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Preparation technology of N-phenylglycinonitrile

A technology of anilinoacetonitrile and preparation process, applied in the preparation of carboxylic acid nitrile, preparation of organic compounds, organic chemistry, etc., can solve the problems of complicated wastewater treatment process, low mother liquor reuse rate and high treatment cost, and reduce wastewater treatment. The effect of low production cost and good social benefit

Active Publication Date: 2012-08-08
内蒙古诚信永安化工有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

However, this method uses the highly toxic substance benzene, which is not conducive to industrialization
[0008] CN200810016883.x "A kind of preparation method of environment-friendly anilinoacetonitrile" has introduced the condensation reaction of aniline and hydroxyacetonitrile, also introduced the reuse of mother liquor and the physicochemical biochemical treatment of mother liquor, but its mother liquor reuse rate is low, only 12 -20%. In addition, its wastewater treatment process is complex, with many equipments and high treatment costs

Method used

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  • Preparation technology of N-phenylglycinonitrile
  • Preparation technology of N-phenylglycinonitrile
  • Preparation technology of N-phenylglycinonitrile

Examples

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Effect test

Embodiment 1

[0029] Add 200g of distilled water into a 500ml four-necked bottle, adjust the pH to 11 with 2g of 25% ammonia water, then add 50g of 99.5% aniline, stir evenly, then add 65g of 50% hydroxyacetonitrile within 5 minutes, and heat to 70-75°C React for 0.5h, then raise the temperature steadily to 90-95°C for 6h. Then gradually cooled to 40-45°C for crystallization, and centrifuged at 15-20°C to obtain N-anilinoacetonitrile with a content of 97.05%, a liquid phase purity of 97.12%, and a colorless transparent crystal with a yield of 99.50%.

[0030] Obtain mother liquor waste water 240g, COD35000ppm, total nitrogen 2000ppm, pH value 11, after described mother liquor waste water can pass through 3 grades of organic matter enrichment devices (toluene is extraction agent), mother liquor waste water COD is reduced to 128ppm, total nitrogen is reduced to 46ppm, pH value 9, decolorized by activated carbon with 1% mother liquor for 0.5h, filtered to a colorless liquid, adjusted to pH 7 w...

Embodiment 2

[0032] Add 200g of mother liquor and 135g of distilled water into a 1000ml four-neck bottle, measure the pH to 10 without adjustment, then add 95g of 99.5% aniline, stir evenly, then add 119g of 50% hydroxyacetonitrile within 5 minutes, heat to 70-75°C for reaction After 1h, the temperature was raised steadily to 95-98°C for 4h. Then gradually cooled to 45-48°C to crystallize, and centrifuged at 20-25°C to obtain N-anilinoacetonitrile with a content of 97.35%, a liquid phase purity of 97.54%, and slightly yellow transparent crystals with a yield of 99.81%.

[0033] Obtain mother liquor waste water 380g, COD25000ppm, total nitrogen 1500ppm, pH value 9.5, after described mother liquor waste water can pass through 4 grades of organic matter enrichment devices (dichloromethane is extraction agent), mother liquor waste water COD is reduced to 155ppm, and total nitrogen is reduced to 40ppm, The pH value is 8, decolorized by activated carbon with 0.5% of the mother liquor for 0.5 h, ...

Embodiment 3

[0035] Add 535g of mother liquor into a 1000ml four-neck bottle, measure the pH to 9 without adjustment, then add 100g of 99.5% aniline, stir evenly, then add 127g of 50% hydroxyacetonitrile within 5 minutes, heat to 70-75°C for 1.5h, Then the temperature was raised steadily to 95-98°C for 2h. Then gradually cooled to 35-40°C for crystallization, and centrifuged at 25-30°C to obtain N-anilinoacetonitrile with a content of 97.65%, a liquid phase purity of 97.70%, and light yellow transparent crystals with a yield of 99.88%.

[0036] Obtain mother liquor waste water 560g, COD30000ppm, total nitrogen 1600ppm, pH value 8.5, after described mother liquor waste water can pass through 5 grades of organic matter enrichment devices (toluene is extraction agent), mother liquor waste water COD is reduced to 130ppm, total nitrogen is reduced to 42ppm, pH value 8, decolorized by activated carbon with 0.5% mother liquor for 0.5h, filtered to a colorless liquid, adjusted to pH 7 with hydroch...

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Abstract

The invention relates to a preparation technology of N-phenylglycinonitrile with the characteristics of economy and environmental protection, and especially provides a technology for mother liquid utilization and wastewater processing in the production of N-phenylglycinonitrile. The preparation technology comprises operations of condensation reaction mother liquid recovery processing, N-phenylglycinonitrile is obtained by carrying out the condensation reaction on aniline, hydroxyacetonitrile and a catalyst in the presence of water (or the mother liquid), the content is greater than 97%, the liquid phase purity is greater than 97%, N-phenylglycinonitrile is a colorless or light yellow transparent crystal, and the yield is greater than 99.5%. The resulting reacted mother liquid can be directly reused in the condensation operation without processing, almost all organic matters can be recovered through physically processing exhaustless wastewater, COD of residual wastewater is less than 200ppm, and the total nitrogen content in the residual wastewater is less than 50ppm. By adopting above optimized technology, the ammonia nitrogen content is reduced, and the COD is reduced, so 75-90% of the mother liquid can be recycled to the condensation reaction and can be repeatedly reused, thereby the wastewater processing amount is reduced; and additionally, the recycle of the mother liquid makes the organic matters in the mother liquid be fully recovered, and yield improvement and cost saving be realized.

Description

technical field [0001] The invention relates to a green and environment-friendly preparation process for producing N-anilinoacetonitrile by using hydroxyacetonitrile, and belongs to the technical field of N-anilinoacetonitrile preparation. Background technique [0002] N-anilinoacetonitrile is the main raw material of indigo, and the method for synthesizing N-anilinoacetonitrile has the following several kinds: [0003] 1. Sodium cyanide method: Patent Application No. CN971045054.0 discloses a "N-phenylaminoacetate manufacturing process", using aniline, sodium cyanide, formaldehyde, in the presence of magnesium salt (magnesium chloride or magnesium sulfate) , generating N-anilinoacetonitrile. [0004] 2. Hydrocyanic acid method: German patents DE3010511, 2621450, 2621728, 2625935, Japanese patents JP591210052, 56141251, Chinese patent CN02113428.6, etc. adopt aniline, formaldehyde, liquid (gas) hydrocyanic acid as raw materials, and add additives. React and crystallize to ...

Claims

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Application Information

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IPC IPC(8): C07C255/25C07C253/30
Inventor 张辰亮李玉顺程丽华殷军利王学花
Owner 内蒙古诚信永安化工有限公司
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