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Tech. of preparing 2,4-di nitro methyl-phenoxide by nitro methyl-phenoxide continuous thermal insulating nitration

A technology of dinitroanisole and nitroanisole, which is applied in the preparation of nitro compounds, organic chemistry and other directions, can solve the problems of large discharge of waste water and waste residues, increase treatment costs, poor product quality, etc., and achieve production Low cost, reduced thermal energy, high reliability

Inactive Publication Date: 2008-01-16
CHANGZHOU JIASEN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] This 2, the preparation technology of 4-dinitroanisole has following shortcoming: cost is high, consumption is big, product quality is relatively poor, especially waste water, waste residue discharge are big, have caused serious environmental pollution, if produce Wastewater and waste residues are treated, which increases the treatment cost, and there is also a hidden danger of secondary pollution

Method used

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  • Tech. of preparing 2,4-di nitro methyl-phenoxide by nitro methyl-phenoxide continuous thermal insulating nitration
  • Tech. of preparing 2,4-di nitro methyl-phenoxide by nitro methyl-phenoxide continuous thermal insulating nitration

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Embodiment 1

[0027] A kind of continuous adiabatic nitration of nitroanisole prepares 2,4-dinitroanisole technology, and described process step is as follows:

[0028] (1). Using 4-nitroanisole as a raw material, the mixed acid is prepared by mixing industrial grade 98% sulfuric acid, 95% nitric acid and 65% nitric acid. The dehydration value of the mixed acid is between 2.0 and 3.2. 4- The molar ratio of nitroanisole to nitric acid is 1:1.05, and a continuous adiabatic nitration reaction occurs in a continuous static mixer adiabatic nitration reactor, and the operating temperature is controlled between 65°C and 120°C.

[0029] (2). After the continuous adiabatic nitration reaction, the material is decompressed to 28.0KPa, the water and a small amount of nitric acid remaining in the nitration reaction are distilled off, and the waste acid is concentrated.

[0030] (3). After evaporating and concentrating, let stand for 1.0h, and carry out liquid-liquid layer separation. The lower water ph...

Embodiment 2

[0037] A kind of continuous adiabatic nitration of nitroanisole prepares 2,4-dinitroanisole technology, and described process step is as follows:

[0038] (1). Using 2-nitroanisole as a raw material, the mixed acid is prepared by mixing industrial-grade 98% sulfuric acid, 95% nitric acid and 65% nitric acid. The dehydration value of the mixed acid is between 2.8 and 4.2. 2- The molar ratio of nitroanisole to nitric acid is 1:1.05, and a continuous adiabatic nitration reaction occurs in a continuous static mixer adiabatic nitration reactor, and the operating temperature is between 65°C and 140°C.

[0039] (2). The material after the continuous adiabatic nitration reaction is decompressed to 78.0KPa to distill water and nitric acid left over from the nitration reaction, and concentrate the waste acid.

[0040] (3). After evaporating and concentrating, let stand for 0.5h, and carry out liquid-liquid layer separation. The lower water phase is sulfuric acid and a small amount of n...

Embodiment 3

[0047] A kind of continuous adiabatic nitration of nitroanisole prepares 2,4-dinitroanisole technology, and described process step is as follows:

[0048](1). The mixture of 2-nitroanisole and 4-nitroanisole is used as a raw material. The mixed acid is prepared by mixing industrial grade 98% sulfuric acid, 95% nitric acid and 65% nitric acid. The dehydration value of the mixed acid is Between 2.8 and 4.2, the molar ratio of nitroanisole and nitric acid is 1:1.05, continuous adiabatic nitration reaction occurs in continuous static mixer adiabatic nitration reactor, and the operating temperature is between 65°C and 140°C .

[0049] (2). The material after the continuous adiabatic nitration reaction is decompressed to 10.0KPa ~ 100KPa to distill water and nitric acid remaining from the nitration reaction, and concentrate the waste acid.

[0050] (3). After evaporating and concentrating, let stand for 0.5h, and carry out liquid-liquid layer separation. The lower water phase is s...

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Abstract

A process for preparing 2,4-dinitro phenylmether from nitro phenylmether by continuous insulated nitrifying includes such steps as pre-heating 2-nitro phenylmether, 4-nitro phenylmether, or their mixture to fuse them, continuous nitrifying reaction on acid mixture, evaporation concentrating, liquid-liquid separation to obtain oil phase (2,4-dinitro phenylmether, cooling while crystallizing, educing out 2,4-dinitro phenylmether, solid-liquid separation to obtain solid 2,4-dinitro phenylmether, separation, refining, solid-liquid separation to obtain solid 2,4-dinitro phenylmether.

Description

technical field [0001] The invention relates to a process for preparing 2,4-dinitroanisole by continuous adiabatic nitration of nitroanisole, which belongs to the field of fine chemical industry. Background technique [0002] 2,4-Dinitroanisole is an important intermediate in organic synthesis. At present, the preparation process of 2,4-dinitroanisole is obtained by methoxylation of 2,4-dinitrochlorobenzene. This preparation process is to put molten 2,4 - Dinitrochlorobenzene and sodium methoxide, heated to about 40°C, controlled at 58°C to 60°C for methoxylation reaction, after the reaction, 2,4-dinitroanisole can be obtained through treatment and operation product. The main reaction structure formula is: [0003] [0004] This 2, the preparation technology of 4-dinitroanisole has following shortcoming: cost is high, consumption is big, product quality is relatively poor, especially waste water, waste residue discharge are big, have caused serious environmental pollut...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/08C07C205/36
Inventor 许文林段玉辉刘学谦
Owner CHANGZHOU JIASEN CHEM