Aldol condensation catalyst, preparation method and method for preparing methyl methacrylate with it

An aldol condensation and catalyst technology, which is applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as insufficient industrial demand, high wear, and poor catalyst strength, and achieve significant industrial applications value, reduce carbon deposition, and improve water resistance

Active Publication Date: 2022-04-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Disclosed in CN104525176B is a kind of microsphere catalyst for fluidized bed. The catalyst has the characteristics of low attrition. Combined with the reaction process control, the cyclic regeneration of the catalyst can be realized, but it still has the disadvantage that the catalyst strength gradually deteriorates and the final attrition is too high.
[0008] Although the above-mentioned patented methods can improve certain performances of the catalyst to a certain extent, they are still insufficient for industrialization. It is necessary to further improve the water resistance of the catalyst, reduce carbon deposition, and finally achieve the purpose of improving the life of the catalyst.

Method used

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  • Aldol condensation catalyst, preparation method and method for preparing methyl methacrylate with it
  • Aldol condensation catalyst, preparation method and method for preparing methyl methacrylate with it
  • Aldol condensation catalyst, preparation method and method for preparing methyl methacrylate with it

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Take 6.82g of zirconium nitrate, 1.16g of bismuth nitrate, 2.78g of aluminum nitrate, 5g of concentrated nitric acid dissolved in 90g of deionized water, add 100g of foamed silica PSI-1, impregnate for 12h, dry at 90°C for 3h, then dry at 120°C 2h, and calcined at 450°C for 3h to prepare a modified foamed silica carrier.

[0072] Dissolve 2.93g of cesium nitrate and 0.646g of potassium nitrate in 45g of deionized water, add 50g of the above-mentioned modified silica carrier, soak for 12h, then dry at 90°C for 3h, and then dry at 120°C for 2h to obtain catalyst precursor A. Catalyst precursor A in 100mL / min N containing 13% water vapor 2 , the temperature was raised to 500°C at 2°C / min, and after being treated for 5 hours, it was taken out and cooled down to room temperature to obtain catalyst precursor B. The catalyst precursor B was soaked in 100 g of a mixture of methanol and methyl propionate (methanol accounted for 40%) for 20 h, and dried at 110° C. for 2 h after ...

Embodiment 2

[0077] Take 2.36g of zirconium nitrate, 0.29g of ammonium metavanadate, 0.24g of antimony acetate and dissolve them in 90g of deionized water, add 100g of foamed silica PSI-1, soak for 12h, dry at 90°C for 3h, then dry at 110°C for 10h , Calcined at 600°C for 1h to obtain a modified foamed silica carrier.

[0078] Dissolve 3.22g of cesium hydroxide and 0.19g of sodium hydroxide in 45g of deionized water, add 50g of the above-mentioned modified carrier, soak for 12h, then dry at 90°C for 3h, and then dry at 110°C for 10h to obtain catalyst precursor A. Catalyst precursor A in 200mL / min N containing 5% water vapor 2 , the temperature was raised to 600°C at 2°C / min, and the catalyst precursor B was obtained after being treated for 1 hour and then taken out and lowered to room temperature. The catalyst precursor B was soaked in 100 g of methanol and methyl propionate mixture (methanol accounted for 10%) for 15 h, and dried at 100° C. for 2 h after removing the liquid to prepare t...

Embodiment 3

[0083] Take 100g of foamed silica PSI-2 and place it at 300°C for 4 hours to calcinate to obtain a modified foamed silica carrier.

[0084] Dissolve 5.05g of cesium hydroxide in 45g of deionized water, add 50g of the above-mentioned modified carrier, impregnate for 12h, then dry at 90°C for 3h, and then dry at 120°C for 2h to obtain catalyst precursor A. Catalyst precursor A in 200mL / min N containing 6% water vapor 2 , the temperature was raised to 550°C at 2°C / min, and the catalyst precursor B was obtained after being treated for 3 hours and then taken out and lowered to room temperature. The catalyst precursor B was soaked in 100 g of methanol and methyl propionate mixture (methanol accounted for 20%) for 30 h, and dried at 100° C. for 2 h after removing the liquid to prepare the catalyst.

[0085] The measured free Cs content of the catalyst is 0.09%, and the BET specific surface area is 209m2 / g, the average pore diameter is 11.35nm.

[0086] The catalyst was tested for ...

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Abstract

The invention provides an aldol condensation catalyst, a preparation method and a method for preparing methyl methacrylate with it. The catalyst of the present invention includes a modified silica carrier and an alkali metal element loaded on the carrier, wherein the modified silica carrier is a foam porous structure, which has the first macropores with a diameter of 10-1000 μm. The first range, and the second range composed of submicron pores of 2nm to 500nm; the thickest part of any part of the support is <1mm; the alkali metal loading on the catalyst is 4 to 9wt% (calculated as alkali metal elements), and the free alkali metal loading The amount is <0.5wt%; the total loading amount of the modifier is 0.5-3wt% (calculated as the modifier element). The catalyst provided by the invention has excellent water resistance, carbon deposition resistance and long-term activity stability, and is suitable for the industrial application of methyl methacrylate prepared by aldol condensation of methyl propionate and formaldehyde.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to an aldol condensation catalyst and a preparation method thereof, and a method for preparing methyl methacrylate through the aldol condensation reaction of methyl propionate and formaldehyde. Background technique [0002] Methyl methacrylate (MMA) is an important organic chemical raw material, mainly used to produce polymethyl methacrylate (PMMA) and acrylic resin materials, and is also widely used in the manufacture of other resins, plastics, coatings, adhesives , lubricants, sizing agents, glazing agents, printing and dyeing auxiliaries and insulating filling materials, etc. [0003] Using ethylene, methanol and carbon monoxide as raw materials to produce methyl propionate through oxo synthesis, and then reacting with formaldehyde through aldol condensation to produce methyl methacrylate is also called the Alpha process, which is environmentally friendly, Due to t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/04B01J23/10B01J23/18B01J23/22B01J23/66B01J27/182B01J35/10C07C67/343C07C69/54
Inventor 易光铨殷艳欣孙康纪勇强黎源
Owner WANHUA CHEM GRP CO LTD
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