Method for preparing carboxylic acid ester by using aldehyde, alcohol and oxidizing agent as raw material
A technology of oxidant and carboxylate, applied in the direction of aldehyde redox preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of long reaction time, high price, low selectivity and yield, etc., and achieve improvement The effect of conversion rate and selectivity, small amount of addition, and simple and easy operation method
Active Publication Date: 2011-04-20
INST OF PROCESS ENG CHINESE ACAD OF SCI
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Problems solved by technology
However, in the above-mentioned patents, either the selectivity and yield of reactants are low, or the selectivity and conversion rate are improved under relatively harsh conditions.
In Chinese patent 2003101152747, although the selectivity and conversion rate of the reaction have been improved under milder conditions, the reaction time is longer, the amount of ionic liquid used is large, the price is higher, and the economy is poor
In summary, no effective solution has been proposed in the existing patents
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment 1
[0018] Weigh 0.0252g of metalloporphyrin (M=Fe, X=Cl, Y=Cl) and 1g of catalyst respectively, put them into the reaction kettle, then measure 63.4ml of methanol and 6.6ml of methacrolein, and add them to the reaction kettle , stirred, heated to 80°C in a circulating water bath, fed oxygen to make the reaction pressure reach 0.3MP, then controlled the flow rate to 12.5ml / min, and reacted for 2h. Liquid chromatography was used as a quantitative analysis method. The conversion of aldehyde was 90.2%, and the selectivity of ester was 96.6%.
Embodiment 2
[0020] As in Example 1, the methacrolein in the raw material was changed to acrolein, the conversion rate of aldehyde was 91.3%, and the selectivity of ester was 98.3%.
Embodiment 3
[0022] Same as Example 1, the metalloporphyrin is dissolved in ethanol, and the methanol in the raw material becomes ethanol. The conversion of aldehyde was 92.1%, and the selectivity of ester was 97.6%.
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The present invention relates to process of pg carboxylate with aldehyde, alcohol and oxidant as materials, and features that in the reaction, metalloporphyrin in small amount is added to result in mild condition and raise the selectivity and conversion rate. The process is flexible, easy to operate, and suitable for both intermittent and continuous production.
Description
Technical field: [0001] A new method for the preparation of carboxylic acid esters from aldehydes, alcohols and oxidizing agents in the presence of metalloporphyrins. Background technique: [0002] Carboxylate is an important chemical, widely used in social production and life, such as methyl methacrylate, which is an essential raw material in the production of plexiglass, advanced coatings and adhesives. Most of the synthesis methods of carboxylic acid esters in the past use organic acids and alcohols as raw materials, and carry out esterification reaction under the action of strong inorganic acids, but the price of raw materials is relatively high, and the reactors are corroded, causing serious problems such as environmental pollution and human poisoning. . Therefore, in recent years, countries are developing new methods for the synthesis of carboxylic acid esters. [0003] Since the 1970s, there have been a number of patents related to the one-step catalytic production ...
Claims
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IPC IPC(8): C07C67/44B01J31/12
Inventor 张锁江李曦芝闫瑞一刁琰琰杨普田伟张垲
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI