Method for preparing catalyst in preparation of acrylic acid by oxidizing acrolein

A technology of catalyst and acrolein, which is applied in the preparation of organic compounds, preparation of carboxylate, chemical instruments and methods, etc., can solve the problems of low conversion rate of acrolein, affecting catalyst stability, reducing catalyst activity, etc., to avoid The effect of hot spot jumping or flying temperature

Active Publication Date: 2013-03-20
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have played a certain role in suppressing the temperature of the hot spot, but generally the amount of catalyst active material at the feed gas inlet of the reactor is less than the amount of catalyst active material at the outlet, resulting in that the catalyst at the inlet loses more than the catalyst at the outlet. Live fast, which affects the stability of the catalyst for long-term operation under high-yield conditions
Adding toxic components to reduce the activity of the catalyst, although it can achieve the effect of suppressing the temperature of the superheated part, makes the conversion rate of acrolein not high in the early stage, resulting in a decrease in the yield, and the toxic components are adsorbed on the active sites of the catalyst Later, after a longer oxidation reaction, it will affect the stability of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 163g of ammonium molybdate, 31.3g of ammonium metatungstate and 47.5g of ammonium metavanadate into 750g of water at 80°C, stir and dissolve to obtain solution A; add 2.1g of lanthanum nitrate and 47.4g of copper nitrate into 100g of water at 60°C, stir Dissolve to obtain solution B, pour solution B into solution A at 60°C to obtain solution C, and dry solution C at 150°C for 10 hours to obtain dry powder. 19.5g of silica sol (20wt%) was added to 100g of dry powder and 88g of silica powder, mixed evenly, extruded into cylindrical particles with a diameter of 1mm and a length of 2mm, and calcined at 380°C for 5h to obtain a shaped catalyst.

[0015] The oxidation reaction is carried out on a small evaluation reaction device with an inner diameter of 20mm (with a casing with an outer diameter of 3mm), the loading amount of the shaped catalyst is 15ml, and the volume percentage of the raw material gas is: acrolein 7%, oxygen 9%, water vapor 15% %, unreacted propylene a...

Embodiment 2

[0017] Add 163g of ammonium molybdate, 28.7g of ammonium metatungstate and 39.5g of ammonium metavanadate to 750g of water at 80°C, stir and dissolve to obtain solution A; add 47.4g of copper nitrate and 2.8g of strontium nitrate into 100g of water at 60°C, stir Dissolve to obtain solution B, pour solution B into solution A at 60°C to obtain solution C, and dry solution C at 150°C for 10 hours to obtain dry powder. Add 12g of propylene glycol and 19.5g of silica sol (20wt%) to 100g of dry powder and 88g of silicon powder, mix evenly, extrude to form cylindrical particles with a diameter of 1mm and a length of 2mm, and roast at 380°C for 5h in nitrogen to obtain a shaped catalyst.

[0018] The oxidation reaction is carried out on a small evaluation reaction device with an inner diameter of 20mm (with a casing with an outer diameter of 3mm), the loading amount of the shaped catalyst is 15ml, and the volume percentage of the raw material gas is: acrolein 7%, oxygen 10%, water vapo...

Embodiment 3

[0020] Add 22g of ethylene glycol, 130.2g of ammonium molybdate, 28.4g of ammonium metatungstate and 38.1g of ammonium metavanadate into 600g of water at 90°C, stir and dissolve to obtain solution A; add 2.6g of lanthanum nitrate, 4.2g of ammonium niobium oxalate and 38.1g of copper nitrate were stirred and dissolved to obtain solution B, and solution B was poured into solution A at 60°C to obtain solution C, and solution C was dried at 120°C for 20 hours to obtain dry powder. Add 3.8g of graphite and 19g of silica sol (30%) to 100g of dry powder and 90g of silicon powder, mix evenly, knead and extrude to form cylindrical particles with a diameter of 1mm and a length of 2mm. The particles were calcined at 380° C. for 5 h in air to obtain a shaped catalyst.

[0021] The oxidation reaction is carried out on a small evaluation reaction device with an inner diameter of 20mm (with a casing with an outer diameter of 3mm), the loading amount of the shaped catalyst is 15ml, and the vo...

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PUM

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Abstract

The invention relates to a method for preparing a catalyst in preparation of acrylic acid by oxidizing acrolein. The general formula of the catalyst is Mo12VaCubWcXdYeOf / Z; and the catalyst is molded by baking for 1 to 24h at the temperature of between 350 and 410 DEG C, and is treated for 3 to 60 hours in mixed gas of air and vapor in any proportion at the temperature of between 260 and 390 DEG C before reaction. The method has the characteristics that: after the catalyst is treated before the reaction, the activity is greatly improved and the catalyst can achieve a steady state at an initial stage of the reaction, so that the danger that the interlocking is caused or the catalyst is damaged caused by hot spot jump or temperature runaway due to overhigh temperature in the running process is avoided; and the catalyst is favorable for being used on industrial devices and is applicable to exhaust gas cycling and non-exhaust gas cycling processes.

Description

technical field [0001] The invention relates to a preparation method and application of a catalyst for acrolein oxidation to acrylic acid. Background technique [0002] Mo-V system composite oxide is an effective catalyst for the oxidation of acrolein to acrylic acid. In industrial production, in order to increase the output, the raw material containing acrolein with a higher concentration or the method of increasing the space velocity is adopted, and the inherent strong exothermic nature of the reaction causes a large amount of heat generated during the reaction to form a high temperature in the catalyst bed. Partially, it is easy to cause excessive oxidation to reduce the selectivity and yield of the catalyst, and also cause accelerated deactivation or even damage of the catalyst. The bigger problem it brings is that the reaction is out of control due to excessive bed temperature or overheating, which makes the driving process extremely difficult, and even faces chain pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/888C07C57/04C07C57/055C07C51/25
Inventor 李雪梅冯世强庄岩施凯敏马建学诸小东邵敬铭
Owner SHANGHAI HUAYI NEW MATERIAL
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