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Method for producing N-cyanoethylaniline and N,N-dicyanoethylaniline by adopting one-step cleaning process

A technology for dicyanoethylaniline and cyanoethylaniline is applied in the field of producing N-cyanoethylaniline and N.N-dicyanoethylaniline by a one-step cleaning process, and can solve the problems of multiplying production cost, measurement error, production The problem of high cost is to achieve the effect of reducing the cost of three wastes treatment, simple process control and low production cost

Active Publication Date: 2014-08-27
浙江汇翔新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 2. It is difficult to operate during the production process. The error in the measurement of each material and the control process of the heating reaction can make N.N-dicyanoethylaniline exceed the standard.
[0007] 3. The production cost is high. In order to control the generation of N.N-dicyanoethylaniline, a large amount of water is added to the reaction, and the production cost of a single kettle is doubled.

Method used

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  • Method for producing N-cyanoethylaniline and N,N-dicyanoethylaniline by adopting one-step cleaning process
  • Method for producing N-cyanoethylaniline and N,N-dicyanoethylaniline by adopting one-step cleaning process
  • Method for producing N-cyanoethylaniline and N,N-dicyanoethylaniline by adopting one-step cleaning process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 10,000 liters enamel reaction kettle with 30 square meters of sheet enamel condenser, after the inspection of the equipment, add 5000kg of aniline industrial products, 220kg of zinc chloride, 10kg of hydroquinone from the metering tank, seal the reaction kettle, open the condensed water and vacuum, and inhale ice Acetic acid 420kg, water 430kg, then add acrylonitrile 3420kg from the metering tank, slowly heat up, there is back distillation at 68-72 ℃, after back distillation for 2-3 hours, the temperature is at 90 ± 1 ℃, keep 90-100 ℃ back distillation for 10 -13 hours, sample the middle control until the middle control aniline is 0.1±0.02%, N.N-dicyanoethylaniline is 10±2%, and the sum of N-cyanoethylaniline and N.N-dicyanoethylaniline is greater than 98%.

[0028] After the end point, stand still for 2 hours, separate the water phase from the bottom, and then pump the organic phase into the middle tank (the temperature of the middle tank is higher than 60 ° C), and pum...

Embodiment 2

[0031] In the 10000 liter enamel kettle, add 4000kg of aniline, 800-1000kg of water phase, add 200kg of light components, add glacial acetic acid, water, and zinc chloride to the total amount of 176kg, 338kg and 344kg according to the calculation. Hydroquinone 8kg, acrylonitrile 2655kg, slowly heat up to 90±1°C for 2-3 hours, keep at 90-100°C, return distillation reaction for 10-13 hours, and control in the middle.

[0032] After the end point is reached, the organic phase is statically separated to the intermediate tank for rectification in a continuous distillation column (similar to Example 1), and the aqueous phase is about 800-1000kg in the next batch.

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Abstract

The invention relates to the field of chemical engineering and in particular relates to a method for producing N-cyanoethylaniline and N,N-dicyanoethylaniline by adopting a one-step cleaning process. The method comprises the following steps: adding aniline, acetic acid, zinc chloride, acrylonitrile, water and a small quantity of p-dihydroxybenzene into a reaction kettle in sequence; slowly heating while starting a re-distillation condenser, and keeping re-distillation for 10 hours after the re-distillation temperature meets the requirement; keeping standing for 1-2 hours, barreling a lowest-layer water phase for analyzing and metering, and feeding an upper-layer organic phase into a middle tank to take part in next reaction; preserving heat of the middle tank to be not less than 60 DEG C, rectifying the product by using a continuous rectifying tower to obtain light components from a first outlet, and returning the light components to a reaction system to obtain N-cyanoethylaniline from a second outlet and obtain N,N-dicyanoethylaniline from a third outlet, wherein the light components are mainly HAC, H2O and acrylonitrile; and incinerating rectified residues to obtain zinc chloride powder which continues to be used as a catalyst. The novel process is simple to control, clean, environment-friendly, low in consumption and safe.

Description

technical field [0001] The invention relates to a chemical field, in particular to the production of N-cyanoethylaniline and N.N-dicyanoethylaniline by a one-step cleaning process. Background technique [0002] Now these two products are produced by a single method, it is difficult to avoid the formation of N.N-dicyanoethylaniline when producing N-cyanoethylaniline, a small amount of N.N-dicyanoethylaniline is difficult to separate, and the conversion rate of aniline is high. Very low, a large amount of COD-containing acid and aniline-containing wastewater are produced during crystallization. [0003] Reaction equation: [0004] [0005] 1. Due to the application requirements of N-cyanoethylaniline, the content of N.N-dicyanoethylaniline should not be higher than 1.5%, and should be in the range of 2-3% during HPLC measurement (its light absorption intensity and N-cyanoethylaniline ratio) 1.78 times), in this case, the conversion rate of aniline is about 92%, and the ex...

Claims

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Application Information

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IPC IPC(8): C07C255/24C07C253/30
Inventor 段玉辉沈林峰
Owner 浙江汇翔新材料科技股份有限公司
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