Supported solid catalyst and preparation method and application thereof

A solid catalyst and supported technology, applied in the chemical industry, can solve the problems of lower ester yield, difficult to handle, yellowish color, etc., and achieve the effects of high selectivity, low production cost, and less industrial wastewater

Active Publication Date: 2016-01-06
HUBEI XUNDA PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Concentrated sulfuric acid or p-toluenesulfonic acid are usually added as esterification catalysts in the synthesis, but the oxidation of the raw material 2-(4'-bromomethylphenyl)propionic acid is easily caused by the oxidation of concentrated sulfuric acid, thereby reducing the yield of esters. At the same time, the color of the product is yellowish, and it must be recrystallized many times to meet the requirements; although p-toluenesulfonic acid avoids the problem of strong oxidation of concentrated sulfuric acid, it is easy to produce difficult-to-treat p-toluenesulfonic acid industrial wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Catalyst preparation: take by weighing 3.04g of Cu(NO 3 ) 2 ·3H 2 O, dissolve it in 20ml water, then add 10g carrier TiO 2 -Al 2 o 3 -SiO 2 (TiO 2 、Al 2 o 3 with SiO 2 The mass percentage is 0.9:0.05:0.05), stirred for 3h, slowly heated up to evaporate the water, and then the obtained solid was roasted at 450°C for 4h to obtain CuO / TiO 2 -Al 2 o 3 -SiO 2 The solid powder is ready for use. Then take 2.31g of (NH 4 ) 2 SO 4 , dissolved in appropriate amount of water, impregnated CuO / TiO 2 -Al 2 o 3 -SiO 2 , dried, and finally roasted at 650°C for 2h to obtain CuO-SO 4 2- / TiO2 -Al 2 o 3 -SiO 2 solid catalyst.

[0023] Synthesis example of 2-(4'-bromomethylphenyl) propionate: In a 50ml three-necked flask equipped with a condenser and a thermometer, add 2.4g of 2-(4'-bromomethylphenyl)propionic acid, 20ml of methanol and 0.24 g of CuO-SO 4 2- / TiO 2 -Al 2 o 3 -SiO 2 Solid catalyst, reacted at 65°C for 8 hours to obtain methyl 2-(4'-bromomethy...

Embodiment 2

[0025] In addition to carrier TiO 2 -Al 2 o 3 -SiO 2 Medium TiO 2 、Al 2 o 3 with SiO 2 Except that the mass percent is 0.5:0.25:0.25, other conditions are the same as in Example 1 to obtain 2-(4'-bromomethylphenyl) methyl propionate, with a yield of 60.3% and a selectivity of 96.3%.

Embodiment 3-6

[0027] Except catalyst, other conditions are with embodiment 1. The results are shown in the table below:

[0028] Example number

[0029] 4

[0030] Remarks: a: The molar ratio of Sn to Pb is 1:1. b: The molar ratio of Sn to Bi is 1:1.

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Abstract

The invention relates to a supported solid catalyst and a preparation method and application thereof. The chemical formula of the catalyst is MxOy-SO42-/TiO2-Al2O3-SiO2, wherein M is metal ions, x and y are valence state balance numbers, and carriers are TiO2-Al2O3-SiO2. The catalyst is prepared in a step-by-step impregnation method, and nitrate or hydrochloride or ammonium persulfate is sequentially loaded to the carriers TiO2-Al2O3-SiO2 so that the catalyst can be prepared. The catalyst is particularly suitable for being used as a catalyst in the technology of synthesizing loxoprofen intermediate 2-(4'-bro-methyl phenyl) propionate and has the advantages that selectivity is high, the conversation rate is high, reaction conditions are moderate, separation of the catalyst is easy, industrial waste water is little, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a supported catalyst and its preparation method and application. Background technique [0002] Traditional non-steroidal anti-inflammatory drugs may cause serious gastrointestinal adverse reactions such as gastric ulcer, bleeding and perforation if taken for a long time, and taking non-steroidal anti-inflammatory drugs is one of the most common causes of serious adverse drug reactions. Loxoprofen, as an improved NSAIDs marketed in the late 1980s, maintains the antipyretic, analgesic, and anti-inflammatory effects of traditional NSAIDs in terms of curative effect, and has a quick onset and strong effect. In terms of safety, loxoprofen significantly reduces the occurrence of gastrointestinal adverse reactions due to its structural characteristics of propionic acid prodrugs. Therefore, loxoprofen has great prospects in the Chinese market due to its good efficacy, anti-inf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/055B01J27/053B01J35/10B01J37/02C07C69/65C07C67/08
Inventor 杜治平文武强李亮丁一刚张巨寿刘生鹏邓伏礼龙秉文
Owner HUBEI XUNDA PHARMA
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