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Preparation method of catalyst used for synthesizing diphenyl carbonate by ester exchange method

A technology of diphenyl carbonate and catalyst, applied in the field of preparation of heterogeneous catalysts, can solve the problems of difficult industrialization due to strong corrosiveness, low yield of diphenyl carbonate, difficult separation and recovery, etc., and achieves cheap and easy catalyst raw materials. The effect of obtaining, small active components, and low cost

Active Publication Date: 2016-02-17
SHAANXI YANCHANG PETROLEUM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the JP56-25138 document, an alkali or alkali metal compound catalyst is used, but the reaction speed of this type of catalyst is slow and a large amount of CO is produced as a by-product. 2 and anisole, low yields of diphenyl carbonate
What adopt in DE2528412 and JP51-105032 document is Lewis acid catalyst, as AlX 3 、TiX 3 、TiX 4 , VOX 3 , VX 5 、FeX 3 、SnX 4 (wherein X is halogen, acetoxy, alkoxy, aryloxy), the yield of diphenyl carbonate is slightly improved, but its strong corrosiveness brings difficulties to industrialization
Generally speaking, although the yield of diphenyl carbonate on the homogeneous catalyst is high, there are problems of separation and recovery, and environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Calcined the pure silicon MCM-41 carrier at 500°C for 2 hours, and placed it in a dry bottle for later use; weighed 4.48 g of butyl titanate and dissolved it in 100 g of ethanol, and stirred for 30 min until it was completely dissolved; then weighed 20 g of the roasted MCM- Add 41 to the ethanol solution of butyl titanate, stir for 30 minutes, then ultrasonicate the solution twice for 20 minutes intermittently, let it stand for 12 hours, vacuum filter, remove the solvent, wash the solute sample, and dry it; put the sample in the muffle furnace Roasting, using temperature programming control, heating at 3°C / min, reaching 120°C for 2 hours, then raising the temperature at 5°C / min, and roasting at 500°C for 5 hours to prepare 18.5g of 5%TiO 2 -MCM-41; Accurately weigh 1.26g of ammonium metavanadate and dissolve it in 100g of ammonia water, stir for 30min until completely dissolved, then prepare 18.5g of 5% TiO 2 - MCM-41 was added to the ammonium metavanadate solution, sti...

Embodiment 2

[0027] Calcinate the pure silicon MCM-41 carrier at 500°C for 2 hours, and place it in a dry bottle for later use; weigh 9.5g of butyl titanate and dissolve it in 100g of ethanol, and stir for 50min until it is completely dissolved; then weigh 20g of the roasted MCM- 41 was added to the ethanol solution of butyl titanate, stirred for 60 minutes, then intermittently ultrasonicated twice for 30 minutes, left to stand for 12 hours, vacuum filtered, solvent removed, washed, and dried in the air; the dried samples were roasted in a muffle furnace, Using temperature programming control, the temperature is raised at 3°C / min, and the temperature is raised to 120°C for 2 hours, then the temperature is raised at 4°C / min, and the temperature is roasted at 500°C for 5 hours, and 21g of 10%TiO is prepared. 2 -MCM-41; Accurately weigh 1.43g of ammonium metavanadate and dissolve it in 100g of ammonia water, stir for 30min until completely dissolved, then prepare 21g of 10% TiO 2 - MCM-41 was...

Embodiment 3

[0029] Calcinate the pure silicon MCM-41 carrier at 500°C for 2 hours, and place it in a dry bottle for later use; weigh 9.5g of butyl titanate and dissolve it in 100g of ethanol, and stir for 60min until it is completely dissolved; then weigh 20g of the roasted MCM-41 Add to the ethanol solution of butyl titanate, stir for 60min, then intermittently sonicate twice for 30min, let it stand for 12h, vacuum filter, remove the solvent, wash, and dry in the air; put the sample into the muffle furnace for roasting, and use the temperature program to raise the temperature Control, heat up at 3°C / min, keep the temperature at 120°C for 2h, then raise the temperature at 5°C / min, and roast at 500°C for 5h, that is, prepare 21.5g of 10%TiO2 -MCM-41; Accurately weigh 3.07g of ammonium metavanadate and dissolve it in 150g of ammonia water, stir for 50min until completely dissolved, then prepare 21.5g of 10% TiO 2 - MCM-41 was added to the ammonium metavanadate solution, stirred for 60 minute...

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PUM

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Abstract

The invention relates to a preparation method of a catalyst used for synthesizing diphenyl carbonate by an ester exchange method. The method is characterized in that a mesoporous molecular sieve MCM-41 is taken as a carrier, butyl titanate and ammonium metavanadate are taken as active components, an immersion method is employed for loading the active components, technical steps of ultrasonic processing and calcination are combined, so that the catalyst containing two active components titanium and vanadium is prepared. The catalyst has the advantages that active components are fine, distribution is uniform, the catalyst has high phenol conversion rate and ester exchange selectivity during a process for preparing diphenyl carbonate by reacting dimethyl carbonate and phenol, a phenol conversion rate can reach more than 46.0%, and no by product is generated. According to the invention, the preparation method is simple, raw materials of the catalyst have the advantages of low cost and easy acquisition, preparation cost is low, and the prepared catalyst does not generate pollution for environment and equipment.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, and relates to a preparation method of a heterogeneous catalyst used for synthesizing diphenyl carbonate by transesterification of dimethyl carbonate and phenol. Background technique [0002] Diphenyl carbonate is an important organic chemical raw material that can be used to synthesize many important organic compounds and polymer materials, especially polycarbonate that can replace highly toxic phosgene and bisphenol A to produce excellent performance. [0003] The currently known synthetic methods of diphenyl carbonate include phosgene method, transesterification method and phenol oxidative carbonylation method. Because phosgene is highly toxic and seriously pollutes the environment, the phosgene method has been basically eliminated; the oxidative carbonylation of phenol has not been industrialized because of the high price of the catalyst; and the transesterificat...

Claims

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Application Information

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IPC IPC(8): B01J29/04C07C69/96C07C68/06
Inventor 张金峰沈寒晰张存社史李刚卢美旭张丽娜
Owner SHAANXI YANCHANG PETROLEUM GRP
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