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Catalyzing method of synthesizing diphenyl carbonate through ester exchange reaction

A technology for diphenyl carbonate and transesterification, which is applied in the preparation of organic carbonates, chemical instruments and methods, catalysts for physical/chemical processes, etc. Good stability, good economic and social benefits, and the effect of not corroding equipment

Inactive Publication Date: 2010-07-14
CHANGZHOU INST OF CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems of difficult catalyst separation and recovery, high price, and unstable performance in the prior art, the present invention provides a heterogeneous catalyst system with industrial application prospects, that is, the oxidation of the prepared VIB elements Mo and W It is used as a catalyst for the synthesis of diphenyl carbonate by transesterification heterogeneous catalytic method using phenyl acetate (PA) and dimethyl carbonate (DMC) as raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. Weigh 40.0 g of ammonium dimolybdate and roast in a muffle furnace at 600°C for 6 hours to prepare the catalyst, cool to room temperature, take it out and put it in a desiccator for later use. The prepared catalyst sample was characterized by XRD, and it was found that the sample was pure molybdenum trioxide.

[0022] 2. Weigh 110.0 grams of phenyl acetate (about 0.80 mol), 12.0 grams of dimethyl carbonate (about 0.13 mol) and 7.0 grams of prepared molybdenum trioxide (about 0.049 mol) catalyst and add it to a 250 ml high-pressure The reaction kettle was sealed with fasteners, and after confirming the airtightness of the high-pressure sealed reaction kettle with nitrogen, it was heated under normal pressure to keep the reaction temperature at 190°C, and the reaction was completed after stirring for 4 hours, and the heating was stopped.

[0023] 3. Stir and cool down to room temperature naturally, open the reaction kettle, discharge the liquid material in the kettle, ...

Embodiment 2

[0025] 1. Weigh 30.0 grams of sodium molybdate and dissolve it in water to form a solution. Slowly add sodium molybdate solution with nitric acid as a precipitant to control the pH value of the system to 7-8. After aging, filtering and washing the obtained precipitate, place it at 100°C After drying in an oven, the catalyst was prepared by roasting at 600° C. for 5 hours, cooled to room temperature, taken out and put into a desiccator for later use. The prepared catalyst sample was characterized by XRD, and it was found that the sample was pure molybdenum trioxide.

[0026] 2. Weigh 110.0 grams of phenyl acetate (about 0.80 mol), 12.0 grams of dimethyl carbonate (about 0.13 mol) and 8.0 grams of prepared molybdenum trioxide (about 0.056 mol) catalyst and add it to a 250 ml high pressure The reaction kettle was sealed with fasteners, and after confirming the airtightness of the high-pressure sealed reaction kettle with nitrogen, it was heated under normal pressure to keep the r...

Embodiment 3

[0029] 1. Weigh 20.0 grams of metallic molybdenum powder and mix it with 30% hydrogen peroxide solution to produce a yellow gel precursor. After the yellow precursor was dried in an oven at 100°C, it was calcined at 600°C for 5 hours to prepare a catalyst, cooled to room temperature, taken out and placed in a desiccator for later use. The prepared catalyst sample was characterized by XRD, and it was found that the sample was pure molybdenum trioxide.

[0030]2. Weigh 110.0 grams of phenyl acetate (about 0.80 mol), 36.0 grams of dimethyl carbonate (about 0.40 mol) and 9.5 grams of prepared molybdenum trioxide (about 0.066 mol) catalyst and add it to a 250 ml high-pressure The reaction kettle was sealed with fasteners, and after confirming the airtightness of the high-pressure sealed reaction kettle with nitrogen, it was heated under normal pressure to keep the reaction temperature at 180°C, and the reaction was completed after stirring for 6 hours, and the heating was stopped. ...

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PUM

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Abstract

The invention discloses a multi-phase catalyzing method of synthesizing diphenyl carbonate (DPC) through ester exchange reaction by using phenyl acetate (PA) and dimethyl carbonate (DMC) as raw materials. A catalyst used in the reaction is an oxide of VIB group elements Mo and W, the catalysis reaction temperature is between 150 and 200 DEG C, and the reaction time is between 4 and 8 hours. The invention has the advantages of simple preparation method of the catalyst, easy acquisition of raw materials, no environment pollution and no corrosion on equipment, the used catalyst can be easily separated, recovered, regenerated and used repeatedly, the consumption of the catalyst in the catalysis reaction is little, the total selectivity on products of methyl phenyl carbonate (MPC) and diphenyl carbonate (DPC) can reach more than 95 percent, and the conversion rate of the diphenyl carbonate (DPC) is about 75 percent, so the catalyst system can be widely used for producing the diphenyl carbonate (DPC).

Description

technical field [0001] The invention discloses a catalytic method for synthesizing diphenyl carbonate by transesterification reaction, especially a heterogeneous method for synthesizing diphenyl carbonate by transesterification reaction using phenyl acetate (PA) and dimethyl carbonate (DMC) as raw materials A catalytic method belongs to the field of applied catalysis. Background technique [0002] Diphenyl carbonate (DPC) is non-toxic and non-polluting. It is an important "green" chemical product that can be used to synthesize many important organic compounds and polymer materials, especially to replace highly toxic phosgene and bisphenol A. Produces polycarbonate with excellent properties. [0003] The synthesis methods of diphenyl carbonate mainly include phosgene method, phenol oxidative carbonylation method and transesterification method. Because phosgene is highly toxic and will cause serious environmental pollution, the traditional phosgene method is being phased out...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96B01J23/24
CPCY02P20/584
Inventor 王公应曹平杨先贵唐聪明王越姚洁雷永诚康涛
Owner CHANGZHOU INST OF CHEM
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