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Preparing method for loaded titania catalyst of ester interchange synthetic phenyl ester oxalate

A technology of titanium dioxide and phenyl oxalate, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as catalyst preparation methods not mentioned, and save separation process and equipment, transformation The efficiency and selectivity of products are improved, and the effect of no pollution to the environment

Active 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
The inventor mentioned in the 02129212.4 patent that phenyl oxalate was catalyzed by a titanium dioxide catalyst, which has the advantages of good selectivity and high yield, but did not mention the preparation method of the catalyst

Method used

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  • Preparing method for loaded titania catalyst of ester interchange synthetic phenyl ester oxalate

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Experimental program
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Embodiment 1

[0018] [Example 1] Preparation and Activity Investigation of Supported Titanium Oxide Catalyst

[0019] The present invention prepares phenol and dimethyl oxalate transesterification and synthesizes phenyl oxalate with supported titanium oxide catalyst implementation investigation. Dry the silica gel carrier particles in a drying oven at 120° C. for later use. Weigh 0.86 g of tetrabutyl titanate and dissolve it in 80 ml of absolute ethanol, stir in nitrogen flow at room temperature for 0.5 h, put 20 g of pretreated silica gel carrier with a particle size of 80 Å, stir well for 2 h, slowly drop Add an ethanol solution containing 0.4 g of deionized water. Put the fully stirred mixture at room temperature for 24-72 hours in a nitrogen stream to obtain a solid powder, dry the solid at 60-200°C for 5 hours, then put it into a muffle furnace and bake it at 550°C for 5 hours , that is, a supported titania catalyst with a titania loading of 1 wt % was prepared.

[0020] In the pres...

Embodiment 2-8

[0022] Changing the Supported Metal Oxide Catalyst TiO 2 / SiO 2 The loaded amount of titanium oxide in the middle is respectively 4%, 8%, 10%, 12%, 14%, 16%, 18%, and under the situation that other conditions are identical with embodiment 1, carry out transesterification reaction, form respectively Embodiment 2-8, investigate reaction result.

[0023] Table 1: TiO 2 / SiO 2 Series of catalysts catalyzed transesterification reaction results (weight percentage)

[0024] Titanium oxide supported DMO selectivity, % yield, %

Embodiment

[0026] Amount, % Conversion % Anisole MPO DPO MPO DPO

[0027] 1 1 45.9 0.6 79.0 19.7 36.3 9.0

[0028] 2 4 46.5 0.8 77.4 21.5 36.0 10.0

[0029] 3 8 52.5 0.9 75.7 23.0 39.7 12.1

[0030] 4 10 62.3 0.9 73.6 23.9 45.9 14.9

[0031] 5 12 66.3 0.4 71.9 27.3 47.7 18.1

[0032] 6 14 63.9 0.4 73.1 26.2 46.7 16.7

[0033] 7 16 60.3 0.6 76.7 22.4 46.3 13.5

[0034] 8 18 53.8 0.4 76.2 22.9 41.0 12.3

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Abstract

A carried TiO2 catalyst used for synthesizing the phenyl oxalate used to prepare diphenyl carbonate (DPC) by ester exchange is prepared through preparing the dipping liquid, pretreating carrier, mixing it with said dipping liquid, hydrolyzing, drying and calcining. It has high activity and no pollution.

Description

technical field [0001] The present invention relates to a kind of supported titanium dioxide catalyst and preparation method thereof for synthesizing phenyl oxalate by transesterification, specifically, relate to dimethyl oxalate (DMO) and phenol transesterification synthesis production diphenyl carbonate (DPC ) The preparation method of the raw material methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO) 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, su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J37/02C07C67/28C07C67/30C07C69/36C07C69/612
Inventor 马新宾杨霞王胜平巩金龙
Owner TIANJIN UNIV
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