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Method for preparing n-phenylglycinonitrile

A technology of anilinoacetonitrile and hydroxyacetonitrile, which is applied to the preparation of carboxylic acid nitriles, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low product yield, cumbersome operation, and large equipment investment, and improve the reaction rate. The effect of improving material conversion rate, improving reaction efficiency and ensuring continuity

Active Publication Date: 2009-08-26
重庆渝化新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many deficiencies in this method: large investment in equipment, cumbersome operation, unstable process control and product quality, low product yield, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The hydroxyacetonitrile solution and the aniline solution described in Table 1 are preheated and mixed respectively through a delivery pump, a flow meter to a pipeline preheater and a pipeline mixer, wherein the flow control and preheating of the hydroxyacetonitrile solution and the aniline solution Temperature and pressure, mixing temperature and pressure are shown in Table 2; The material that pipeline mixer comes out enters two groups of series-connected (each group of pipeline reactors are made up of two pipeline reactors in series) pipeline reactors continuously, At the inlet of the first group of pipeline reactors, add an aqueous sodium bicarbonate solution of auxiliary agent A with a mass percentage of about 25%. The amount of the aqueous sodium bicarbonate solution added is 4% of the amount of hydroxyacetonitrile in terms of mass percentage, and the flow rate is controlled at 120l / h so that the pH value of the reaction material is controlled at 4 to 6; the materi...

Embodiment 2

[0034] Wherein the parameter of each raw material used is shown in Table 1; Every process parameter is shown in Table 2 and Table 3; Auxiliary agent A is the sodium carbonate aqueous solution of about 30% by mass percentage, and its add-on is counted as 2% of the hydroxyacetonitrile consumption by mass percentage , and continuously and evenly join in the pipeline reactor, so that the pH value of the reaction material is controlled at 5~7, all the other steps are with embodiment 1; In the present embodiment, 38620kg of anilinoacetonitrile was obtained in 24 hours, and the purity of gained anilinoacetonitrile was 96.1%, the yield is 99.9%

Embodiment 3

[0036] Wherein the parameter of each raw material used is shown in Table 1; Every process parameter is shown in Table 2 and Table 3; Auxiliary A is the potassium bicarbonate aqueous solution that mass percent is about 20%, and its addition is counted as 0.5% of the hydroxyacetonitrile consumption in mass percent %, flow control at 10l / h, so that the pH value of the reaction material is controlled at 4~7, and all the other steps are with embodiment 1; In the present embodiment, 13336kg of anilinoacetonitrile was obtained in 24 hours, and the gained anilinoacetonitrile purity was 95.7%. The rate is 99.8%.

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Abstract

The present invention provides a method for preparing n-phenylglycinonitrile, wherein the method comprises a step of executing condensation reaction for generating n-phenylglycinonitrile when the phenylamine and glycolonitrile are used as raw materials. The invention is characterized in that according to the continuous production method, the raw materials continuously pass through a pipe type preheater, a pipe type mixer, a pipe type reactor and a reaction still for executing condensation reaction for generating the n-phenylglycinonitrile. The method of the invention has the advantages of fewer devices, simple and brief technical route, saved costs of man power, device, raw materials, energy, etc., improved operating environment, extraordinary automatic control realization, excellent guaranteed safety production operability and continuity, equitability and stability of production thereby guaranteeing the stability of product quality, increasing the product purity and yield. The product purity in the invention is above 95.5%, and the product yield is above 99.8%.

Description

technical field [0001] The invention relates to a method for preparing anilinoacetonitrile by using aniline and hydroxyacetonitrile as raw materials. Background technique [0002] Anilinoacetonitrile, the appearance is khaki or yellow-brown solid, the freezing point is 46°C (industrial products ≥39°C), the density is 1050-1200kg / m3, insoluble in water, easily soluble in acetone. Anilinoacetonitrile is mainly used to produce potassium anilinoacetate, the final product is indigo dye, and can also be used as raw materials for other fine chemicals. [0003] Existing anilinoacetonitrile preparation method is more, wherein the hydroxyacetonitrile method, namely with aniline and hydroxyacetonitrile as raw material mixed reaction to generate anilinoacetonitrile and water, belongs to electrophilic substitution reaction, C 6 h 5 NH 2 +HOCH 2 CN→C 6 h 5 NHCH 2 CN+H 2 O, the early stage of the reaction is a fast reaction, and the late stage is a medium-slow reaction. At present...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/42C07C253/30
Inventor 周明权甘永昌
Owner 重庆渝化新材料有限责任公司
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