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Solid base catalyst for synthesizing dimethyl carbonate, its preparing process and use thereof

A technology of solid base catalyst and dimethyl carbonate, which is applied in the direction of organic carbonate preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of catalyst active component loss, catalyst activity decline, etc., and achieve easy separation , the rate of inactivation is reduced, and the effect of excellent stability

Inactive Publication Date: 2006-08-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At a reaction temperature of 64°C, the PC feed space velocity is 0.3h -1 , when the reflux ratio was 6:1, after 12 hours of reaction, the conversion rate of PC reached 97.4%, but after 20 hours of reaction, the catalyst activity gradually decreased, which may be caused by the loss of active components of the catalyst during the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Prepare 0.1M ZrOCl separately 2 solution, 0.1M KF solution, 0.1MCaCl 2 solution and 20% (volume content) ammonia solution; under continuous heating and stirring, the ZrOCl 2 The solution and ammonia water were added dropwise into the beaker at the same time, the temperature was controlled at 30°C, and the pH value of the precipitate was 10. After the precipitation is complete, CaCl 2 And KF solution and drip into the beaker, aged for 2 hours, washed repeatedly until no Cl -1 Detection; the washed precipitate was baked at 105°C for 12 hours, and then baked in a muffle furnace at 500°C for 4 hours to obtain a catalyst. CaF in the catalyst 2 The content is 15wt%, zirconia 85.0wt%.

[0022] The catalyst is crushed into 2-1.2mm (10-20 mesh) and applied to the catalytic rectification device. Under normal pressure, the temperature of the reaction section is controlled by an external heat source to be 120°C, the temperature of the bottom of the tank is 110°C, the temperat...

Embodiment 2

[0024] CaF in the catalyst 2 The content is 20% (wt). Prepare 0.15M ZrOCl separately 2 solution, 0.15MKF solution, 0.15MCaCl 2 solution and 30% (volume content) ammonia solution; under continuous heating and stirring, the ZrOCl 2 The solution and ammonia water were added dropwise into the beaker at the same time, the temperature was controlled at 40°C, and the pH value of the precipitate was 10. After the precipitation is complete, CaCl 2 And KF solution and drip into the beaker, aged for 2 hours, washed repeatedly until no Cl -1 Detection; the washed precipitate was baked at 110°C for 12 hours, and then baked in a muffle furnace at 600°C for 4 hours to obtain a catalyst. CaF in the catalyst 2 The content is 20wt%, zirconia 80wt%.

[0025] The catalyst is crushed into 2-1.2mm (10-20 mesh) and applied to the catalytic rectification device. Under normal pressure, the temperature of the reaction section is controlled by an external heating source to be 140°C, the temperat...

Embodiment 3

[0027] Prepare 0.15M ZrOCl separately 2 solution, 0.15M KF solution, 0.15MCaCl 2 solution and 30% (volume content) ammonia solution; under continuous heating and stirring, 0.15M ZrOCl 2 The solution and ammonia water were added dropwise into the beaker at the same time, the temperature was controlled at 40°C, and the pH of the precipitate was 11. After the precipitation is complete, CaCl 2 And KF solution and drip into the beaker, aged for 2 hours, washed repeatedly until no Cl -1 Detection; the washed precipitate was baked at 110°C for 12 hours, and then baked in a muffle furnace at 600°C for 4 hours to obtain a catalyst. CaF in the catalyst 2 The content is 25wt%, zirconia 75wt%.

[0028] The catalyst is crushed into 2-1.2mm (10-20 mesh) and applied to the catalytic rectification device. Under normal pressure, the temperature of the reaction section is controlled by an external heat source to 100°C, the temperature of the bottom of the tank is 120°C, the temperature of...

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PUM

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Abstract

The invention is a kind of solid alkali catalyst for synthesizing dimethyl ester carbonate whose weight percentage components are: calcium fluoride 15%-30%, zirconium oxide 70%-85%. The ZrOCl2 liquid and ammonia are dropped into the reactor to be deposited, after being deposited; they are dried, baked and produced into catalyst. The invention has excellent stability, the speed of activity losing is decreased greatly, avoids the default of normal solid easy to be contaminated by CO2, H2O. The product can be used repeatedly.

Description

technical field [0001] The invention belongs to a solid base catalyst for synthesizing dimethyl carbonate, in particular to a solid base catalyst for synthesizing dimethyl carbonate from propylene carbonate or ethylene carbonate, as well as its preparation and application. technical background [0002] Dimethyl carbonate (DMC), as a new environment-friendly chemical reagent, has attracted extensive attention at home and abroad in recent years for its synthesis and application due to its unique physical and chemical properties. The industrial methods for synthesizing dimethyl carbonate mainly include methanol oxidative carbonylation and transesterification. Among them, the transesterification method has become a method with great industrial application prospects due to mild reaction conditions, high yield and co-production of ethylene glycol or propylene glycol. The catalysts used in the synthesis of dimethyl carbonate by transesterification are mainly homogeneous metal orga...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/138B01J27/135B01J21/06C07C68/06C07C69/96
Inventor 孙予罕魏伟王慧王秀芝赵宁
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI