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Preparation of loaded molybdenum oxide catalyst for synthesis of phenyloxalate by ester interchange process

A technology of phenyl oxalate and catalyst, which is applied in the field of supported molybdenum oxide catalyst and its preparation, can solve the problems such as the catalyst preparation method not mentioned, and achieve the goal of saving separation process and equipment, reducing production cost and energy consumption Effect

Active Publication Date: 2005-02-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 applicant mentioned in the 200410018842.6 patent that the molybdenum trioxide catalyst is used to synthesize phenyl oxalate, which has the advantages of high yield and good selectivity, but does not mention the preparation method of the catalyst

Method used

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  • Preparation of loaded molybdenum oxide catalyst for synthesis of phenyloxalate by ester interchange process
  • Preparation of loaded molybdenum oxide catalyst for synthesis of phenyloxalate by ester interchange process

Examples

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Embodiment 1

[0021] The present invention is the implementation and investigation of molybdenum oxide supported catalyst for the preparation of phenol and dimethyl oxalate transesterification method for synthesizing phenyl oxalate by slurry impregnation method. Grind molybdenum trioxide into 200-mesh fine particles, dry in a drying oven at 120°C, and set aside. Weigh 1.278g of dried molybdenum trioxide and add 70ml of deionized water to form a mixed solution. Weigh 20 g of 80-mesh activated carbon carrier particles, place them in a rotary evaporator, and impregnate them with an impregnation solution at 95° C. for 8 hours. The impregnated catalyst was dried at a drying temperature of 120° C. for 6 hours; taken out to obtain a molybdenum oxide-supported catalyst with a molybdenum loading of 4 wt%.

[0022] Catalyst that the present invention makes is under heterogeneous catalyzed reaction condition with dimethyl oxalate and phenol as raw material to prepare methyl phenyl oxalate and dipheny...

Embodiment 2-4

[0024] Changing the Supported Molybdenum Trioxide Catalyst MoO 3 The load of molybdenum in / C is respectively 8%, 16%, 32%, and under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, form embodiment 2-4 respectively, investigate reaction result.

[0025] Table 1: MoO 3 / C series catalyst preparation method and catalytic transesterification reaction results (weight percentage)

[0026] Molybdenum trioxide Deionization Impregnation Impregnation Drying

[0027] Molybdenum loaded DMO yield, %

[0028] Example Mass Water Volume Temperature Time Temperature

[0029] Amount, % Conversion %

[0030] g ml ℃ h ℃ MPO DPO

[0031] 1 4 1.28 70 90 8 120 49.5 40.6 8.7

[0032] 2 8 2.73 80 90 12 120 59.0 48.0 10.8

[0033] 3 16 6.32 90 95 24 120 64.3 54.2 9.7

[0034] 4 32 18.48 110 95 36 120 56.8 47.2 7.4

Embodiment 5-7

[0036] Switch to SiO2 2 Support, prepared MoO by slurry impregnation method 3 / SiO 2 Series of catalysts, supported molybdenum trioxide catalyst MoO 3 / SiO 2 The loads of molybdenum in the medium were 4%, 8%, and 16% respectively. Under the same conditions as in Example 1, the transesterification reaction was carried out to form Examples 5-7 respectively, and the reaction results were investigated.

[0037] Table 2: MoO 3 / SiO 2 Series catalyst preparation method and catalytic transesterification reaction results (weight percentage)

[0038] Molybdenum trioxide Deionization Impregnation Impregnation Drying

[0039] Molybdenum loaded DMO yield, %

[0040] Example Mass Water Volume Temperature Time Temperature

[0041] Amount, % Conversion %

[0042]g ml ℃ h ℃ MPO DPO

[0043] 5 4 1.28 80 80 12 140 46.1 38.1 6.8

[0044] 6 8 2.73 100 90 24 140 57.8 47.3 10.3

[0045] 7 16 6.32 120 95 36 140 54.6 46.0 8.2

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Abstract

A carried MoO3 catalyst for synthesizing phenyl oxalate by ester exchange reaction between phenol and dimethyl oxalate is prepared through preparing MoO3 slurry, grinding carrier, mixing them together, immersing and drying.

Description

technical field [0001] The invention relates to a supported molybdenum oxide catalyst for synthesizing phenyl oxalate by a transesterification method and a preparation method thereof, and relates to the transesterification synthesis of phenol and dimethyl oxalate as a raw material methyl phenyl oxalate for the production of diphenyl carbonate (DPC) Catalyst of acid ester and diphenyl oxalate and preparation method thereof. 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] or [0005] [0006] 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 ha...

Claims

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Application Information

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IPC IPC(8): B01J23/28B01J37/02C07C67/28C07C67/30C07C69/36C07C69/612
Inventor 马新宾巩金龙王胜平杨霞
Owner TIANJIN UNIV
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