Alkylated hydrophobic MOFs material and application thereof in cyclohexene hydration

An alkylation and alkylation modification technology, applied in the field of chemical engineering, can solve problems such as low conversion rate, and achieve the effects of improving catalytic efficiency, good application prospects, and increasing contact area

Active Publication Date: 2021-06-11
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cyclohexene hydration reaction system is a three-phase reaction of oil phase-water phase-solid phase, and the unmodified MOFs material is at the bottom of the water phase and cannot contact the oil phase, resulting in a low conversion rate.

Method used

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  • Alkylated hydrophobic MOFs material and application thereof in cyclohexene hydration
  • Alkylated hydrophobic MOFs material and application thereof in cyclohexene hydration
  • Alkylated hydrophobic MOFs material and application thereof in cyclohexene hydration

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Preparation of alkylated hydrophobic MOFs material UiO-66-HAc-OTS:

[0042] (1) Weigh 0.932ZrCl respectively 4 , 1.32g H 2 Dissolve BDC (1,4 phthalic acid) and 5 mL acetic acid in 24 mL DMF (N, N-dimethylformamide), and sonicate for 30 min to obtain solution A;

[0043] (2) After solution A is completely dissolved, transfer it to a reaction kettle lined with polytetrafluoroethylene, seal it, and heat it statically at 120°C for 24 hours;

[0044] (3) When the crystallization is completed and cooled to room temperature, the solution A is centrifuged, and the solid is retained, washed three times with N,N-dimethylformamide, and then washed three times with methanol to remove residual reactants and exchange N , N-dimethylformamide, after washing, white powdery product is obtained;

[0045] (4) Transfer the white powdery sample obtained in step (3) to a watch glass, and put it in a vacuum drying oven, set 100 ° C, and vacuum dry for 24 hours to obtain UiO-66-Hac; (step...

Embodiment 2

[0055] The UiO-66-HAc-OTS obtained in Example 1 was used to catalyze the hydration reaction of cyclohexene, and the reaction conditions were referred to step 2 of Example 1, except that the selected hydration reaction temperature was different. The selection of the reaction temperature and the reaction results are shown in Table 1.

[0056] The influence of table 1 reaction temperature on cyclohexene hydration reaction

[0057]

[0058] It can be seen from Table 1 that the hydration of cyclohexene is a reversible exothermic reaction. Increasing the reaction temperature effectively increases the effective collision between molecules and accelerates the reaction rate. At the same time, the adsorption rate of cyclohexene and the desorption rate of cyclohexanol on the catalyst surface are both accelerated. The reaction conversion rate is effectively improved. When the reaction temperature is too low, the molecular activity is low and the conversion rate is not high; when the r...

Embodiment 3

[0060] The UiO-66-HAc-OTS obtained in Example 1 was used to catalyze the hydration reaction of cyclohexene, and the reaction conditions were referred to step 2 of Example 1, except that the selected hydration reaction time was different. The selection of reaction time and reaction results are shown in Table 2.

[0061] The influence of table 2 reaction time on cyclohexene hydration reaction

[0062]

[0063]

[0064] As can be seen from Table 2, the reaction time has little influence on the selectivity of cyclohexanol, but has a certain influence on the conversion rate of cyclohexene. When the reaction time was 1h, the conversion rate of cyclohexene was 10.5%; when the reaction time was increased to 4h, the conversion rate of cyclohexene reached a maximum of 18.8%; the reaction time was prolonged, and the conversion rate of cyclohexene tended to balance, but Cyclohexanol yield decreased slightly. This is because prolonging the reaction time will increase the concentrat...

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PUM

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Abstract

The invention discloses an alkylated hydrophobic MOFs material which is a Zr-based metal organic framework material subjected to acid modification and alkylation modification. The acid modification is preferably modification with acetic acid ; and the alkylation modification is modification with n-octyl trimethoxy silane. The invention also discloses an application of the alkylated hydrophobic MOFs material in preparation of cyclohexanol by cyclohexene hydration. Compared with an unmodified MOFs material, the modified MOFs material has acidic sites and certain hydrophobicity, so that the MOFs material is preferentially gathered on an oil-water interface, the emulsion stability is improved, the liquid-liquid interface area is greatly increased, and the conversion rate is further increased.

Description

technical field [0001] The invention belongs to the field of chemical engineering, and in particular relates to an alkylated hydrophobic MOFs material and its application in cyclohexene hydration. Background technique [0002] Cyclohexene is hydrated to prepare cyclohexanol. Cyclohexanol is used as a paint solvent in paint, as a matting agent in textiles, and as a matting agent in chemical industry to generate oxalic acid, which is further synthesized into nylon 66. With the development of the times, nylon 66 is widely used in the synthesis of electronic products, wristbands, automobiles and a series of precision equipment. It can be seen that cyclohexanol plays an important role in chemical industry, paint, textile and other aspects. [0003] The process development route of cyclohexanol is divided into three stages. The first is the phenol hydrogenation method, which generates cyclohexanol through hydrogenation, but there is a disadvantage of excessive energy consumption....

Claims

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Application Information

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IPC IPC(8): B01J31/22C08G83/00C07C29/04C07C35/08
CPCB01J31/2239B01J31/1691C08G83/008C07C29/04B01J2531/48B01J2231/32C07C2601/14C07C35/08
Inventor 田晖刘帅李建树曹敏孙大海陈小平
Owner YANTAI UNIV
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