenzene and o-chloronitrobenzene can be produced in the absence of a catalyst Ammonification with ammonia water, m-chloronitrobenzene needs to be ammonified in the presence of a catalyst, and the separation of p-chloronitrobenzene and o-chloronitrobenzene and m-chloronitrobenzene is realized under the situation of using a small amount of water, and the separation of the product The quality has been improved, but the product utilization value is low, the economic value is not high, and the separation method is not perfect, there is still a lot of room for improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add meta oil, potassium fluoride and tetrabutylammonium chloride with a mass ratio of 350:67:4.1 into the still, and raise the temperature to 115°C under the vacuum condition of -0.08MPa , discharge the water vapor in the system, then continue to heat up to 140°C, react with ultrasonic power at 20kHz for 2h, cool down to 73°C, add water, separate the oil layer and water layer with a coke content of 0.3%, and the water layer is decolorized For the production of potassium fluoroborate.

[0027] (2) Put the oil layer in an ice-water bath at -5°C, stir and crystallize at a rate of 50 r / min for 4 hours, filter and separate, and take the filtrate to obtain o-fluoronitrobenzene.

[0028] (3) Place the separated crystals in a rectification tower, first heat to 100°C to melt the crystals, continue to heat up, set the tower top temperature to 205°C, and the tower bottom temperature to 235°C, rectify through a non-condensing collector, The crude product of p-fluoronitrobenzen...

Embodiment 2

[0032] (1) Add meta-oil, potassium fluoride and tetrabutylammonium chloride with a mass ratio of 350:67:4.5 into the still, and raise the temperature to 120°C under a vacuum condition of -0.07MPa , discharge the water vapor in the system, then continue to heat up to 145°C, react with ultrasonic power of 27kHz for 3h, cool down to 78°C, add water, separate the oil layer and water layer with a coke content of 0.3%, and the water layer is decolorized For the production of potassium fluoroborate.

[0033] (2) Put the oil layer in an ice-water bath at 0° C., stir and crystallize at 100 r / min for 6 h, filter and separate, and take the filtrate to obtain o-fluoronitrobenzene.

[0034] (3) Place the separated crystals in a rectification tower, first heat to 120°C to melt the crystals, continue to heat up, set the tower top temperature to 210°C, and the tower bottom temperature to 240°C, rectify through a non-condensing collector, The crude product of p-fluoronitrobenzene is extracted...

Embodiment 3

[0038] (1) Add meta oil, potassium fluoride and tetrabutylammonium chloride with a mass ratio of 350:67:4.3 into the still, and raise the temperature to 118°C under the vacuum condition of -0.075MPa , discharge the water vapor in the system, then continue to heat up to 142°C, react with ultrasonic power of 22kHz for 2.5h, cool down to 75°C, add water, separate the oil layer and water layer with a coke content of 0.3%, and the water layer is decolorized Later used in the production of potassium fluoroborate.

[0039] (2) Put the oil layer in an ice-water bath at -2°C, stir and crystallize at a rate of 60 r / min for 5 h, filter and separate, and take the filtrate to obtain o-fluoronitrobenzene.

[0040] (3) Place the separated crystals in a rectification tower, first heat to 105°C to melt the crystals, continue to heat up, set the tower top temperature to 208°C, and the tower bottom temperature to 238°C, rectify through a non-condensing collector, The crude product of p-fluoronitr...

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Abstract

The invention provides a comprehensive development separation method of m-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene mixture. The comprehensive development separation method ofm-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene mixture comprises following steps: the m-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene mixture, potassium fluoride, and tetrabutylammonium chloride are introduced into a distiller, under vacuum conditions, water vapour in the system is discharged, the temperature is increased to 140 to 145 DEG C, ultrasonicreaction is carried out, the temperature is reduced to 73 to 78 DEG C, water is added, and an oil layer and a water layer are obtained through separation; the oil layer is introduced into an ice waterbath for stirring crystallization, filtering is carried out to obtain filtrate o-fluoronitrobenzene; a crystal product obtained through separation is introduced into a rectifying tower, crystal melting is carried out, tower top temperature is controlled to be 205 to 210 DEG C, tower bottom temperature is controlled to be 235 to 240 DEG C, a non-condensing collector is adopted for rectification, and a p-fluoronitrobenzene crude product and a m-fluoronitrobenzene crude product are obtained; the p-fluoronitrobenzene crude product is heated to 150 to 180 DEG C, is cooled to 50 to 55 DEG C, and iscooled to 25 to 30 DEG C slowly for separation, a filtrate is collected, and purified p-fluoronitrobenzene is obtained; the m-fluoronitrobenzene crude product is cooled to 10 to 15 DEG C, is heated to 30 to 40 DEG C slowly, separation is carried out, and a crystal product is collected to obtain purified m-fluoronitrobenzene.

Description

technical field [0001] The invention belongs to the technical field of meta-oil utilization, and in particular relates to a comprehensive development and separation method of chloronitrobenzene meta-oil. Background technique [0002] Meta-position oil is a mixture of m-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene, wherein the proportion of o-chloronitrobenzene is 1-3%, the melting point is 31-33°C, and the boiling point is 246°C , the proportion of p-chloronitrobenzene is 46-49%, the melting point is 83-84°C, the boiling point is 242°C, the proportion of m-chloronitrobenzene is 48-50%, the melting point is 44-46°C, and the boiling point is 235- At 236°C, the physical properties of the components of m-chloronitrobenzene, p-chloronitrobenzene and o-chloronitrobenzene are relatively similar. During the rectification and crystallization process of separating p-chloronitrobenzene and o-chloronitrobenzene, m- Chloronitrobenzene will gradually enrich and have...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/12C07C201/10C07C201/16
CPCC07C201/10C07C201/16C07C205/12
Inventor 解卫宇许舟
Owner SHANGYU XIES CHEM IND
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