Preparation method of metal organic framework material and application of metal organic framework material in cyclohexyl hydroperoxide decomposition reaction

A technology of cyclohexyl hydroperoxide and metal-organic framework, which is applied in the field of fine chemicals, can solve the problems that the catalyst cannot be recycled many times, the loss of chromium, and the irreversible deactivation of molecular sieves, etc., and achieves good catalytic effect, short synthesis cycle and excellent preparation process. simple effect

Active Publication Date: 2016-06-29
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the rapid loss of chromium is the cause of the irreversible deactivation of the molecular sieve, and the catalyst cannot be recycled for many times

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 2.0gCr (NO 3 ) 3 9H 2 O and 0.82g terephthalic acid dissolved in 25mL0.05mol L -1 sodium acetate solution, stirred at room temperature for 30 min. The obtained solution was transferred to a 50 mL self-generating autoclave with polytetrafluoroethylene, and the reaction autoclave was placed in a blast drying oven heated to 200° C. for 12 hours. After the reaction, the reaction kettle was left to stand, slowly cooled to room temperature, and the obtained liquid was centrifuged, and the separated solid was first washed with N,N-dimethylimide at 70°C for 1 hour, then washed with ethanol for 1 hour, and finally Wash with water for 1h. The obtained solid was vacuum-dried at 150° C. for 12 h to obtain a Cr metal-organic framework material, which was denoted as MIL-101 (Cr).

[0034] The following examples illustrate the catalytic decomposition method of cyclohexyl hydroperoxide in the cyclohexane oxidation solution provided by the present invention.

[0035] The cyclohexa...

Embodiment 2

[0038] Take 0.05g of the catalyst prepared in Example 1 and 10mL (about 8.22g) of cyclohexane oxidation solution, and add them into a 50mL three-necked flask. Heat to 70°C while stirring, and react at constant temperature for 100 minutes. After cooling to room temperature, the reaction solution was taken out for analysis. The conversion rate of cyclohexyl hydroperoxide is 97.9%, the selectivity of cyclohexanone and cyclohexanol is 100%, and cyclohexanone:cyclohexanol=6.5:1 (molar ratio).

Embodiment 3

[0040] According to the operation process of embodiment 2, the difference with embodiment 2 is: the catalyst quality of catalyzing the decomposition of cyclohexyl hydroperoxide is 0.1g. The conversion rate of cyclohexyl hydroperoxide is 98.2%, the selectivity of cyclohexanone and cyclohexanol is 100%, and cyclohexanone:cyclohexanol=6.7:1 (molar ratio).

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Abstract

The invention discloses a preparation method of a metal organic framework material and application of the metal organic framework material in a cyclohexyl hydroperoxide decomposition reaction. Transition metal salt and terephthalic acid or a derivative thereof are subjected to a hydrothermal synthesis reaction in a sodium acetate solution to obtain the metal organic framework material, then the metal organic framework material serving as a catalyst is added into industrial cyclohexane uncatalysed oxidation liquid, the temperature is controlled to be 50-150 DEG C, the time is controlled to be 0.1-5 h, cyclohexyl hydroperoxide decomposition is carried out to obtain hexamethylene and cyclohexanone, the conversion rate of cyclohexyl hydroperoxide is larger than 95%, and the selectivity of alcohol ketone reaches up to 100%; the activity of the repeatedly-recycled catalyst is kept unchanged basically. Compared with other catalysts containing metal active components, the catalyst is high in catalytic efficiency, recyclable and stable in reusability; when the catalyst is applied to the cyclohexyl hydroperoxide decomposition reaction, the decomposition process is conducted under the alkali-free condition, the catalytic efficiency is very high, and pollution caused by waste alkali liquor to the environment is avoided.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of a metal organic framework material and its application in the decomposition reaction of cyclohexyl hydroperoxide. Background technique [0002] As an important petrochemical raw material, cyclohexanone is mainly used to synthesize caprolactam and adipic acid, which are monomers of polyamide and nylon; it is an important solvent in medicine, coatings, plastic recycling and other industries. The demand is constantly growing and the application prospect is relatively broad. At present, the commonly used method for industrial production of cyclohexanone is cyclohexane oxidation, which includes two processes of catalytic oxidation and non-catalytic oxidation oxidation. The non-catalytic oxidation of cyclohexane from DSM in the Netherlands is the most widely used to prepare cyclohexanone. The process is divided into two steps. First, cyclohexane is uncat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C63/28B01J31/22C07C27/04C07C29/132C07C35/08C07C45/53C07C49/403
CPCY02P20/52Y02P20/584C07C51/418B01J31/2239B01J2231/54B01J2531/62B01J2531/842C07C29/132C07C45/53C07C63/28C07C35/08C07C49/403
Inventor 袁霞郭露露吴剑李立霞
Owner XIANGTAN UNIV
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