Preparation method of methyl phenyl oxalate and phenostal
A technology of methyl phenyl oxalate and diphenyl oxalate, which is applied in the field of raw materials for the preparation of diphenyl carbonate, to achieve the effects of improving selectivity, saving separation processes and equipment, and reducing production costs
Inactive Publication Date: 2003-04-23
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 organic tin compound, aluminum, titanium, vanadium organic acid compound, etc., but all are homogeneous catalysts soluble in the system , 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
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment 2
[0014] The catalyst was changed to TS-1 molecular sieve with a Sn loading of 2% (weight), and under the same conditions as in Example 1, the transesterification reaction was carried out, and the reaction results were investigated. [Example 3]
Embodiment 3
[0015] The catalyst was changed to a 4% (weight) TS-1 molecular sieve with a Sn loading of 4%, under the same conditions as in Example 1, the transesterification reaction was carried out, and the reaction results were investigated. 【Example 4】
Embodiment 4
[0016] The catalyst was changed to 8% (weight) TS-1 molecular sieve with a loading of Sn. Under the same conditions as in Example 1, the transesterification reaction was carried out, and the reaction results were investigated. [Example 5-7]
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The present invention uses dimethyl oxalate and phenol as raw material, under the condition of that the raw material feeding mole ratio of dimethyl oxalate: phenol is 1:20-20:1, reaction time is 1-4 hr, reaction temp. is 170-190 deg.C, autoreaction pressure is 0-1.0 MPa and in the presence of catalyst the ester exchange reaction process is made, a it is characterized by that it catalyst is tin modified TS-1 molecular sieve, and the dose of said catalyst is 1 / 64-1 / 16 of total feeding amount.
Description
technical field [0001] The present invention relates to a kind of processing method that is used to prepare the raw material of diphenyl carbonate (DPC), specifically, relate to the preparation method of methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO), especially Using tin-modified TS-1 molecular sieve as a catalyst, methyl phenyl oxalate and diphenyl oxalate were prepared through the transesterification reaction between dimethyl oxalate (DMO) and phenol under heterogeneous conditions. 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: or [0003] 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 bee...
Claims
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Login to View More IPC IPC(8): C07C67/28C07C67/30C07C69/36C07C69/612
Inventor 马新宾王胜平郭宏利那平许根慧
Owner TIANJIN UNIV