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Kaolin-loaded Keggin type heteropolyacid catalyst, preparation and application in methylacrolein oxidation

A technology of heteropoly acid and catalyst, which is applied in the field of catalyst preparation and application to achieve the effects of abundant raw materials, high MAL conversion rate and large specific surface area

Pending Publication Date: 2022-08-05
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that it is still a huge challenge to select a carrier with high thermal stability and suitable acidity and alkalinity for the preparation of supported heteropolyacid catalysts.

Method used

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  • Kaolin-loaded Keggin type heteropolyacid catalyst, preparation and application in methylacrolein oxidation
  • Kaolin-loaded Keggin type heteropolyacid catalyst, preparation and application in methylacrolein oxidation
  • Kaolin-loaded Keggin type heteropolyacid catalyst, preparation and application in methylacrolein oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation steps of the catalyst are as follows: 1) Take 15 g of phosphomolybdic vanadium heteropoly acid, dissolve it in 300 mL of water, and stir evenly. Then take 0.705gCsOH . H 2 O was dissolved in water and added dropwise; then 0.235g KOH was dissolved in water and added dropwise; then 0.332g NH was taken 4 HCO 3 Dissolved in water, added dropwise and stirred for 8h to obtain Cs + , NH 4 + and K + Modified phosphomolybdic vanadium heteropoly acid solution. Then, the solution was evaporated in a rotary evaporator until about 50 mL remained, the sample was transferred to a watch glass, and dried at 80° C. overnight to obtain a heteropolyacid catalyst precursor.

[0035] 2) then get 6g kaolin carrier and put it into the 250mL flask (A); get 8g heteropolyacid catalyst precursor and put it in the beaker, add deionized water to it, stir (B); B is slowly added dropwise to A , stirred for 5 h, then transferred the sample to a watch glass and dried at 80 °C ove...

Embodiment 2

[0039] Dissolve 15 g of phosphomolybdic vanadium heteropoly acid in 200 mL of water and stir evenly. Then take 0.705gCsOH . H 2 O was dissolved in water, added dropwise and stirred for 3h to obtain Cs + Modified phosphomolybdic vanadium heteropoly acid solution. Then, the solution was evaporated in a rotary evaporator until about 50 mL remained, and the sample was transferred to a watch glass and dried overnight to obtain a heteropolyacid catalyst precursor.

[0040] Then get 6g kaolin carrier and put it in 250mL flask (A); Get 5g heteropolyacid catalyst precursor and put it in the beaker, add deionized water to it, and stir (B); B is slowly added dropwise to A, After stirring for 9 h, the sample was transferred to a watch glass and dried overnight to obtain a supported catalyst precursor. The precursor was calcined in nitrogen at 340 °C for 10 h to obtain the target catalyst: Cs 0.5 H 3.5 PMo 11 VO 40 / Kaolin, in which the active component Cs 0.5 H 3.5 PMo 11 VO 4...

Embodiment 3

[0043] Dissolve 15 g of phosphomolybdic vanadium heteropoly acid in 400 mL of water and stir evenly. Then dissolve 0.504g NaOH in water, add dropwise, then dissolve 0.7056g KOH in water, add dropwise, stir for 5h to obtain Na + and K + Modified phosphomolybdic vanadium heteropoly acid solution. Then, the solution was evaporated in a rotary evaporator until about 40 mL remained, the sample was transferred to a watch glass, and dried at 68°C overnight to obtain a heteropolyacid catalyst precursor.

[0044] Then get 7g kaolin carrier and put it in the 250mL flask (A); get 3g heteropolyacid catalyst precursor and put it in the beaker, add deionized water to it, and stir (B); B is slowly added dropwise to A, After stirring for 8 h, the sample was transferred to a watch glass and dried at 70 °C overnight to obtain a supported catalyst precursor. The precursor was calcined in air at 380 °C for 11 h to obtain the target catalyst: Na 1.5 K 1.5 HPMo 11 VO 40 / Kaolin, in which the...

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Abstract

The invention relates to a kaolin-loaded Keggin type heteropolyacid catalyst, preparation thereof and application of the kaolin-loaded Keggin type heteropolyacid catalyst in methylacrolein oxidation. The invention provides a Keggin type heteropolyacid loaded composite catalyst with kaolin as a carrier and a preparation method of the Keggin type heteropolyacid loaded composite catalyst, heteropolyacid is highly dispersed and loaded on the kaolin carrier, and the prepared catalyst shows very high selectivity and stability for a reaction for preparing MAA through MAL gas phase oxidation. The composition of the catalyst is XaPMo12-dVdO40 / Kaolin, X is one or more of counter ions, Kaolin represents a kaolin carrier, and a is the atom number of the X element in the catalyst and is 0.5-3; d is the number of vanadium atoms and is 0 or 1; in the supported catalyst, XaPMo12-dVdO40 is used as an active component, and kaolin is used as a carrier. When the catalyst is used for oxidizing methylacrolein into methacrylic acid, the catalyst has high MAL conversion rate and high MAA selectivity.

Description

technical field [0001] The invention relates to a kaolin-supported Keggin-type heteropoly acid catalyst and its preparation and application in the oxidation of methacrolein, and belongs to the field of catalyst preparation and application. Background technique [0002] Methyl methacrylate (MMA) is an important organic polymer monomer, mainly used in liquid crystal display light guide plates, medical functional materials, plexiglass, printing and dyeing auxiliaries, waterproofing agents, adhesives, PVC modifiers Wait. Widely used and in great demand, it has received more and more attention. [0003] There are three main synthesis methods of MMA, namely: acetone cyanohydrin method (ACH method), isobutylene oxidation method, and ethylene carbonylation method. The acetone cyanohydrin method is the most widely used method for producing MMA, but this process uses highly toxic hydrocyanic acid and highly corrosive concentrated sulfuric acid in the production process. Although th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/199B01J27/24B01J35/10B01J37/02B01J37/08C07C51/235C07C57/045
CPCB01J27/199B01J27/24B01J37/0201B01J37/08C07C51/235B01J35/613C07C57/04Y02P20/584
Inventor 汪宝和朱倩文马静朱璟
Owner TIANJIN UNIV
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