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Method for co-producing adipic acid and nitrocyclohexane

A technology of nitrocyclohexane and cyclohexane, which is applied in the direction of chemical instruments and methods, preparation of nitro compounds, carboxylate preparation, etc., can solve the problems of high cost, difficult separation of soluble catalysts, low selectivity of adipic acid, etc. question

Active Publication Date: 2013-09-11
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although these methods can obtain higher cyclohexane conversion rate and adipic acid selectivity, there are also many problems: first, under its reaction temperature and pressure conditions, acetic acid has greater corrosion to equipment; secondly, The target product adipic acid and other by-products are difficult to separate and purify from the acetic acid solvent; thirdly, the soluble catalyst is difficult to separate from the acetic acid solvent, although FRA2722783 (1996) and FRA2746671 (1997) have proposed a method to solve the catalyst recycling , but the process is complex and expensive
However, low cyclohexane conversion (approximately 2.5%), long reaction times, low overall selectivity to major products (adipic acid and nitrocyclohexane) and a sharp increase in adipic acid selectivity with increasing temperature reduce

Method used

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  • Method for co-producing adipic acid and nitrocyclohexane
  • Method for co-producing adipic acid and nitrocyclohexane
  • Method for co-producing adipic acid and nitrocyclohexane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Embodiment 1: press cyclohexane and NO 2 The molar ratio of cyclohexane to catalyst is 0.2:1, and the mass ratio of cyclohexane to catalyst is 1:0.1. Add 5.04g cyclohexane and 13.80g liquid NO to a 0.2L autoclave 2 And 0.54g catalyst Cr-AlVPO; react at 80°C and 2.0MPa for 24h under stirring conditions. Stratification after standing and cooling, the upper layer is an oil phase, mainly containing unreacted cyclohexane and product nitrocyclohexane, the lower layer is mainly a mixture of adipic acid crystals, catalyst solids, and reaction water; filter all materials And wash the filter cake with quantitative cyclohexane and distilled water respectively; The collected filtrate and washing liquid are separated to obtain the oil phase and the water phase and are measured respectively. The oil phase is quantitatively determined by gas chromatography internal standard method. The composition was determined by liquid chromatography external standard method; the filter cake was d...

Embodiment 2

[0079] Embodiment 2: As in Embodiment 1, the difference lies in that the reaction temperature is 100° C., and the reaction pressure is 2.9 MPa. The conversion rate of cyclohexane was 75.4%, the selectivity of adipic acid was 81.7%, the selectivity of nitrocyclohexane was 11.5%, and the sum of the two selectivities was 93.2%.

Embodiment 3

[0080] Embodiment 3: as embodiment 1, by cyclohexane and NO 2 Add 8.40g cyclohexane and 4.60g liquid NO at a molar ratio of 1:1.0 2 , the catalyst is VPO; the reaction temperature is 60°C, and the reaction pressure is 0.6MPa. The conversion rate of cyclohexane was 11.1%, the selectivity of adipic acid was 80.6%, the selectivity of nitrocyclohexane was 11.9%, and the sum of the two selectivities was 92.5%.

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Abstract

The present invention relates to a method for high selectivity co-production of adipic acid and nitrocyclohexane. According to the present invention, a nitrogen oxide NOx is adopted as an oxidant and a nitrating agent to carry out one step high selectivity conversion of cyclohexane into adipic acid and nitrocyclohexane, and adjustments of a reactant ratio, a reaction temperature, a reaction pressure, a type and an amount of a catalyst or an induction agent, and other conversion conditions are adopted to achieve regulation of a production ratio of the adipic acid and the nitrocyclohexane; and NO produced from the reaction can be recycled and then reacts with oxygen to be converted into NOx so as to be recycled.

Description

technical field [0001] The invention relates to a method for one-step conversion from cyclohexane to co-produce adipic acid and nitrocyclohexane with high selectivity. Background technique [0002] Adipic acid (ADA), commonly known as fatty acid, is a white solid at room temperature with a molecular formula (CH 2 ) 4 (COOH) 2 , molecular weight 146.1430, normal melting point 152°C. Adipic acid is a very important industrial material and intermediate, mainly used in the manufacture of nylon 66, plasticizers, greases, pesticides and adhesives. So far, the synthesis route of adipic acid mainly includes cyclohexane oxidation two-step method, cyclohexene hydration-oxidation two-step method, cyclohexane (molecular oxygen) oxidation one-step method, butadiene carbonylation method, cyclohexene hydrogen peroxide Oxidation one-step method and biological oxidation method, etc. [0003] Nitrocyclohexane is a colorless oily liquid at room temperature, molecular formula C 6 h 11 NO...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/14C07C51/275C07C205/05C07C201/08
CPCC07C201/08C07C51/316C07C2601/14C07C205/05C07C55/14
Inventor 罗和安游奎一蹇建周忠仓刘平乐
Owner XIANGTAN UNIV
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