Heteropolyacid catalyst and preparation method thereof

A heteropolyacid salt and catalyst technology, applied in the field of heteropolyacid salt catalyst and its preparation, can solve the problems of production efficiency reduction, restriction of industrial production efficiency, reactant overoxidation, etc.

Active Publication Date: 2015-07-29
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the above various improvement methods have been adopted, due to the large particle size and small specific surface area of ​​the catalyst prepared by the co-precipitation method, the local heat accumulation in the reaction process is still relatively serious, which not only causes the overoxidation of the reactants, b...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 20g of molybdenum trioxide, 1g of vanadium pentoxide and 1.5g of 85% phosphoric acid in 150ml of deionized water, and heat the solution under reflux at 90-100° C. for 5 hours to obtain a red transparent solution. Cool the above solution to room temperature, then add 50 g of silicon carbide powder to the solution, and stir for 60 minutes to make the phosphorus molybdenum vanadium heteropolyacid absorbed by silicon carbide, which is called material A.

[0031] Mix 5 g of ferric nitrate, 10 g of copper nitrate, 4 g of arsenic pentoxide, and 2.5 g of potassium nitrate in 200 ml of deionized water to obtain solution B.

[0032] Add solution B to material A under stirring to obtain a blue slurry, continue stirring for 60 minutes, then dry, calcinate at 400°C for 4 hours, and press into tablets to obtain catalyst A.

[0033] Catalyst has composition (excluding heat conducting agent):

[0034] P 1.12 Mo 12 V 0.95 As 3.0 Fe 1.07 Cu 3.58 K 2.14

Embodiment 2

[0036] Add 20g of molybdenum trioxide, 1g of vanadium pentoxide and 1.5g of 85% phosphoric acid in 150ml of deionized water, and heat the solution under reflux at 90-100° C. for 5 hours to obtain a red transparent solution. Cool the above solution to room temperature, then add 50 g of silicon carbide powder to the solution, and stir for 60 minutes to make the phosphorus molybdenum vanadium heteropolyacid absorbed by silicon carbide, which is called material A.

[0037] Mix 5 g of ferric nitrate, 10 g of copper nitrate, 3 g of antimony pentoxide, and 4.51 g of cesium nitrate in 200 ml of deionized water to obtain solution B.

[0038] Add solution B to material A under stirring to obtain a blue slurry, continue stirring for 60 minutes, then dry, calcinate at 450°C for 3 hours, and press into tablets to obtain catalyst B.

[0039] Catalyst has composition (excluding heat conducting agent):

[0040] P 1.12 Mo 12 V 0.95 Sb 1.60 Fe 1.07 Cu 3.58 Cs 2.0

Embodiment 3

[0042] Add 20g of molybdenum trioxide, 1g of vanadium pentoxide and 1.5g of 85% phosphoric acid in 150ml of deionized water, and heat the solution under reflux at 90-100° C. for 5 hours to obtain a red transparent solution. Cool the above solution to room temperature, then add 50 g of silicon carbide powder to the solution, and stir for 60 minutes to make the phosphorus molybdenum vanadium heteropolyacid absorbed by silicon carbide, which is called material A.

[0043] Mix 5 g of ferric nitrate, 10 g of copper nitrate, 2 g of arsenic pentoxide, 3 g of antimony pentoxide, and 2.5 g of potassium nitrate in 200 ml of deionized water to obtain solution B.

[0044] Add solution B to material A under stirring to obtain a blue slurry, continue to stir for 60 minutes, then dry, calcinate at 400°C for 10 hours, and press into tablets to obtain catalyst C.

[0045] Catalyst has composition (excluding heat conducting agent):

[0046] P 1.12 Mo 12 V 0.95 As 1.50 Sb 1.60 Fe 1.07 Cu ...

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PUM

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Abstract

The invention provides a heteropolyacid catalyst and a preparation method thereof. The chemical formula of the catalyst is as follows: PaMo12VbAcBdCeDfOg. Solid heat-conduction powder is added to an aqueous solution containing phosphorus, molybdenum and alum, so that molybdovanadophosphoric acid generated in a reaction is attached to the surface of the solid heat-conduction powder, then other saline solutions are added, and heteropolyacid deposition layers are uniformly supported on surfaces of solids. The catalyst with good product selectivity, long service life and high mechanical strength is obtained through drying, roasting, forming and other procedures. The catalyst obtained with the preparation method can be applied to selective oxidation preparation of methacrylic acid through methylacrolein.

Description

technical field [0001] The invention relates to a preparation method of a heteropolyacid salt catalyst and its application in the reaction of preparing methacrylic acid through the selective oxidation of methacrolein. Background technique [0002] Methyl methacrylate (MMA) is an important chemical intermediate, mainly used in the production of plexiglass, and can also be polymerized with other monomers to form copolymers, used for coating modifiers, polyvinyl chloride modifiers and Medical polymer materials, etc. At present, the production of methacrylic acid (MAA) has acetone cyanohydrin method, methacrolein method, etc. From the perspective of environmental protection and economic technology, the production of MAA with methacrolein as a raw material has a good development prospect. Using methacrolein as a raw material to prepare MAA requires the use of heteropolyacid salts as catalysts. The higher activity of the catalysts can easily cause peroxidation and reduce the yiel...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C51/235C07C57/055
Inventor 任万忠房德仁王文华许文友陈小平
Owner YANTAI UNIV
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