Method for preparing p-hydroxybenzonitrile

A technology for p-hydroxybenzonitrile and methyl hydroxybenzoate is applied in the field of preparation of p-hydroxybenzonitrile, can solve problems such as lack of energy saving and environmental protection, and achieve the effects of reducing technological process and simplifying reaction steps

Inactive Publication Date: 2016-03-23
JIANGSU RUIDA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, lack a kind of energy saving and environmental protection, can the preparation method of p-hydroxybenzonitrile of continuous automation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of preparation method of p-hydroxybenzonitrile of the present invention, comprises the steps:

[0019] Add filler and catalyst to the fixed bed reactor, dissolve the feed methyl p-hydroxybenzoate in the organic solvent, and add it together with deionized water into the fixed bed reactor, control the reaction temperature of the reactor to be 300°C, and the reaction pressure to be 0KPa, continuous discharge, after rectification, p-hydroxybenzonitrile is obtained.

[0020] Filling is added to the lower end of the fixed bed reactor, catalyst is added to the reaction bed, the reaction temperature of the reaction bed is controlled to be 300°C, and the middle temperature of the upper glass bulb is 300°C.

[0021] The organic solvent is pyridine; the mass concentration of the pyridine is 99%, and the mass ratio of methyl p-hydroxybenzoate:pyridine:water is 2:6:1.

[0022] The filler is glass spheres, the catalyst is silica spheres, and the mass ratio of the feed to the ...

Embodiment 2

[0030] The difference between embodiment 2 and embodiment 1 is: a kind of preparation method of p-hydroxybenzonitrile of the present invention, comprises the steps:

[0031] Add the filler and catalyst to the fixed bed reactor, dissolve the feed methyl p-hydroxybenzoate in the organic solvent, and put it into the fixed bed reactor together with water, control the reaction temperature of the reactor to 380°C, and the reaction pressure to 0.05KPa , continuous discharge, after rectification, obtained p-hydroxybenzonitrile.

[0032] Add filler to the lower end of the fixed bed reactor, add catalyst to the reaction bed, control the reaction temperature of the reaction bed to 380°C, and the middle temperature of the upper glass bulb to 360°C.

[0033] The mass ratio of methyl p-hydroxybenzoate:pyridine:water is 3:6.5:1. The mass ratio of the feed to the catalyst was 0.3. The aspect ratio is 8:1, and a buffer zone of 48 cm is left below the feed port. The buffer zone is filled with...

Embodiment 3

[0038] The difference between embodiment 3 and embodiment 1 is:

[0039] A kind of preparation method of p-hydroxybenzonitrile of the present invention, comprises the steps:

[0040] Add the filler and catalyst to the fixed bed reactor, dissolve the feed methyl p-hydroxybenzoate in the organic solvent, and put it into the fixed bed reactor together with water, control the reaction temperature of the reactor to 480°C, and the reaction pressure to 0.1KPa , continuous discharge, after rectification, obtained p-hydroxybenzonitrile.

[0041] Add filler to the lower end of the fixed bed reactor, add catalyst to the reaction bed, control the reaction temperature of the reaction bed to 480°C, and the middle temperature of the upper glass bulb to 460°C.

[0042] The mass concentration of the pyridine is 99%, and the mass ratio of methyl p-hydroxybenzoate:pyridine:water is 3.5:7:1.

[0043] The filler is glass spheres, the catalyst is silica spheres, and the mass ratio of the feed to ...

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PUM

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Abstract

The invention discloses a method for preparing p-hydroxybenzonitrile. The method comprises the following steps: adding filler and a catalyst into a fixed-bed reactor, dissolving feed, i.e., methyl p-hydroxybenzoate in an organic solvent, then, adding the solution into the fixed-bed reactor together with water, controlling the reaction temperature of the reactor to 300-480 DEG C and the reaction pressure of the reactor to 0-0.1KPa, carrying out continuous discharging, and carrying out rectification, thereby preparing p-hydroxybenzonitrile. The method is energy-saving and environment-friendly, continuous automated production can be achieved, reaction steps are simplified, process flows are reduced, and the problem in former p-hydroxybenzonitrile production that waste gases, waste water and waste residues are severe and the continuous automated production cannot be achieved is solved.

Description

technical field [0001] The invention relates to the technical field of energy saving and environmental protection, in particular to a preparation method of p-hydroxybenzonitrile. Background technique [0002] p-Hydroxybenzonitrile is an intermediate of organophosphorus insecticides fenitronil and benzonitrile, an intermediate of herbicide bromoxynil, and an intermediate of liquid crystal materials, spices, etc. There are many ways to synthesize, the early method is T.Sandmeyer method, but the synthesis method has many steps, harsh reaction conditions, using cyanide as raw material, equivalent CuCN as catalyst, easy to cause serious pollution to the environment, and high production cost , these problems have seriously restricted industrial applications, so people try to utilize other approaches to realize the synthesis of p-hydroxybenzonitrile, thereby avoiding the use of this type of highly toxic cyanide reagent. At present, the main method used in China is the ammoniation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/22C07C255/53
CPCC07C253/22C07C255/53
Inventor 周士涛付博周乔
Owner JIANGSU RUIDA TECH CO LTD
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