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Supported catalyst for diphenyl carbonate synthesis by reaction of phenylacetate and dimethyl carbonate and preparation method thereof

A technology of supported catalyst and dimethyl carbonate, which is applied in the field of supported catalyst and its preparation, can solve the problems of poor catalyst stability, difficult separation of reactants, unstable catalyst, etc., and achieve stable performance, safe and simple operation, pressure and The effect of low temperature

Active Publication Date: 2012-11-14
江苏丹化煤制化学品工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101628874 reported that the β-diketone compounds of Group IV metals were used as catalysts, and the catalysts had good selectivity, stability and catalytic activity, but the preparation was complicated and the price was relatively expensive
US5349102, US5276134, US4182726, CN101768082 reported that organotitanium and organotin are used as catalysts, which also have good catalytic effects, but the catalysts are less stable, easy to absorb moisture and hydrolyze in the air, and have unstable performance, which is limited in industrial applications
CN101774911 reported that the oxides of VIB group elements Mo and W were used as catalysts to solve the instability problem of catalysts. At the same time, the preparation method of catalysts is simple, the raw materials are easy to get, no pollution to the environment, no corrosion to equipment, and easy to recycle, but the catalysts are easy to Deactivation, poor catalytic activity, low selectivity, difficult separation of reactants, high energy consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Heteropoly acid H 6 [V 2 Mo 18 o 62 ] ?XH 2 Preparation of O: Dilute 10g Na 2 MoO 4 2H 2 O was dissolved in 45ml of water, and 0.54g of NH was added 4 VO 3 , stirred until completely dissolved, then added 8ml of concentrated HCl, and refluxed for 8h. Add 10gNH after cooling 4 Cl, and suction filtered after the solid precipitated out. Weigh the obtained solid, dissolve it in deionized water twice the mass of the solid, extract it with diethyl ether (analytical grade), add concentrated HCl drop by drop until the amount of the ether compound in the bottom layer no longer increases, and separate the ether compound , dried under vacuum, and finally recrystallized in a sulfuric acid solution with a concentration of 0.5% by mass to obtain crystals, which were dried to obtain H 6 [V 2 Mo 18 o 62 ].

[0021] Catalyst preparation: first pretreat the molecular sieve carrier SBA-15, and roast the molecular sieve SBA-15 at 500°C for 4 hours; 28.28g of H 6 [V 2 Mo 1...

Embodiment 2

[0024] h 8 [P 2 Mo 16 V 2 o 62 ]?XH 2 Preparation of O: under magnetic stirring and pH meter monitoring, in 100mL sodium molybdate solution (0.16mol), add 25mL sodium dihydrogen phosphate solution (0.02mol), dropwise add 1:1 sulfuric acid (concentrated sulfuric acid and deionized water Sulfuric acid solution with a volume ratio of 1:1) to adjust pH=4, then add 100mL ammonium metavanadate solution (0.02mol), add 1:1 sulfuric acid dropwise to adjust pH=3.80, and reflux for 8h. After cooling, it was transferred into a separatory funnel, and 150 mL of ether was added. Add a small amount of 1:1 sulfuric acid in small amounts, oscillate, separate layers after standing, separate the red oily substance in the lower layer and place it in a vacuum desiccator to remove ether to obtain a solid, recrystallize with deionized water to obtain crystals, and dry to obtain H 8 [P 2 Mo 16 V 2 o 62 ].

[0025] Catalyst preparation: first pretreat the molecular sieve carrier MCM-41, and ...

Embodiment 3

[0028] h 8 [P 2 Mo 17 V 1 o 62 ]?XH 2 Preparation of O: under magnetic stirring and pH meter monitoring, in 75mL sodium molybdate solution (0.17mol), add 25mL sodium dihydrogen phosphate solution (0.02mol), add dropwise 1:1 sulfuric acid (concentrated sulfuric acid and deionized water Sulfuric acid solution with a volume ratio of 1:1) to adjust pH=4, then add 100mL ammonium metavanadate solution (0.01mol), add 1:1 sulfuric acid dropwise to adjust pH=3.60, and reflux for 8h. After cooling, it was transferred into a separatory funnel, and 150 mL of ether was added. Add a small amount of 1:1 sulfuric acid in small amounts, oscillate, separate layers after standing, separate the red oily substance in the lower layer and place it in a vacuum desiccator to remove ether to obtain a solid, recrystallize with deionized water to obtain crystals, and dry to obtain H 8 [P 2 Mo 17 V 1 o 62 ].

[0029] Catalyst preparation: first pretreat the molecular sieve carrier natural morde...

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PUM

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Abstract

The invention discloses a supported catalyst for diphenyl carbonate synthesis by reaction of phenylacetate and dimethyl carbonate and a preparation method thereof. The active components of the catalyst are molybdenum oxide and vanadium oxide, wherein the carrier of the catalyst is a molecular sieve, the charge capacity of the carrier is between 12.5 and 75 percent, and the ratio scope of the amounts of the molybdenum oxide and the vanadium oxide is (2.6:1)-(17:1). The catalyst has the characteristics of high catalytic activity, high selectivity, long service life and the like, and has high industrial application value.

Description

technical field [0001] The invention relates to a supported catalyst for synthesizing diphenyl carbonate by reacting phenyl acetate and dimethyl carbonate and a preparation method thereof, belonging to the technical field of catalyst preparation. Background technique [0002] Diphenyl carbonate is the main raw material for the synthesis of polycarbonate. Polycarbonate has excellent properties such as transparency, high impact strength, and flame retardancy. Its performance ranks first among the six general-purpose engineering plastics, and it is mainly used for advanced insulation. , electronic appliances, mechanical parts, construction, optics and other materials, its consumption in engineering plastics is second only to polyamide. At present, the annual demand for polycarbonate in the world is 4-5 million tons, and it is expected that the demand will still maintain a growth rate of 7-10%. There are only a small amount of phosgene products in my country, and polycarbonate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03B01J29/78B01J29/26B01J29/48C07C69/96C07C68/06
Inventor 吴晓金于克生吴维果许叶飞
Owner 江苏丹化煤制化学品工程技术有限公司
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