A kind of anti-carbon aldol condensation catalyst and its preparation method and the method of using the catalyst to prepare methyl methacrylate

A condensation catalyst, carbon deposition aldol technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc. The effect of easy carbon deposition and poor stability, reduced carbon deposition rate, and reduced regeneration frequency

Active Publication Date: 2019-07-23
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the applicant found in the research that the above-mentioned alkali metal catalysts have a relatively serious carbon deposition problem in the aldol condensation reaction, resulting in a gradual decrease in catalyst activity, a single use time of the catalyst is too short and the stability is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Weigh 3.064g of Cs 2 CO 3 , 0.041g of Pt(NO 3 ) 2 and 0.016g of Nd(NO 3 ) 3 ·6H 2 Dissolve O in 30.0ml deionized water to make an impregnation solution; weigh 50.0g SiO 2 Carrier, immersed in the above solution at room temperature, after 0.5 hours of immersion, 50 ° C vacuum rotary evaporation for 1 hour, the vacuum degree is 10 4 Pa, to prepare the catalyst precursor.

[0062] Place the catalyst precursor in a quartz tube reactor, and heat it to 200°C at a rate of 5°C / min in 95% nitrogen and 5% water vapor by volume percentage; adjust the atmosphere to 95% nitrogen and 5% carbon monoxide, the catalyst was heated to 450°C at a rate of 2°C / min; the atmosphere was adjusted to 100% nitrogen, and kept at a temperature of 450°C for 5 hours; the temperature was lowered to room temperature at a rate of 10°C / min to complete the activation of the catalyst preparation.

Embodiment 2

[0064] Weigh 10.999g of CsNO 3 , 0.844g of C 4 h 6 o 4 Pd and 0.439g PrCl 3 Dissolve in a mixed solution of 20.0ml deionized water and 10ml acetone to configure as an impregnation solution; weigh 50.0g SiO 2 The carrier was immersed in the above solution at room temperature, and after immersion for 2 hours, it was evaporated to dryness in vacuum at 60°C for 2 hours, and the vacuum degree was 10 2 Pa, to prepare the catalyst precursor.

[0065] Place the catalyst precursor in a quartz tube reactor, and heat it to 250°C at a rate of 10°C / min in 95% nitrogen and 5% water vapor by volume percentage; adjust the atmosphere to 90% nitrogen and 10% carbon monoxide, the catalyst was heated to 500°C at a rate of 5°C / min; the atmosphere was adjusted to 100% nitrogen, and kept at a temperature of 500°C for 8 hours; the temperature was lowered to room temperature at a rate of 15°C / min to complete the activation of the catalyst preparation.

Embodiment 3

[0067] Weigh 7.221g of CH 3 COOCs, 0.311g of IrCl 3 and 0.380g of Nd(NO 3 ) 3 ·6H 2 Dissolve O in 30.0ml deionized water to make an impregnation solution; weigh 50.0g SiO 2 The carrier is immersed in the above solution at room temperature. After soaking for 0.1 hour, it is evacuated to dryness in vacuum at 40°C for 0.5 hour, and the vacuum degree is 10 5 Pa, to prepare the catalyst precursor.

[0068] The catalyst precursor is placed in a quartz tube reactor, heated to 100°C at a rate of 1°C / min in 100% nitrogen by volume percentage; the atmosphere is adjusted to 99% nitrogen and 1% hydrogen, and the catalyst is Heating at a rate of 1 °C / min to 400 °C; adjusting the atmosphere to 100% nitrogen, and maintaining it at a temperature of 400 °C for 2 hours; cooling to room temperature at a rate of 5 °C / min to complete the preparation of the activated catalyst.

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PUM

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Abstract

The invention discloses an anti-carbon deposition aldol condensation catalyst, which comprises an active component, an anti-carbon deposition agent, an active auxiliary agent and a carrier, and the active component is selected from one or more of inorganic salts of Cs and organic salts of Cs The anti-coking agent is selected from one or more of oxides, chlorides, nitrates, carbonates and organic acid salts of Pt, Rh, Ru, Pd, Ir, Fe, Co and Ni, and the active auxiliary The agent is selected from one or more of soluble salts of La, Ce, Nd, Pr and Pm, and the carrier is silicon dioxide. Through the controllable precursor preparation and catalyst activation process, the obtained catalyst is used to catalyze the aldol condensation reaction of methyl propionate and formaldehyde to prepare methyl methacrylate, which has high catalytic activity, good selectivity, strong anti-coking ability and Features of high stability.

Description

[0001] Technical field: [0002] The invention relates to a carbon-deposition-resistant aldol condensation catalyst and its preparation method and application. The catalyst can be used to prepare methyl methacrylate through the aldol condensation reaction of methyl propionate and formaldehyde, and specifically belongs to the technical field of catalysts. [0003] Background technique: [0004] 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. [0005] The reaction of methyl propionate and formaldehyde to prepare MMA is a typical aldol condensation reaction. At present, some domestic and foreign patent documents have reported suitable catalysts for this reaction, mainly fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/63B01J23/04C07C67/343C07C69/54
CPCB01J23/04B01J23/63C07C67/343C07C69/54
Inventor 胡进万毅易光铨于海彬李庆志韩红宇初乃波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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