Load type solid body base catalyst of synthesizing dimethyl carbonate and method of preparing the same

A solid base catalyst, dimethyl carbonate technology, applied in the preparation of organic carbonate, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of low catalytic reaction speed, low reaction temperature, reactivity to be improved, and difficulty in repeated use. and other problems, to achieve the effects of good stability, high selectivity and simple preparation

Inactive Publication Date: 2008-08-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Generally speaking, the transesterification reaction mostly uses alkali metal hydroxide, alkali metal carbonate and alkali metal alkoxide etc. Homogeneous catalyst, not suitable for separation from the product, difficult to reuse
Zhong Bing etc. (Chinese patent 01130469.3) the composite catalyst reaction activity that the phenolic resin of invention and alkaline earth metal carbonate forms is higher, and catalytic reaction speed is fast and reaction temperature is lower, and in 75ml autoclave, propylene carbonate (PC) And formaldehyde molar ratio is 1: 6, and catalyst consumption is 3%wt, and reaction temperature is 80 ℃, reacts 1 hour under stirring condition, and PC transformation rate is 52.9%, and DMC yield is 49.6%, but because this solid base has strong The basic site, the catalyst is easily destroyed by CO in the atmosphere 2 polluted
Wei Tong et al. (Chinese patent 02135213.5) used a composite catalyst formed of calcium fluoride and zirconia, which has excellent stability and can avoid CO 2 、H 2 Contaminated by impurities such as O, the reaction is in an autoclave, the molar ratio of methanol and propylene carbonate (PC) is 10:1, the catalyst consumption is 2%wt, and the reaction temperature is 150°C. After reacting for 1 hour under stirring conditions, PC is converted Yield 72.5%, DMC yield 68.9%, reactivity needs to be improved

Method used

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  • Load type solid body base catalyst of synthesizing dimethyl carbonate and method of preparing the same

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Experimental program
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Effect test

Embodiment 1

[0030] Weigh 14.17g Ca(NO 3 ) 2 4H 2 O and 11.25gAl(NO 3 ) 3 9H 2 O was dissolved in 300ml deionized water to make a mixed salt solution; weigh 5.76g NaOH and 6.36g NaOH 2 CO 3 Dissolve in 300ml deionized water to make a mixed alkali solution; pour the above two solutions into the opened fully back-mixed liquid membrane reactor at the same time, control the rotation speed of the rotor at 5000 rpm, and the reaction mixture stays in the reactor for 3 Minutes, pour the obtained slurry into a crystallization kettle, crystallize at a constant temperature of 100°C for 6 hours, then centrifuge and wash until the pH value is equal to 7, and dry the sample in an oven at 60°C for 24 hours to obtain the layered precursor Ca 2+ -Al 3+ -LDHs. The resulting layered precursor Ca 2+ -Al 3+ - LDHs were calcined in a muffle furnace at 500°C for 2 hours to obtain a particle size of 6.6nm and a specific surface area of ​​190m 2 / g catalyst support Ca 2+ -Al 3+ -(O).

[0031] (2) Pre...

Embodiment 2

[0038] (1) Preparation of catalyst carrier:

[0039] Weigh 38.46g Mg(NO 3 ) 2 ·6H 2 O and 18.78g Al(NO 3 ) 3 9H 2 O was dissolved in 130ml deionized water to make a mixed salt solution, and 12.8g NaOH and 10.6g NaOH were weighed 2 CO 3 Dissolve in 130ml of deionized water to make a mixed alkali solution; pour the above two solutions into the opened fully back-mixed liquid membrane reactor at the same time, the rotor speed is controlled at 8000 rpm, and the reaction mixture stays in the reactor for 2.0 Minutes, pour the obtained slurry into a crystallization kettle, crystallize at a constant temperature of 60°C for 6 hours, then centrifuge and wash until the pH value is equal to 7, and dry the sample in an oven at 60°C for 24 hours to obtain the layered precursor Mg 2+ -Al 3+ -LDHs. The resulting layered precursor Mg 2+ -Al 3+ -LDHs were calcined in a muffle furnace at 500°C for 2 hours to obtain a particle size of 6.2nm and a specific surface area of ​​200m 2 / g ca...

Embodiment 3

[0046] (1) Preparation of catalyst carrier:

[0047] Weigh 41.03g Mg(NO 3 ) 2 ·6H 2 O and 15.01g Al(NO 3 ) 3 9H 2 O was dissolved in 130ml deionized water to make a mixed salt solution; weigh 12.8g NaOH and 8.48g NaOH 2 CO 3 Dissolve in 130ml of deionized water to make a mixed alkali solution; pour the above two solutions into the opened fully back-mixed liquid membrane reactor at the same time, control the rotor speed at 7000 rpm, and the reaction mixture stays in the reactor for 3.0 Minutes, pour the obtained slurry into a crystallization kettle, crystallize at a constant temperature of 60°C for 6 hours, then centrifuge and wash until the pH value is equal to 7, and dry the sample in an oven at 60°C for 24 hours to obtain a layered precursor Mg 2+ -Al 3+ -LDHs. The resulting layered precursor Mg 2+ -Al 3+ - LDHs were calcined in a muffle furnace at 500°C for 2 hours to obtain a particle size of 5.6nm and a specific surface area of ​​210m 2 / g catalyst support Mg...

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Abstract

The invention relates to a carrier type solid base catalyst for synthesizing dimethyl carbonate, which belongs to the technical field of catalytic material. The catalyst's formula is KF / M<2+>-N<3+>-(O), wherein M<2+>-N<3+>-(O) represents the composite metal oxide, M<2+> can be divalent metal ion (Mg<2+> or Ca<2+> ) and N<3+> can be trivalent metal ion (Fe<3+> and / or Al<3+>). The catalyst is prepared from potassium fluoride and composite metal oxide at a certain weight ratio by immersing the potassium fluoride into the composite metal oxide, wherein the composite metal oxide is prepared from hydrotalcite precursor and in nucleation / crystallization isolation method by calcining at a certain temperature. The catalyst has the advantages of nanoscaled particle size, high specific surface area and high activity, selectivity in catalytic reaction and simple preparation, and can be reused as it can be centrifugally separated after reacting.

Description

technical field [0001] The invention belongs to the technical field of catalytic materials, and in particular provides a supported solid base catalyst for synthesizing dimethyl carbonate (DMC) and a preparation method thereof. A supported solid base catalyst for synthesizing dimethyl carbonate and a preparation method thereof. Background technique [0002] Dimethyl carbonate (DMC) has lively chemical properties, excellent physical properties, and is non-toxic and easy to biodegrade. Electrolyte, bisphenol A polycarbonate monomers and carbonylation, methylation and carbonyl methoxylation reagents are widely used in the chemical and chemical fields. At present, countries are actively researching DMC-based environmentally friendly chemical raw materials. Green chemistry process. The industrial methods for synthesizing DMC mainly include methanol oxidative carbonylation and transesterification. Among them, the transesterification method has become a method with great industri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/138B01J27/12C07C68/06C07C69/96
Inventor 张慧刘文景
Owner BEIJING UNIV OF CHEM TECH
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