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
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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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