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Process for preparation of carboxylic acid esters

A synthesis method and technology of carboxylate, which is applied in the preparation of carboxylate, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of equipment corrosion, incomplete solution, limited alcohol varieties and sources, and achieve the source of raw materials Extensive, simple process, high product purity

Inactive Publication Date: 2008-04-09
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These production methods need acid and alkali as catalysts, which seriously corrode equipment. CN03108171.1 discloses a kind of acid catalyst with sulfuric acid and heteropolyacid (salt) as corrosion inhibitor, although it can reduce some corrosion problems to metal equipment. , but it cannot be completely solved, and the synthetic raw materials used are still carboxylic acids and alcohols. Due to the very limited varieties and sources of alcohols, various types of carboxylic acid esters cannot be produced.

Method used

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  • Process for preparation of carboxylic acid esters
  • Process for preparation of carboxylic acid esters
  • Process for preparation of carboxylic acid esters

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In 500ml cyclohexane, add the metalloporphyrin with the structure of Fig. 1, R 1 = H, R 2 =R 3 =CH 3 , M=Mn, to a metalloporphyrin concentration of 3ppm. Pass into 0.8MPa air, stir the reactant at 160°C for 4 hours, the conversion rate of cyclohexane is 20%, the reaction products are cyclohexyl glutarate and cyclohexyl adipate, and the selectivity of monoester and diester is 78% .

Embodiment 2

[0021] In 100ml acetic acid and 300ml isobutane, add the metalloporphyrin with the structure of Figure 2, the metalloporphyrin concentration is 10ppm, in the formula R 1 =R 2 =OCH 3 , R 3 =Cl,M 1 = M 2 = Fe, add Cu 2 O to 20ppm, feed 1.8MPa oxygen-containing 15% air. The reactant was stirred at 120° C. for 6 hours, the conversion rate of isobutane was 8%, and the selectivity of the reaction product tert-butyl acetate was 67%.

Embodiment 3

[0023] In 150ml propionic acid and 300ml containing C 2 -C 4 In the mixed alkanes, add metalloporphyrins with the structure shown in Figure 1, where R 1 =R 2 =C 2 h 5 , R 3 =Br, M=Fe, to a metalloporphyrin concentration of 20ppm, add CoCl 2 to 30ppm. 0.4MPa air was introduced, and the reactant was stirred at 85° C. for 10 hours. The conversion rate of alkane was 20%, and the selectivity of mixed propionate in the reaction product was 55%.

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Abstract

The invention discloses a Synthesis of carboxylic ester. In neutral environment, using paraffin, naphthene, olefin, aromatic hydrocarbons or other low carbon hydrocarbon mixture as material, molecule oxygen as oxidant, one or multiple kind of single metalloporphyrin of general formula (I) or mu-oxidant bimetalloporphyrin of general formula (II), or their solid carrier as accelerant individually to be accelerant or the composite catalyst of they and metal salt or oxidate, the metalloporphyrin's concentration in accelerant is 1-100ppm; controlling the reaction temperature is 80-200deg C,reaction pressure is 0.1~2MPa., React for 1-10h, molecule oxygen firstly oxygenating hydrocarbon to carboxyl acid and alcohol, and then carboxyl acid and alcohol are further oxygenated to ester. This invention can completes oxidation and esterification reaction of hydrocarbon at the same time, has no pollution, no corrosion, the technique is simple, the raw material soure is broad, need not separate intermediate product, product's purity is high and can produce miscellaneous carboxylate.

Description

technical field [0001] The present invention relates to a kind of synthetic method of carboxylate. Background technique [0002] Carboxylic acid esters are important fine organic chemical products, mainly used as solvents, additives, drugs, flavors and fragrances, etc. At present, the industrial production of carboxylic acid ester compounds is mainly obtained through the esterification reaction or transesterification reaction of carboxylic acid and alcohol. These production methods need acid and alkali as catalysts, which seriously corrode equipment. CN03108171.1 discloses a kind of acid catalyst with sulfuric acid and heteropolyacid (salt) as corrosion inhibitor, although it can reduce some corrosion problems to metal equipment. , but it cannot be completely solved, and the synthetic raw materials used are still carboxylic acids and alcohols. Since the types and sources of alcohols are very limited, various types of carboxylic acid esters cannot be produced. Contents of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C27/12C07C69/00B01J31/22
Inventor 郭灿城姜权胡海洋刘强
Owner HUNAN UNIV
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