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A kind of n-(1-ethylpropyl)-3,4-dimethylaniline continuous production device and method

A technology of dimethylaniline and ethylpropyl, which is applied in the field of N--3,4-dimethylaniline continuous production equipment, can solve the problem of low material utilization rate, improve the conversion rate of raw materials and reduce side effects Response, the effect of reducing production costs

Active Publication Date: 2017-04-19
绍兴贝斯美化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The material utilization rate of the existing method is not high, and it is easy to generate a large amount of waste water and waste acid

Method used

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  • A kind of n-(1-ethylpropyl)-3,4-dimethylaniline continuous production device and method
  • A kind of n-(1-ethylpropyl)-3,4-dimethylaniline continuous production device and method
  • A kind of n-(1-ethylpropyl)-3,4-dimethylaniline continuous production device and method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Ortho-xylene and nitric-sulfur mixed acid are put into the mixer from their respective high-level tanks through the metering pump, wherein, in the nitric-sulfur mixed acid, the molar ratio of nitric acid to sulfuric acid is 1:0.5-1; the molar amount of nitric acid in the nitric-sulfur mixed acid Calculated, the molar ratio of o-xylene and nitric acid mixed acid is 1:1.5-2. After mixing o-xylene and nitric-sulfur mixed acid in the mixer, nitrogen is pressed into the double-ring nitration reactor, and the feed flow rate of the ortho-xylene and nitric-sulfur mixed acid mixture is 1.5-2m / s. The mixed material is pressed into the nitration system, and the organic phase and the acid phase are fully contacted to carry out multi-stage nitration reaction. The temperature in the ring-shaped nitration reactors at all levels is controlled at 10-25°C by means of heat exchangers.

[0083] The reaction solution flows out of the nitrification system and enters the first phase-separati...

Embodiment 2

[0089] Compared with Example 1, the difference is that in the nitric-sulfur mixed acid, the mol ratio of nitric acid and sulfuric acid is 1:0.1-0.44; in terms of the molar amount of nitric acid in the nitric-sulfur mixed acid, the mol ratio of o-xylene and nitric-sulfur mixed acid is 1:1.1-2; the feed flow rate of o-xylene and nitric acid mixed acid mixture is 1.5-2m / s. The temperature in the annular nitration reactors at all levels is controlled to be 10-15° C. through heat exchangers.

[0090] After the continuous production ended, the conversion rate of o-xylene was 96.5%, and in the nitration reaction solution (the reaction solution at the discharge port of the last stage reactor of the nitration system, sampled once every 30min), the conversion rate of 4-nitro-o-xylene The content is greater than 93%, and the purity of 4-nitro-o-xylene collected by rectification is greater than 99.6% (purity by GC area normalization method).

[0091] In the catalytic hydrogenation reacti...

Embodiment 3

[0094] Compared with Example 1, the difference is that in the catalytic hydrogenation reaction, the hydrogenation reactor is added

[0095] 0.1-0.2eqv (based on 4-nitro-o-xylene) of dodecylsulfonic acid, the pH of the reaction system is controlled between 5.5-6, and the residence time of the material in the hydrogenation reactor is 0.5-1h. After the continuous reaction was finished, it was determined that the conversion rate of 4-nitro-o-xylene was 99.6%, and the yield of N-(1-ethylpropyl)-3,4-dimethylaniline was 99.1%. GC The purity is 99.5%.

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Abstract

The invention discloses an N-(1-ethyl propyl)-3,4-dimethylaniline continuous synthesis system and method. The method is characterized in that o-xylene and nitric-sulfuric acid carry out nitration reaction in a nitration system; a reaction liquid passes through a first split phase tank, a labyrinth washing system and a distillation system in sequence to undergo distillation treatment; collected 4-nitro-o-xylene and 3-pentanone carry out catalytic hydrogenation reaction in a hydrogenation reactor; then N-(1-ethyl propyl)-3,4-dimethylaniline is prepared through treatment carried out by a falling film evaporation system. The production system provided by the invention has the beneficial effects that all the materials are recycled, thus reducing the production cost; the raw material conversion rate of single batch production is effectively increased, thus reducing the amount of waste acid and wastewater.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a continuous production device and method for N-(1-ethylpropyl)-3,4-dimethylaniline. Background technique [0002] N-(1-ethylpropyl)-3,4-dimethylaniline, molecular formula: C 13 h 21 N molecule: 191.3125, boiling point 290.2°C, CAS: 56038-89-2, structural formula: Formula 1: It is the main intermediate of pendimethalin, a high-efficiency, low-toxicity, broad-spectrum herbicide. [0003] [0004] There are many methods for synthesizing N-(1-ethylpropyl)-3,4-dimethylaniline, for example, EP630883 discloses a synthetic method: 3,4-dimethylnitrobenzene first undergoes 3,4-dimethylaniline is obtained by reduction of iron powder, and then condensed with 3-pentanone under acid catalysis and dehydrated to obtain imine, and the imine is hydrogenated and reduced under the action of a rare metal catalyst to obtain N-(1-ethane propyl)-3,4-dimethylaniline: see Equation 1 for t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/48C07C209/36
CPCC07C201/08C07C209/36C07C205/06C07C211/48
Inventor 田园沈亮明黄淑芳陈湘朋姚文斌应天祥
Owner 绍兴贝斯美化工股份有限公司