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Preparation method and application of catalyst for synthesizing dimethyl carbonate

A technology of dimethyl carbonate and catalyst, applied in the field of catalytic synthesis of dimethyl carbonate, can solve the problems of large amount of catalyst and difficulty in recycling and reuse, and achieve the effects of small amount of catalyst, excellent thermal stability and simple preparation

Active Publication Date: 2014-04-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

R. Srivastava used 0.25g Fe-Zn double metal cyanide complex to catalyze the transesterification reaction of 10mmol propylene carbonate and 100mmol methanol, and reacted at 170°C for 8h, and the yield of >86% of dimethyl carbonate and 100% of dimethyl carbonate could be obtained. Dimethyl carbonate selectivity (Journal of Catalysis 2006, 241:34–44), but the significant disadvantage is the large amount of catalyst
At the same time, due to the thermal instability of Fe-Zn double metal cyanide complex, it is difficult to recycle and reuse it.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 0.6g potassium hexacyanocobaltate K 3 [Co(CN) 6 ] was dissolved in 50mL deionized water, and 6.0g of water-soluble triblock copolymer EO of ethylene oxide and propylene oxide was added 20 PO 70 EO 20 , stirred until completely dissolved, then added dropwise until 2.0 g of ZnCl was dissolved 2In 10ml of aqueous solution, the reaction was stirred at 75°C for 2 hours, and then filtered to isolate a solid. Redisperse the obtained solid in 50ml of deionized water, add 10ml of an aqueous solution in which 2.0g of sodium hydroxide was dissolved, stir and react for 12 hours, filter, wash repeatedly with deionized water to obtain a solid filter cake, vacuum dry at 80°C, and ball mill , and then calcined at 250° C. for 5 hours, and cooled to room temperature under nitrogen to prepare the catalyst.

Embodiment 2

[0029] 10.0g Potassium Bromopentacyanocobaltate K 3 [Co(CN) 5 Br] was dissolved in 50mL of deionized water, added 18ml of tert-butanol t-BuOH, stirred until completely transparent and dissolved, and then added dropwise until 50.0g of ZnCl was dissolved 2 In 20ml of aqueous solution, the reaction was stirred at 90°C for 8 hours, and then filtered to isolate a solid. The resulting solid was redispersed in 50ml of water, 40ml of an aqueous solution in which 8.0g of potassium hydroxide was dissolved was added, stirred and reacted for 16 hours, filtered, washed repeatedly with deionized water to obtain a solid filter cake, vacuum-dried at 100°C, ball milled, and then Calcined at 150°C for 7 hours and cooled to room temperature under nitrogen to prepare the catalyst.

Embodiment 3

[0031] 1.5g potassium pentacyanocobaltate azide K 3 [Co(CN) 5 N 3 ] was dissolved in 50mL deionized water, added 10ml glycerin, stirred until completely transparent and dissolved, then added dropwise until 10.0g ZnCl was dissolved 2 In 10ml of aqueous solution, the reaction was stirred at 45°C for 24 hours, and then filtered to isolate a solid. The resulting solid was redispersed in 50ml of water, 10ml of aqueous solution in which 3.0g of ammonia water was dissolved was added, stirred and reacted for 24 hours, filtered, washed repeatedly with deionized water to obtain a solid filter cake, dried in vacuum at 120°C, ball milled, and then heated at 220 The catalyst was prepared by roasting at ℃ for 5 hours and cooling to room temperature under nitrogen.

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Abstract

The invention relates to the field of environment-friendly organic synthesis, and aims to provide a preparation method and application of a catalyst for synthesizing dimethyl carbonate. The method comprises the following steps of: dissolving polycyano cobalt metal salt in de-ionized water, adding alcohol or water-soluble polymer and stirring until the materials are fully dissolved; dropwise adding zinc halide aqueous solution into the mixed solution, stirring, filtering and separating to obtain solid; dispersing the solid in water again; adding ammonia water or aqueous solution of alkali metal hydroxide, stirring to react, filtering and repeatedly washing to obtain solid filter cake; drying under vacuum; ball-milling; rebaking; and cooling to room temperature under a nitrogen condition to prepare a product. The catalyst provided by the invention has the advantages of simplicity in preparation, single composition, no need of extra addition of a large amount of carrier or auxiliary agent, less using amount of the catalyst in reaction, mild reaction conditions, high catalytic activity and selectivity of reaching 100 percent, suitability for industrial production, yield of the dimethyl carbonate of reaching over 50 percent, superior thermal stability and capability of being recycled.

Description

technical field [0001] The invention belongs to the field of green organic synthesis, and in particular relates to a method for catalytically synthesizing dimethyl carbonate. Background technique [0002] Dimethyl carbonate (DMC) is an important organic raw material. Because it is environmentally friendly, non-toxic and harmless, it is generally used as a carbonylation and methylation reagent in organic synthesis to replace toxic phosgene and sulfuric acid disulfide. Methyl esters are widely used in pharmaceutical, agricultural and other fields. At the same time, it can also be used as a gasoline additive to increase the octane number and oxygen content of gasoline. [0003] At present, there are four main methods for preparing DMC: phosgene method, methanol oxidative carbonylation method, methanol, carbon dioxide one-step synthesis method and transesterification method. Due to the use of toxic phosgene or carbon monoxide as the reaction monomer, the former two methods are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C69/96C07C68/06
Inventor 张兴宏魏人建杜滨阳戚国荣
Owner ZHEJIANG UNIV
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