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Method for preparing m-phthalonitrile

A technology for isophthalonitrile and m-xylene, which is applied in the field of preparing isophthalonitrile, can solve the problems of low yield of the target product, expensive raw materials, and the catalyst is difficult to meet the requirements of a fluidized bed, and achieves good catalysis Activity, reduce production costs, enhance the effect of wear resistance

Inactive Publication Date: 2005-06-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by the present invention is to overcome the shortcomings that the catalyst used in the previous process is difficult to adapt to the requirements of the fluidized bed, or use expensive raw materials and the yield of the target product is not high, and provide a new method for the preparation of Isophthalonitrile method

Method used

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  • Method for preparing m-phthalonitrile
  • Method for preparing m-phthalonitrile
  • Method for preparing m-phthalonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Catalyst preparation:

[0054] 201 g V 2 o 5 Add it into a solution at a temperature of 80-90° C. consisting of 440 milliliters of water and 420 grams of oxalic acid, stir well, and react to obtain a vanadium oxalate solution.

[0055] 40% (weight) SiO 2 1250 grams of silica sol were slowly added to the above solution under stirring, and then respectively added by 798 grams of Cr (NO 3 ) 3 9H 2 A solution composed of O and 300 ml of water, 68.6 g of H 3 BO 3 and 560 ml of water and 39.2 g (NH 4 ) 6 Mo 7 o 24 4H 2 A solution consisting of O and 50 ml of water, 0.11 molar phosphoric acid solution, and finally 9.4 g of NaNO 3 and 20 milliliters of water, then add 113.7 grams of 30% (by weight) TiCl 3 Hydrochloric acid solution, stirred and mixed, heated and evaporated to a solid content of 42% (weight), to obtain a viscous slurry.

[0056] The above slurry is sprayed into shape, the gas inlet temperature of the sprayer is 250°C, the outlet temperature is 130°...

Embodiment 2~7

[0063] The preparation method of the catalyst is the same as in Example 1, except that the composition of the catalyst is changed, and the evaluation conditions of the catalyst in Example 1 are used. The evaluation results are listed in Table 1.

[0064] Example

Embodiment 8

[0069] Catalyst preparation method is the same as embodiment 1, and changing catalyst evaluation condition is:

[0070] m-xylene: ammonia: air=1:5:35 (mol), catalyst weight loading (WWH) 0.04 hours -1 , the reaction temperature is 425°C, and the reaction pressure is 0.01MPa.

[0071] Reaction result: m-xylene conversion rate 98.6%

[0072] m-dibenzonitrile selectivity 81.2%

[0073] Yield of m-dibenzonitrile 80.1%

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Abstract

The invention relates to a method for preparing isophthalonitrile by ammoxidation of m-xylene. The invention mainly solves the disadvantages that the catalyst used in the prior art is difficult to adapt to the requirements of the fluidized bed or uses relatively expensive raw materials or has poor reaction selectivity. The present invention adopts the fluidized bed catalyst process using vanadium-chromium-boron-titanium as the main active component, the reaction temperature is 330-480°C, the reaction pressure is normal pressure to 0.05MPa, and the catalyst load (WWH) is 0.03-0.1 hours -1 , The raw material molar ratio is m-xylene: ammonia: the technical scheme of air=1: 2~13: 10~50, has solved this problem preferably, can be used in the industrial production of isophthalonitrile.

Description

technical field [0001] The present invention relates to a process for the preparation of isophthalonitrile. Background technique [0002] Isophthalonitrile (abbreviated as IPN) is an important organic raw material for organic synthesis. Tetrachloroisophthalonitrile synthesized by chlorination is an efficient and low-toxic fungicide; m-xylylenediamine obtained by hydrogenation is a performance Excellent curing agent for epoxy resin, and raw material for polyurethane resin and nylon resin. [0003] The simplest and most economical production method of isophthalonitrile is obtained by gas-phase ammoxidation of m-xylene under the action of a catalyst, and its core technology is the catalyst. [0004] In the 1950s, Japan’s Showa Denko developed the production technology of m-xylene ammoxidation in a fixed bed to synthesize isophthalonitrile. In the 1970s, Japan’s Mitsubishi Gas Co., Ltd. and the US Badger Company jointly developed a fine-grained fl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/28C07C255/51
Inventor 陈金华顾龙勤金文清
Owner CHINA PETROLEUM & CHEM CORP