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Preparation method and application of metal organic framework material loaded with Schiff base complex

A technology of metal-organic framework and Schiff base, which is applied in the preparation and application field of metal-organic framework materials loaded with Schiff base complexes, can solve the problems that catalysts cannot be recycled, achieve good decomposition effect, mild reaction conditions, The effect of increasing alcohol content

Active Publication Date: 2017-08-18
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the catalyst cannot be recycled, and cyclohexanone and cyclohexanol are easy to be deeply oxidized to acid and ester

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 1.6 g of sodium hydroxide solid and dissolve it in 150 mL of deionized water, slowly add 3.6 g of aminoterephthalic acid and 8 g of chromium nitrate nonahydrate to the above solution, and stir at room temperature until the solid is completely dissolved. The resulting solution was transferred to an autogenous autoclave lined with polytetrafluoroethylene, and the autoclave was placed in a blast drying oven heated to 150°C to react for 10 h. After the reaction, the reaction kettle was left to cool down to room temperature, and the reaction product was obtained for centrifugation. The solid product was washed with N,N-dimethylformamide and ethanol at 70°C for 1 hour, and the solid was obtained by centrifugation after washing. Disperse the solid in a polytetrafluoroethylene reactor filled with ethanol, perform solvothermal treatment at 90°C, take it out after 6 hours, and vacuum dry it at 150°C for 12 hours after centrifugation to obtain the amino-modified metal organic...

Embodiment 2

[0039] Take 0.1 g of the catalyst prepared in Example 1, 10 mL (about 8.32 g) of cyclohexane oxidation solution (composed of 8.16% cyclohexyl hydroperoxide, 1.71% cyclohexanone, 2.56% cyclohexanol, 0.76% acid, 1.98% ester %, cyclohexane 84.83%), was added into a 50mL three-necked flask, stirred and reacted at 80°C for 110min, after the reaction was completed, it was left to cool to room temperature, and the reaction liquid was taken out for analysis. The analysis results show that the conversion rate of cyclohexyl hydroperoxide is 97%, the total selectivity of alcohol and ketone is 99.8%, and cyclohexanone:cyclohexanol=1:1.50 (molar ratio).

Embodiment 3

[0041] According to the operation process of embodiment 2, the difference from embodiment 2 is that the catalyst is the catalyzer after repeating embodiment 2 three times. The conversion rate of cyclohexyl hydroperoxide is 97.5%, the total selectivity of alcohol and ketone is 99.8%, cyclohexanone:cyclohexanol=1:1.46 (molar ratio).

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Abstract

The invention discloses a preparation method and an application of a metal organic framework material loaded with a Schiff base complex. Salen is formed by introducing salicylic aldehyde onto an amino functionalization metal organic framework material, then, Salen and transition metal ions form a complex, the metal organic framework material loaded with the Schiff base complex is prepared, and the material is applied to a cyclohexyl hydroperoxide decomposition reaction. The prepared catalyst is high in catalytic performance, the catalytic activity of the catalyst is basically not reduced after being recycled repeatedly, the catalyst is stable in performance and is applied to catalysis of the cyclohexyl hydroperoxide decomposition reaction, the decomposition conversion rate can reach 97%, the total selectivity of alcohol ketone can reach 99.8%, the good decomposition effect can be obtained without alkaline liquor, the environmental problem caused by the waste liquor is effectively avoided, the environmental pollution is significantly reduced, and meanwhile, the proportion of cyclohexanol to cyclohexanone is significantly increased.

Description

technical field [0001] The invention relates to the preparation of a metal-organic framework material loaded with a Schiff base complex and its application in catalytic decomposition of cyclohexyl hydroperoxide to generate cyclohexanol and cyclohexanone under alkali-free conditions. Background technique [0002] Cyclohexanone is an important organic chemical raw material, mainly used in the manufacture of polyamide (nylon 6, nylon 66) monomers such as caprolactam and oxalic acid; it is also a key intermediate (cyclo Hexeneethylamine) is an important raw material; in polyurethane coatings, rubber vulcanization accelerators, color inks, plastic recycling and other industries, the demand for cyclohexanone is growing. [0003] At present, the industry generally adopts the method developed by the Dutch DSM company, that is, cyclohexyl hydroperoxide is subjected to heterogeneous decomposition under the action of a cobalt salt catalyst and an aqueous sodium hydroxide solution, and ...

Claims

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Application Information

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IPC IPC(8): C07C249/02C07C251/24B01J31/22C07C27/00C07C45/53C07C49/403C07C29/00C07C35/08
CPCY02P20/584C07C249/02B01J31/2217B01J2531/0252B01J2531/62B01J2531/845C07C29/00C07C45/53C07C251/24C07C49/403C07C35/08
Inventor 吴剑夏莉萍袁霞郭露露
Owner XIANGTAN UNIV
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