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Preparation method of catalyst for preparing unsaturated aldehyde and unsaturated acid in high selectivity

An acid catalyst, high selectivity technology, applied in the direction of oxidation to prepare carboxylic acid, oxidation to prepare carbonyl compounds, etc., can solve the problems of uneven mixing, poor repeatability, affecting catalyst performance, etc., to reduce yield and selectivity. improved effect

Inactive Publication Date: 2011-03-30
SHANGHAI HUAYI ACRYLIC-ACID CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the molybdenum oxide is roasted by ammonium molybdate, environmental factors such as temperature and atmosphere in the roasting process have a great influence on the color, type, grain size, and specific surface area of ​​the obtained molybdenum oxide. Then it affects the performance of the catalyst obtained after adding, and because it is added in the form of solid to the preparation process of the catalyst, there is a problem of uneven mixing, resulting in poor repeatability
Another more important problem is that we found in the research that the catalyst described in this patent cannot be well applied to the high space velocity reaction, and it can only be used at a lower propylene space velocity. When the propylene space velocity increases Especially up to 80h -1 Above, the rate of decline in conversion rate is very significant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021]Heat 3000mL of water to 60°C, add 1421.6g of ammonium molybdate and 6.8g of potassium nitrate, stir and dissolve to obtain solution (1), and keep the temperature at 70°C. After heating 1300mL of water to 50°C, add 1009.1g of cobalt nitrate, 543.3g of nickel nitrate, and 484.0g of iron nitrate in sequence, and stir to dissolve. ~70°C. Prepare 300ml of ammonia water. Under vigorous stirring at 70°C, drop the solution of (2) into the solution of (1), and at the same time add ammonia water to maintain the pH value of the slurry. Continue to stir until the mixture is homogeneous. The slurry was dried at 145°C for 24 hours, and the dried sample was pulverized and calcined at 210°C for 15 hours. The obtained powder and silicon powder are mixed evenly into a mixture according to a 7:3 weight ratio, and 3% by weight graphite of the mixture weight is added and SiO 2 The silica sol with a content of 2% by weight is mixed, extruded into particles with a diameter of 1 mm and a le...

Embodiment 2

[0024] Heat 3000mL of water to 60°C, add 1421.6g of ammonium molybdate and 6.8g of potassium nitrate, stir and dissolve to obtain solution (1), and keep the temperature at 70°C. After heating 1300mL of water to 50°C, add 1009.1g of cobalt nitrate, 543.3g of nickel nitrate, and 484.0g of iron nitrate in sequence, and stir to dissolve. ~70°C. Prepare 300ml of ammonia water. Under vigorous stirring at 70°C, drop the solution of (2) into the solution of (1), and at the same time add ammonia water to maintain the pH value of the slurry. Continue to stir until the mixture is homogeneous. The slurry was dried at 145°C for 24 hours, and the dried sample was pulverized and calcined at 210°C for 15 hours. The obtained powder and silicon powder are mixed evenly into a mixture according to a 7:3 weight ratio, and 3% graphite of the mixture weight is added and SiO 2 Silica sol with a content of 2% by weight is mixed, extruded into particles with a diameter of 1 mm and a length of 1 to ...

Embodiment 3

[0027] The preparation process is the same as in Example 2, except that 520.0 g of ammonium tungstate is added to solution (1), stirred and dissolved to obtain solution (1), solution (2) is changed to add 1060.4 g of cobalt nitrate, 556.6 g of iron nitrate, stirred and dissolved, and then Add 4ml of nitric acid and 490.2g of bismuth nitrate, stir and dissolve to obtain solution (2), and the rest of the preparation method is the same as in Example 3.

[0028] Get 50 grams of catalyst and pack in the fixed-bed tubular reactor, pass into the mixed gas of propylene after preheating, air, steam, the mol ratio of propylene / oxygen / water / is 1: 1.8: 1.5, and total space velocity is 1600h -1 . After 200 hours of reaction, the reaction temperature was 342°C, the conversion rate of propylene was 98.3%, the yield of acrolein and acrylic acid was 94.8%, and the yield of carbon oxide was 2.3%.

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Abstract

The invention discloses a preparation method of a catalyst for preparing unsaturated aldehyde and unsaturated acid in high selectivity. The catalyst is Mo-Bi-Fe-Co composite metal oxide. On the basis of a co-precipitation preparation method, a two-section roasting process is introduced, and simultaneously, a method for adjusting a formula and a method for treating by water solutions of soluble molybdenum, alkali metal and alkali earth metal are combined, so that the selectivity of the catalyst is greatly improved, the yield of the carbon oxide is effectively reduced, and the catalyst can be used for preparing the unsaturated aldehyde and the unsaturated acid in high selectivity, still has very good activity and stability at a high air speed and is suitable for tail gas recycling or non-tail gas recycling processes.

Description

technical field [0001] The invention relates to a method for preparing unsaturated aldehyde and unsaturated acid catalyst with high selectivity. The prepared catalyst can prepare unsaturated aldehyde and unsaturated acid with high selectivity, and still has good activity and Stability, suitable for tail gas recirculation or non-tail gas recirculation process. Background technique [0002] Low-carbon unsaturated acids, including acrylic acid and methacrylic acid, are important organic chemical products. They are mainly prepared industrially by two-step oxidation of olefins, that is, olefins are partially oxidized on Mo-Bi composite oxide catalysts to form aldehydes, and the resulting aldehydes Further oxidation on Mo-V composite oxide or heteropolyacid catalyst to generate the corresponding acid. In order to increase the production capacity of the production device, the method of increasing the concentration of propylene in the feed gas or the method of increasing the space ...

Claims

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Application Information

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IPC IPC(8): B01J23/887B01J23/888C07C57/04C07C51/16C07C47/22C07C45/28
Inventor 李雪梅焦昆王剑施凯敏庄岩马建学褚小东邵敬铭
Owner SHANGHAI HUAYI ACRYLIC-ACID CO LTD
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