Oxide surface treatment method and application of oxide surface treatment method in reaction for preparing 6-aminocapronitrile from caprolactam
A surface treatment, aminocapronitrile technology, applied in chemical instruments and methods, chemical/physical processes, carboxylic acid amide dehydration preparation and other directions, can solve the problems of complex operation process, low conversion rate of caprolactam per pass, etc., to simplify the process flow , The effect of improving the one-way conversion rate and simple processing method
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Embodiment 1
[0050] The treatment method steps of the oxide surface are as follows:
[0051] (1) Weigh 10g metal oxide TiO 2 , put it into a tube furnace and calcined at 350°C for 6h under the atmosphere of Ar gas, and obtain the pretreated material after natural cooling;
[0052] (2) Weigh 0.5g NaBH respectively according to the mass ratio of 0.25:1 4 and 2g of TiO prepared in step (1) 2 Mixed and added to 25g of deionized water for ultrasonic dispersion for 30min, the resulting mixture was stirred at 60°C for 12h, then heated and evaporated to dryness to obtain a mixture;
[0053] (3) Put the mixed material prepared in the step (2) into a tube furnace and roast at 550° C. for 4 hours under an Ar gas atmosphere to prepare the roasted material;
[0054] (4) Transfer the calcined material prepared in step (3) to deionized water for 5 times of centrifugal washing at a rate of 6000rpm, and then transfer to ethanol aqueous solution for centrifugal washing 2 times; place it under an atmosphe...
Embodiment 2
[0057] The treatment method step of oxide surface is with reference to embodiment 1, and difference is that in step (2) reducing agent NaBH 4 and TiO 2 Mass ratio is changed into 0.5:1, all the other steps are with embodiment 1, the TiO after processing 2 denoted as TiO 2 -2,TiO 2 -2 photos such as figure 1 as shown in b.
[0058] The surface treated oxide TiO 2 -2 is used as a catalyst to catalyze the specific steps of the caprolactam system 6-aminocapronitrile reaction with reference to Example 1, the difference is that the catalyst TiO 2 -1 for TiO 2 -2, all the other steps are with reference to Example 1, and the catalytic results are listed in Table 1. Catalyst TiO 2 -2 lifespan as image 3 shown.
Embodiment 3
[0060] The treatment method step of oxide surface is with reference to embodiment 1, and difference is that in step (2) reducing agent NaBH 4 and TiO 2 Mass ratio is changed into 2:1, all the other steps are with embodiment 1, the TiO after processing 2 denoted as TiO 2 -3,TiO 2 -3 photos such as figure 1 as shown in c.
[0061] The surface treated oxide TiO 2 -3 is used as a catalyst to catalyze the specific steps of the caprolactam system 6-aminocapronitrile reaction with reference to Example 1, the difference is that the catalyst TiO 2 -1 for TiO 2 -3, all the other steps are with reference to Example 1, and the catalytic results are listed in Table 1.
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