Preparation for composite titanium oxide catalyst of ester interchange synthetic phenyl ester oxalate

A technology of phenyl oxalate and catalyst, which is applied in the field of preparation of composite oxide catalysts, can solve problems such as not seen, and achieve the effects of low cost, mild operating conditions, conversion rate and product selectivity

Inactive Publication Date: 2005-02-23
TIANJIN UNIV
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Problems solved by technology

But in above-mentioned all patents, relate to when using dimethyl oxalate as raw material to prepare the raw material of synthetic diphenyl carbonate by transesterification, i.e. methyl phenyl oxalate or diphenyl oxalate, although the transesterification catalyst used is constantly Update, change and improve, it can be alkali metal, cadmium, zirconium, lead, iron, copper, zinc compound or organotin compound, aluminum, titanium, vanadium organic acid compound, etc., but all are homogeneous soluble in the reaction system Catalyst, that is, all the transesterification reactions to be carried out are homogeneous reactions, so all the above-mentioned patented technologies use complex separation systems or equipment to separate the catalyst and the reaction
There is no literature on the use of composite titanium silicon oxide catalysts for the synthesis of phenyl oxalate and its preparation

Method used

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  • Preparation for composite titanium oxide catalyst of ester interchange synthetic phenyl ester oxalate

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Effect test

Embodiment 1

[0015] [Example 1] Preparation and Activity Investigation of Composite Titanium Silicon Oxide Catalyst

[0016] The present invention prepares phenol and dimethyl oxalate transesterification and synthesizes phenyl oxalate with composite titanium silicon oxide catalyst implementation investigation. Add 0.05 g of acetylacetone dropwise into an absolute ethanol solution containing 0.26 g of tetrabutyl titanate, and stir thoroughly to obtain solution A. Prepare an ethanol solution containing 20.82 g of ethyl silicate, add 5 ml of glacial acetic acid and 10 ml of deionized water, and stir thoroughly to obtain solution B. Slowly drop solution B into solution A in a nitrogen flow, stir well to obtain a miscible solution, let stand in a nitrogen flow at room temperature for 24 to 72 hours, precipitate to form a gel, and vacuum dry the gel at 60 to 80°C After 2 to 6 hours, after crushing and grinding, put it into a muffle furnace and bake at 550° C. for 5 hours to prepare a titanium-s...

Embodiment 2-5

[0019] The catalyst was changed to composite TiO 2 -SiO 2 A series of catalysts, wherein the content of titanium oxide is respectively 2.5%, 5%, 10%, 20%, under the situation that other conditions are exactly the same as in Example 1, carry out transesterification reaction, respectively form embodiment 2-5, investigate reaction result.

[0020] Table 1: TiO 2 -SiO 2 Series catalyst transesterification results (weight percentage)

[0021] Titanium Oxide Containing DMO Selectivity, % Yield, %

Embodiment

[0023] Amount, wt% Conversion % Anisole MPO DPO MPO DPO

[0024] 1 1 43.5 0.2 83.4 16.1 36.3 7.0

[0025] 2 2.5 39.7 0.4 78.2 21.4 31.1 8.5

[0026] 3 5 29.5 0.7 86.3 12.9 25.5 3.8

[0027] 4 10 27.3 0.8 85.0 14.1 23.2 3.9

[0028] 5 20 49.6 0.2 77.0 22.6 38.2 11.2

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Abstract

A composite titanium oxide-silicon oxide as the catalyst for synthesizing phenyl oxalate by ester exchange, which is used to prepare diphenyl carbonate (DPC), is prepared through preparing the precursor solutions, mixing to obtain sol, depositing, drying and calcining. It has high activity.

Description

technical field [0001] The invention relates to a composite titanium silicon oxide catalyst for synthesizing phenyl oxalate by transesterification and a preparation method thereof, in particular, it belongs to the preparation technology of the composite oxide catalyst. Background technique [0002] The preparation of methylphenyl oxalate and diphenyl oxalate from dimethyl oxalate and phenol is the key technology for all the preparation of diphenyl carbonate from dimethyl oxalate and phenol. The reaction steps experienced by this key technology are as follows: [0003] [0004] The diphenyl carbonate preparation process with this key technology as the core appeared in the 1990s, but it developed rapidly. In particular, Ube Corporation in Japan has been committed to research in this area and has applied for many patents, such as EP1013633A1, US5811573, CN1164529A, TW438765 , US5834615, EP0832872A1, US5922827, EP0832910A2, etc. But in above-mentioned all patents, relate to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J37/03C07C67/28C07C67/30C07C69/36C07C69/612
Inventor 马新宾杨霞王胜平巩金龙
Owner TIANJIN UNIV
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