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Repeatedly used catalyst for synthesizing dimethyl carbonate

A dimethyl carbonate and catalyst technology, which is applied in the field of flower-like micro-nano structure catalysts for the synthesis of dimethyl carbonate, can solve the problems of reduced catalytic activity, complex catalyst components, and easy loss of catalysts after repeated use, so as to achieve easy expansion and application , the effect of high catalytic efficiency

Inactive Publication Date: 2010-09-15
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in previous reports, the catalyst components are relatively complex, and there are some challenges in the preparation process of the catalyst, and the catalyst is easily lost during repeated use, resulting in a decrease in catalytic activity.

Method used

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  • Repeatedly used catalyst for synthesizing dimethyl carbonate
  • Repeatedly used catalyst for synthesizing dimethyl carbonate
  • Repeatedly used catalyst for synthesizing dimethyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The ethylene glycol precursor of 0.05g flower-shaped micro-nano structure magnesium oxide is dispersed in the mixed solution of 100mL ethanol and water (ethanol: water=10:1, V / V), then add 0.05g CTAB and 0.18g ammoniacal liquor ( 28%, wt%), after being completely dissolved, add 0.05g tetraethyl orthosilicate, stir for 3 hours to stop the reaction, the product is dried at 50°C after centrifugation, and then roasted at 550°C for 10 hours to obtain a white powdery solid, which is Catalyst for the synthesis of dimethyl carbonate. This white powder is confirmed to be magnesium oxide crystal through X-ray diffraction pattern (see image 3 ), the results of transmission electron microscopy showed that the surface of magnesium oxide with flower-like micro-nano structure was covered with silicon dioxide (see Figure 4 ).

[0033] Get 60 mg of the catalyst and add it to a 25 mL round-bottomed flask, add 4 mL of a mixed solution of ethylene carbonate (or propylene carbonate) and...

Embodiment 2

[0036] 1.0g flower-like micro-nano structure magnesium oxide is dispersed in the mixed solution of 100mL ethanol and water (ethanol: water=1: 10, V / V), then add 0g CTAB and 0.5g ammoniacal liquor (28%, wt%), After complete dissolution, add 0.5 g of methyl orthosilicate and stir for 24 hours to stop the reaction. The product is centrifuged, dried at 80°C, and then calcined at 350°C for 10 hours to obtain a white powdery solid.

[0037] Get 60 mg of the catalyst and add it to a 25 mL round-bottomed flask, add 4 mL of a mixed solution of ethylene carbonate (or propylene carbonate) and methanol (ester: alcohol = 8: 1, mol / mol), react for 6 hours under stirring at 140 ° C, take the bottle The internal products were analyzed by gas chromatography, and the calculation results are shown in Table 1.

[0038] After the catalyst was centrifuged, it was washed three times with methanol and then re-added to carry out the above reaction. After repeating this for 9 times, the product after t...

Embodiment 3

[0040]The ethylene glycol precursor of 0.4g flower-like micro-nano structure magnesium oxide is dispersed in the mixed solution of 100mL ethanol and water (ethanol: water=2: 3, V / V), then add 0.2g CTAB and 0.5g ammoniacal liquor ( 28%, wt%), after completely dissolving, add 0.4g propyl orthosilicate, stir for 3 hours to stop the reaction, the product is dried at 80°C after centrifugation, and then roasted at 550°C for 10 hours to obtain a white powdery solid.

[0041] Get 60 mg of the catalyst and add it to a 25 mL round-bottomed flask, add 4 mL of a mixed solution of ethylene carbonate (or propylene carbonate) and methanol (ester: alcohol = 8: 1, mol / mol), react for 6 hours under stirring at 140 ° C, take the bottle The internal products were analyzed by gas chromatography, and the calculation results are shown in Table 1.

[0042] After the catalyst was centrifuged, it was washed three times with methanol and then re-added to carry out the above reaction. After repeating thi...

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Abstract

The invention discloses a catalyst for synthesizing dimethyl carbonate and a preparation method thereof. The catalyst is prepared by the following steps of: 1) dispersing alkaline-earth metal oxides with flower-shaped micro-nano-structures or glycol precursor thereof in a mixed solvent of water and ethanol, adding ammonia water into the mixed solvent, and then adding silicate ester into the mixedsolvent to obtain a mixed system; 2) reacting the mixed system at the temperature of between 10 and 80 DEG C for 0.5 to 24 hours, and centrifugally collecting a solid product after the reaction is finished; and 3) drying the solid product at the temperature of between 50 and 200 DEG C, and roasting at the temperature of between 350 and 800 DEG C for 1 to 15 hours to obtain the catalyst. The catalyst has high catalytic efficiency. During catalyzing methanol and ethylene carbonate or propylene carbonate to perform ester exchange reaction, the conversion rate of the ethylene carbonate or propylene carbonate is over 90 percent and the selectivity of the product dimethyl carbonate is over 95 percent. The catalyst is easy to extend and apply, and maintains the catalytic activity after being repeatedly used for more than 10 times.

Description

technical field [0001] The invention belongs to the field of solid base catalysts, in particular to a reusable flower-shaped micro-nano structure catalyst for synthesizing dimethyl carbonate. Background technique [0002] Dimethyl carbonate (DMC) is an environmentally friendly organic intermediate and gasoline additive, but also a good polar aprotic solvent. Its synthesis and application have received extensive attention in recent years. The industrial methods for synthesizing dimethyl carbonate mainly include phosgene method, methanol oxidation carbonyl carbon method and transesterification method. Synthesis of DMC by transesterification of ethylene carbonate or propylene carbonate and methanol is a promising method because of the simple process, mild reaction conditions and the ability to generate diols. [0003] Commonly used catalysts for the synthesis of DMC by transesterification include homogeneous catalysts such as alkali metal alkoxides and heterogeneous catalysts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/14C07C69/96C07C68/06
Inventor 宋卫国崔志民江雷
Owner INST OF CHEM CHINESE ACAD OF SCI
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