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Benzoic acid based anhydrous and solvent-free method for preparing heptanaphthenic acid

A technology for cyclohexanecarboxylic acid and benzoic acid, which is applied in the preparation of carboxylic acids by ozone oxidation, organic chemistry, etc., can solve the problems of difficult solvent separation, harsh reaction conditions, and low product yields, and achieves advanced technical routes, high selectivity, and The effect of high product purity

Inactive Publication Date: 2015-08-19
XI'AN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these processes all have the problems of many by-products, difficult solvent separation, harsh reaction conditions and low product yields.

Method used

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  • Benzoic acid based anhydrous and solvent-free method for preparing heptanaphthenic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Weigh benzoic acid and catalyst respectively according to the mass ratio of 7:1;

[0060] The weighed benzoic acid is placed in a heating container for heating and dissolving, and the heating temperature is controlled at 100° C. to obtain the benzoic acid after heating;

[0061] Take the hydrogenation reactor, add the hot-dissolved benzoic acid together with the weighed catalyst into the hydrogenation reactor; heat the hydrogenation reactor, and feed nitrogen into the hydrogenation reactor after heating to room temperature; Heating, when the temperature in the hydrogenation reactor reaches 150°C and the pressure is 1MPa, and the pressure in the hydrogenation reactor is stable at 1MPa and does not absorb hydrogen, the hydrogenation reactor is cooled to At 70°C, open the hydrogenation reactor to obtain reactants; filter the obtained reactants to obtain crude cyclohexanecarboxylic acid;

[0062] Put the crude cyclohexanecarboxylic acid into the rectification tower, after ...

Embodiment 2

[0064] Take respectively benzoic acid and catalyst according to the mass ratio of 8:1;

[0065] The weighed benzoic acid is placed in a heating container for heating and dissolving, and the heating temperature is controlled at 120° C. to obtain hot-dissolved benzoic acid;

[0066] Take the hydrogenation reactor, add the hot-dissolved benzoic acid together with the weighed catalyst into the hydrogenation reactor; heat the hydrogenation reactor, and feed nitrogen into the hydrogenation reactor after heating to room temperature; Heating, when the temperature in the hydrogenation reactor reaches 160°C, the pressure is 1.2MPa, and the pressure in the hydrogenation reactor is stable at 1.2MPa, and no hydrogen is absorbed, the hydrogenation reactor is cooled, and the hydrogenation reactor Lower the temperature to 75°C, open the hydrogenation reactor to obtain reactants; filter the obtained reactants to obtain crude cyclohexanecarboxylic acid;

[0067] Put the crude cyclohexanecarbox...

Embodiment 3

[0069] Take respectively benzoic acid and catalyst according to the mass ratio of 9:1;

[0070] The weighed benzoic acid is placed in a heating container for heating and dissolving, and the heating temperature is controlled at 140° C. to obtain hot-dissolved benzoic acid;

[0071] Take the hydrogenation reactor, add the hot-dissolved benzoic acid together with the weighed catalyst into the hydrogenation reactor; heat the hydrogenation reactor, and feed nitrogen into the hydrogenation reactor after heating to room temperature; Heating, when the temperature in the hydrogenation reactor reaches 170°C, the pressure is 1.5MPa, and the pressure in the hydrogenation reactor is stable at 1.5MPa, and no hydrogen is absorbed, the hydrogenation reactor is cooled, and the hydrogenation reactor Cooling down to 80°C, opening the hydrogenation reactor to obtain reactants; filtering the obtained reactants to obtain crude cyclohexanecarboxylic acid;

[0072] Put the crude cyclohexanecarboxyli...

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Abstract

The invention discloses a benzoic acid based anhydrous and solvent-free method for preparing heptanaphthenic acid. The method specifically comprises the following steps of: S1, separately weighing benzoic acid and a catalyst; S2, putting the weighed benzoic acid in step 1 in a heating container to be heated and dissolved at the temperature of 100-140 DEG C to obtain thermally dissolved benzoic acid; S3, taking a hydrogenation reaction kettle; adding the thermally dissolved benzoic acid obtained in S2 together with the catalyst weighed in S1 into the hydrogenation reaction kettle; replacing three times by nitrogen, reacting to obtain a reaction product; and filtering the reaction product to obtain a heptanaphthenic acid coarse product; and S4, feeding the heptanaphthenic acid coarse product obtained in S3 to a rectifying tower to obtain heptanaphthenic acid. According to the benzoic acid based anhydrous and solvent-free method for preparing heptanaphthenic acid disclosed by the invention, high purity heptanaphthenic acid is obtained by using benzoic acid by adopting an anhydrous and solvent-free one-step hydrogenation method.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of chemical and chemical materials, and in particular relates to a method for preparing cyclohexanecarboxylic acid anhydrous and solvent-free based on benzoic acid. Background technique [0002] Cyclohexanecarboxylic acid is an important intermediate in organic synthesis, and it is a good photocuring agent, which can be used in the synthesis of anti-pregnancy 392 drugs and the new drug praziquantel for the treatment of schistosomiasis. Derivatives of cyclohexanecarboxylic acid, such as: trans-4-isopropyl cyclohexanecarboxylic acid is an intermediate in the production of the new drug nateglinide for the treatment of diabetes, and methyl cyclohexanecarboxylic acid is also an important intermediate with a wide range of uses. [0003] There are more than 20 methods for preparing cyclohexanecarboxylic acid, among which the methods using Grignard reagent method, benzoic acid catalytic hydrog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C61/08C07C51/36
CPCC07C51/36C07C2601/14C07C61/08
Inventor 薛凝刘新纪杜燕萍刘斌丁涛王志刚胡新煜
Owner XI'AN POLYTECHNIC UNIVERSITY
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