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Preparation method of terephthalonitrile through ammonium oxidation

A terephthalonitrile and ammoxidation technology, which is applied in the preparation of hydrocarbon ammoxidation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of reaction heat removal and terephthalonitrile Low nitrile yield, small reaction load and other problems, to achieve the effect of improving catalytic efficiency, improving selectivity and yield, and improving wear resistance

Active Publication Date: 2014-07-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the low yield of terephthalonitrile in the prior art, the reaction load is small, and the problem of difficult reaction heat removal is provided, and a new method for preparing terephthalonitrile by ammoxidation is provided.

Method used

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  • Preparation method of terephthalonitrile through ammonium oxidation
  • Preparation method of terephthalonitrile through ammonium oxidation
  • Preparation method of terephthalonitrile through ammonium oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Catalyst preparation:

[0036] 224g V 2 o 5 and 187 grams of Cr 2 o 3 Add it into a solution at a temperature of 80-90° C. consisting of 980 milliliters of water and 912 grams of oxalic acid, stir well, and react to obtain a vanadium oxalate solution.

[0037] The weight percent concentration is 40% SiO 2 1250 grams of silica sol was slowly added to the above solution under stirring, and then 283.6 grams of 85% phosphoric acid, 12.4 grams of KNO3 , 71.6 g Co(NO 3 )·6H 2 A solution of O and 500 ml of water, 76.4 g of H 3 BO 3 and 500 ml of water and 43.5 g (NH 4 ) 6 Mo 7 o 24 4H 2 O and the solution that 100 milliliters of waters form, stir, heat and evaporate to solid content 40% (weight), obtain viscous slurry.

[0038] The above slurry was spray-dried in a spray dryer to shape, and the formed catalyst precursor was pre-calcined at 300°C for 2 hours, and then fired at 650°C for 4.5 hours to obtain the catalyst in terms of atomic ratio:

[...

Embodiment 2～11

[0050] Using the catalyst prepared in [Example 1], according to the reaction process conditions in Table 1, the yield and selectivity of the product terephthalonitrile were obtained, and the results are shown in Table 1.

[0051] Table 1

[0052]

Embodiment 12～22

[0054] Catalyst preparation method is the same as [Example 1], change the proportioning or composition of catalyst, obtain the catalyst composition of Table 2, and evaluate simultaneously by [Example 1] catalyst evaluation method. Its result list 2.

[0055] Table 2

[0056]

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Abstract

The invention relates a preparation method of terephthalonitrile through ammonium oxidation, and aims to solve the problems of low yield of terephthalonitrile, small reaction load, or difficult reaction heat dissipation in the presence of a conventional catalyst in the prior art. A fluidized bed catalyst is used to solve the problems mentioned above, wherein the fluidized bed catalyst comprises 30 to 80% of silica carrier and 20 to 70% of active component, and the active component is represented by a formula V<1.0>CrPX<c>Y<d>Z<e>O<m>; wherein the X is selected from at least one component of boron oxides and arsenic oxides, Y is selected from at least one component of alkali metal oxides and alkali earth metal oxides, Z is selected from at least one component of oxides of Ni, Co, Pb, Fe, Mo, and W. The fluidized bed catalyst well solves the problems mentioned above and is capable of being applied to the industrial terephthalonitrile production.

Description

technical field [0001] The present invention relates to a process for the preparation of terephthalonitrile by ammoxidation. Background technique [0002] Terephthalonitrile is an important intermediate for dyes, medicines, pesticides and spices. For example, after chlorination, fluorination and hydrolysis of terephthalonitrile, pyrethroid pesticide products can be obtained; p-xylylenediamine obtained by hydrogenation is a resin curing agent with excellent performance. [0003] The most convenient and advanced method for preparing terephthalonitrile is the direct ammoxidation process of p-xylene, which has been developed and matured in the past 30 years. Because of its short process flow, easy operation, good product quality and high yield, it has developed rapidly in recent years. . Because the reaction is carried out under high temperature conditions, side reactions such as deep oxidation and ammoxidative decomposition are prone to occur, which seriously affects the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/51C07C253/28B01J23/887B01J23/86B01J23/26B01J23/888B01J23/30
Inventor 杨为民顾龙勤陈亮曾炜
Owner CHINA PETROLEUM & CHEM CORP
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