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Catalyst for non-carrier high-activity high-selectivity ammoxidation preparation of 2,6-dichlorobenzonitrile, preparation method and applications thereof

The technology of dichlorobenzonitrile and catalyst is applied in the catalyst and preparation and application fields for preparing 2,6-dichlorobenzonitrile with unsupported high activity and selective ammonia oxidation, and can solve the problem that it is difficult to prepare high-performance vanadium hydroxide base Catalysts, low catalyst activity, etc., to achieve high selectivity and simple industrial use

Active Publication Date: 2019-11-05
张家港楚人新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2,6-Dichlorobenzonitrile is mainly prepared by the ammoxidation reaction, and the ammoxidation reaction mainly depends on the performance of the catalyst. The vanadium-based ammoxidation catalyst is mainly prepared by the impregnation method, and it is difficult to prepare a high-performance catalyst by other methods. Vanadium hydroxide based catalyst
[0005] However, the hydrothermal method is a common method for preparing vanadium compounds, and the activity of the prepared catalysts is often low.
There are few reports on the preparation of high-performance vanadium hydroxide-based catalysts by hydrothermal method

Method used

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  • Catalyst for non-carrier high-activity high-selectivity ammoxidation preparation of 2,6-dichlorobenzonitrile, preparation method and applications thereof
  • Catalyst for non-carrier high-activity high-selectivity ammoxidation preparation of 2,6-dichlorobenzonitrile, preparation method and applications thereof
  • Catalyst for non-carrier high-activity high-selectivity ammoxidation preparation of 2,6-dichlorobenzonitrile, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of catalyst that prepares 2,6-dichlorobenzonitrile by ammoxidation of non-carrier high activity selectivity, and this catalyst is composed of VCr 0.5 Al 0.5 o 4 .

[0031] The preparation method of above-mentioned catalyst adopts hydrothermal method, and concrete steps are as follows:

[0032] (1) Weigh 0.03mol V 2 o 5 , 0.03mol CrO 3 , 0.03mol Al(NO 3 ) 3 9H 2 Mix O with 0.18mol oxalic acid, add 400ml distilled water, stir in a water bath at 353K for 2h to form VOC 2 o 4 , Cr 2 (C 2 o 4 ) 3 and Al 2 (C 2 o 4 ) 3 uniform mixed solution;

[0033] (2) Filter the mixed solution and transfer it to a 500mL autoclave, react at 533K for 24h, and cool down to room temperature after the reaction;

[0034] (3) Filter the product obtained in step (2) to obtain a black sample, wash and dry it, and then calcinate it at 573K for 2h to obtain a non-supported highly active 2,6-dichlorotoluene ammoxidation catalyst, which is composed of V 1 Cr 0.5 Al 0.5 o ...

Embodiment 2~6

[0038] The preparation methods of the five catalysts in Examples 2-6 are similar to those in Example 1. M salt and its dosage are respectively 0.030mol Fe(NO 3 ) 3 , 0.030mol Co(NO 3 ) 3 , 0.030mol Ti(OH) 4 (prepared by hydrolysis and filtration of tetrabutyl titanate) 0.0043mol (NH 4 ) 6 Mo 7 o 24 and 0.0025mol(NH 4 ) 10 W 12 o 41 Respectively replace Al(NO in Example 1 3 ) 3 .

[0039] The crystal phase of embodiment 2-6 gained catalyst consists of figure 1 shown. The obtained catalyst V 1 Cr 0.5 Fe 0.5 o 4 and V 1 Cr 0.5 co 0.5 o 4 is an amorphous structure; V 1 Cr 0.5 W 0.5 o 4.75 The catalyst is composed of two crystal phases, and the diffraction angles 2θ=14.1°, 23.3°, 28.3° and 49.9° belong to WO 3 Crystal phase, diffraction angle 2θ=37.0°, 42.1° and 55.1° belong to Cr 2 o 3 crystal phase. V 1 Cr 0.5 Mo 0.5 o 4.75 The diffraction peaks appearing at 2θ=37.0°, 42.1° and 55.1° correspond to Cr 2 o 3 ; for V 1 Cr 0.5 Ti 0.5 o 4.25 Ca...

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Abstract

The invention discloses a catalyst for non-carrier high-activity high-selectivity ammoxidation preparation of 2,6-dichlorobenzonitrile, wherein the catalyst has a composition of VaCrbMcOx, M is one selected from Fe, Al, W, Ti, Mo, Co and the like, a is 1, b is 0.1-0.9, c is 0.1-0.9, b+c is 1, and based on the value of x, the algebraic sum of the valence of the positive and negative elements in thecatalyst is zero. According to the present invention, by using the hydrothermal synthesis, the uniform dispersion of the active species of the catalyst is promoted; and the catalyst is prepared by using the hydrothermal method, the calcination decomposition process does not exist, the disadvantages of non-uniform active substance and requirement of high-temperature calcination decomposition of the impregnation method are avoided, and the yield and the selectivity of the catalytic product are not reduced.

Description

technical field [0001] The invention relates to a catalyst for preparing 2,6-dichlorobenzonitrile by non-carrier high-activity selective ammoxidation and a preparation and use method thereof. Background technique [0002] 2,6-Dichlorobenzonitrile is widely used in fields such as agriculture, automobiles, electrical appliances, and machinery, and is an important chemical product. 2,6-Dichlorobenzonitrile is mainly prepared by the ammoxidation reaction, and the ammoxidation reaction mainly depends on the performance of the catalyst. The vanadium-based ammoxidation catalyst is mainly prepared by the impregnation method, and it is difficult to prepare a high-performance catalyst by other methods. Vanadium hydroxide based catalyst. At present, many research papers and patent documents related to the preparation of 2,6-dichlorobenzonitrile by ammoxidation have been published at home and abroad. The main production process and catalytic effect are shown in Table 1: [0003] Table...

Claims

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Application Information

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IPC IPC(8): B01J23/26B01J23/28B01J23/30B01J23/86B01J37/10C07C253/28C07C255/50
CPCB01J23/26B01J23/28B01J23/30B01J23/862B01J23/864B01J23/002B01J37/10B01J37/0018C07C253/28B01J2523/00B01J2523/31B01J2523/55B01J2523/67B01J2523/842B01J2523/845B01J2523/47B01J2523/68B01J2523/69C07C255/50
Inventor 刘业硕李雄建张思巍王安东黄驰
Owner 张家港楚人新材料科技有限公司
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