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Method for preparing antimony-containing catalyst used for ammoxidation of alkane

An oxidation reaction and catalyst technology, which can be used in the preparation of hydrocarbon ammoxidation, catalyst activation/preparation, physical/chemical process catalysts, etc. Good catalyst stability, good test results, good repeatability

Active Publication Date: 2012-09-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The technical problem to be solved by the present invention is to overcome problems such as the complex preparation process and low yield caused by the reflux of Sb whiskers in the prior art documents, the easy volatilization of active components and the poor stability of the catalyst, etc., and provide a new method for Preparation method of antimony-containing catalyst for alkane ammoxidation reaction

Method used

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  • Method for preparing antimony-containing catalyst used for ammoxidation of alkane
  • Method for preparing antimony-containing catalyst used for ammoxidation of alkane
  • Method for preparing antimony-containing catalyst used for ammoxidation of alkane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 17.0 grams of ammonium heptamolybdate and 2.4 grams of antimony trioxide were dissolved in 40.0 grams of hot water to make solution (I); 3.37 grams of ammonium metavanadate were dissolved in 70.0 grams of hot water to make solution (II) ; Dissolve 2.99 grams of niobium oxalate in 9.0 grams of hot water to make a solution (III); dissolve 3.0 grams of oxalic acid in 5 grams of water to make a solution (IV). Solution (I) is joined in the solution (II) under stirring, then add solution (III) and solution (IV) successively, finally add 50 grams of silica sols that weight concentration is 40%, make the slurry of catalyst, will The slurry was stirred and evaporated at 90°C until a viscous slurry was obtained, then dried, ground, calcined in an air atmosphere at 300°C for 1 hour, and then calcined in a nitrogen atmosphere at 600°C with a flow rate of 60 ml / min for 2 hours. Propane ammoxidation catalyst 50% Mo 1 V 0.3 Nb 0.17 Sb 0.1 o x +50% SiO2 2 After tableting, 20-40 m...

Embodiment 2～5 and comparative example 2～4

[0049] Catalysts with different compositions in the following table were prepared by the same method as in Example 1, and the ammoxidation of propane to acrylonitrile was carried out under the following reaction conditions with the prepared catalyst. See Table 1 for specific changes and results.

[0050] The reaction conditions of above-mentioned embodiment and comparative example are:

[0051] Fixed bed reactor with an inner diameter of 8 mm

[0052] Reaction temperature 400°C

[0053] Reaction pressure Atmospheric pressure

[0054] Catalyst loading 2.0 grams

[0055] Catalyst contact time 1.2 g·s / ml

[0056] Raw material ratio (mole) propane / ammonia / air=1 / 1.2 / 10

[0057] Table 1

[0058]

Example

Catalyst composition

Preparation key steps

propane

Conversion rates%

Acrylonitrile

selectivity%

Example 1

50%Mo 1 V 0.3 Nb 0.17 Sb 0.1 o x +50% SiO2 2

O...

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Abstract

The invention relates to a method for preparing an antimony-containing catalyst used for ammoxidation of alkane, which mainly solves the problem of poor stability of the catalyst due to difficult stable combination between Sb and Mo, complex preparation process, unstable preparation environment and easy volatilization of active ingredients of the catalyst existing in the prior art. In the method,the Mo-V-Nb-Sb base is used as a main ingredient of the catalyst, and a silica carrier and a composition including the MoVaNbbSbcDdOx general formula based on an atomic ratio are contained, wherein Dis one of Sn, Ti, Fe, Bi, Te and W. The preparation environment is changed by dissolving corresponding salts or oxides of Mo and Sb; then respectively adding the solution of the corresponding salts or the oxides of V and Nb into the mixture; adding a proper amount of reducing agent into the mixture; and finally adding silica sol into the mixture. The technical scheme adopting a two-stage calcination mode can better solve the problem. The method can be applied to industrial production of unsaturated nitriles by using ammoxidation of alkane.

Description

technical field [0001] The invention relates to a method for preparing an antimony-containing catalyst used for alkane ammoxidation. In particular, it relates to a method for preparing a catalyst for producing acrylonitrile by ammoxidation of propane or a catalyst for producing methacrylonitrile by ammoxidation of isobutane. Background technique [0002] Although most of the production of acrylonitrile currently adopts the propylene ammoxidation process of BP / Sohio, with the changes in the petrochemical market and the in-depth research on the selective oxidation of alkanes, due to the price difference between propane and propylene or the price of isobutane and isobutene The process route of producing acrylonitrile by propane ammoxidation or isobutane ammoxidation to methacrylonitrile has been paid more and more attention. [0003] In order to obtain a catalyst with high activity and high selectivity for the ammoxidation of propane to acrylonitrile, people have made a series...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/28B01J23/30B01J23/31B01J37/16B01J37/08C07C253/24C07C255/08
CPCY02P20/52
Inventor 缪晓春张顺海汪国军吴粮华
Owner CHINA PETROLEUM & CHEM CORP
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