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Loaded heteropolyacid catalyst for preparing methacrylic acid through oxidization of methacrolein

A technology for supporting heteropolyacids and catalysts, which can be applied in physical/chemical process catalysts, molecular sieve catalysts, organic compound/hydride/coordination complex catalysts, etc. Catalyst activity and other issues, to achieve the effect of improving catalyst performance, low price, and improving catalytic performance

Active Publication Date: 2016-03-02
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, directly loading phosphomolybdic acid or phosphomolybdovanadic acid on the carrier can be combined with SiO on the surface of the carrier 2 reaction, reducing the activity of the catalyst, and it is easy to lose during the reaction
Therefore, in most of the current studies, the amination of the carrier is adopted. The amination method used needs to be roasted in an ammonia atmosphere at a high temperature (900°C). produced industrially and supported on aminated SiO 2 However, the catalyst still has the problem of poor thermal stability and deactivation due to decomposition. Therefore, it is necessary to develop a new preparation or modified carrier technology to prepare a supported heteropolyacid catalyst with high activity and strong thermal stability.

Method used

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  • Loaded heteropolyacid catalyst for preparing methacrylic acid through oxidization of methacrolein
  • Loaded heteropolyacid catalyst for preparing methacrylic acid through oxidization of methacrolein
  • Loaded heteropolyacid catalyst for preparing methacrylic acid through oxidization of methacrolein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 3g of urea, dissolve it in 50mL of deionized water, and make 10g of urea have a specific surface area of ​​500m 2 g -1 SiO 2 Added to the solution, stirred at 60°C for 2h, stirred and dried at 80°C, and dried the obtained solid in a drying oven at 80°C for 12h. Put the dried solid into a sealed quartz dish, then put it into a muffle furnace, raise it to 550°C at 5°C / min, and bake it for 5h. After the calcination, the modified SiO 2 carrier.

[0031] Weigh 10g of phosphomolybdovanadic acid, dissolve it in 50mL of deionized water, and dissolve the modified SiO 2 Add it to the phosphomolybdovanadic acid solution, raise the temperature to 80°C, and stir vigorously for 6 hours to obtain a yellow suspension.

[0032] Weigh 1.09gCsNO 3 , 0.021gY (NO 3 ) 3 ·6H 2 O, 0.053gCu(NO 3 ) 2 , 0.272gFe(NO 3 ) 3 Dissolve in 20 mL deionized water. Then the prepared solution was slowly added dropwise to the above suspension, and after the dropwise addition was completed...

Embodiment 2

[0038] Weigh 6g of urea, dissolve it in 50mL deionized water, and make 10g specific surface area 1000m 2 g -1 The SBA-15 molecular sieve was added to the solution, stirred at 50°C for 2h, stirred and dried at 80°C, and the obtained solid was dried in a drying oven at 80°C for 12h. Put the dried solid into a sealed quartz dish, then put it into a muffle furnace, raise it to 550°C at 5°C / min, and bake it for 5h. After the calcination, the modified SBA-15 carrier is obtained.

[0039] Weigh 20g of phosphomolybdovanadic acid, dissolve it in 50mL of deionized water, add the modified SBA-15 into the phosphomolybdovanadic acid solution, raise the temperature to 80°C, and stir vigorously for 6 hours to obtain a yellow suspension.

[0040] Weigh 2.188gCsNO 3 , 1.593gH 3 AsO 4 , 0.425gZn (NO 3 ) 2 , 0.411gSn (NO 3 ) 4 , 0.165gNbO(NO 3 ) 3 Dissolve in 20 mL deionized water. Then the prepared solution was slowly added dropwise to the above suspension, and after the dropwise ad...

Embodiment 3

[0045] Weigh 4g of melamine, dissolve it in 50mL hot deionized water, make 10g specific surface area 1000m 2 g -1 The MCM-41 molecular sieves were added to the solution, stirred at 80°C for 6h, stirred and dried at 80°C, and the obtained solid was dried in a drying oven at 80°C for 12h. Put the dried solid into a sealed quartz dish, then put it into a muffle furnace, raise it to 550°C at 5°C / min, and bake it for 5h. After the calcination, the modified MCM-41 carrier is obtained.

[0046] Weigh 10g of phosphomolybdovanadic acid, dissolve it in 50mL of deionized water, add the modified MCM-41 into the phosphomolybdovanadic acid solution, raise the temperature to 80°C, and stir vigorously for 6 hours to obtain a yellow suspension.

[0047] Weigh 1.094gCsNO 3 , 0.316gCu(NO 3 ) 2 , 0.327gCo(NO 3 ) 2 ·6H 2 O, 0.072gZr(NO 3 ) 2 , 0.133gTi(NO 3 ) 4 Dissolve in 20 mL deionized water. Then the prepared solution was slowly added dropwise to the above suspension, and after th...

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Abstract

The invention relates to a heteropolyacid catalyst loaded with a modified silicon oxide carrier for preparing methacrylic acid through oxidization of methacrolein. Firstly, polymerization is conducted on the surface of the silicon oxide carrier through calcination of amino compounds to generate a carbonized nitrogen layer containing a proper number of amino groups; then, heteropolyacid loading is conducted through the amino groups on the surface of the carrier, counter ions are added, and then the loaded heteropolyacid catalyst is obtained. The catalyst prepared with the method has excellent catalytic performance in reaction for preparing methacrylic acid through oxidization of methacrolein, and has a long catalysis life.

Description

technical field [0001] The invention relates to a heteropolyacid catalyst for preparing methacrylic acid by oxidation of methacrolein and a preparation method thereof, belonging to the field of catalyst preparation and application. Background technique [0002] Methyl methacrylate (MMA) is an important industrial intermediate, which can be used to produce plexiglass, functional polymer materials and plasticizers. The traditional process of producing MMA is the acetone cyanohydrin method. Although the process is mature, it uses raw materials such as highly toxic hydrocyanic acid and corrosive sulfuric acid, and will produce a large amount of solid waste such as ammonium bisulfate, which is harmful to the environment. Pollution is high, so new clean alternative processes are needed. In the new process currently developed, it can be divided into three-step method and four-step method based on the number of reaction steps. The four-step method is to first generate acrolein thro...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C51/25C07C57/055
CPCB01J27/19B01J27/24B01J29/0341C07C51/252C07C57/04
Inventor 张锁江周理龙王蕾曹云丽闫瑞一刁琰琰韩军兴
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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