Preparation method and applications of B-SBA-16 loaded silicotungstic acid type ionic liquid composite catalyst

A B-SBA-16, 1. B-SBA-16 technology, applied in the field of immobilized ionic liquid composite catalysts, can solve the problems of not widely used and difficult synthesis process, so as to improve the catalytic effect and strengthen the acidity Effect

Inactive Publication Date: 2019-11-19
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] SBA-16 mesoporous molecular sieve is a kind of mesoporous molecular sieve with excellent structural properties but not yet widely used. It uses F127 as template agent and tetraethyl orthosilicate as silicon source, through hydrolysis and aging process in acidic environment The obtained molecular sieve with a cage-shaped three-dimensional cubic ordered structure has been favored by many researchers since the synthesis and preparation of Zhao Dongyuan's project, but because of the relatively difficult synthesis process, many researchers are discouraged and use it. As a carrier, it is rarely used in the field of immobilized ionic liquids

Method used

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  • Preparation method and applications of B-SBA-16 loaded silicotungstic acid type ionic liquid composite catalyst
  • Preparation method and applications of B-SBA-16 loaded silicotungstic acid type ionic liquid composite catalyst
  • Preparation method and applications of B-SBA-16 loaded silicotungstic acid type ionic liquid composite catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] First, prepare B-SBA-16, and then prepare the silicotungstic acid ionic liquid. After the ionic liquid is successfully prepared, it is introduced into the pores of the molecular sieve to obtain the immobilized ionic liquid. The specific method is as follows:

[0036] Step 1. Synthesis of B-SBA-16

[0037] Dissolve 2g of F127 in 90ml of 1.62mol / L hydrochloric acid in a beaker, stir magnetically until the solution is clear and transparent, transfer the solution to a 250ml three-necked flask, drop 8g of TEOS into the flask drop by drop, and then continue to 34 Stir vigorously in a water bath at ℃ for 20h; after the reaction, filter and wash with suction, transfer the filter cake to a polytetrafluoroethylene reactor, add a certain amount of deionized water, stir evenly, aging in a hydrothermal environment at 100℃ for 24h, the aging is over Then continue to filter and wash for 2-3 times, then dry at 100°C for 12h; calcined at 550°C to remove the template, heating rate 1°C / min, ho...

Embodiment 2

[0050] The solid-supported ionic liquids with the silicon to boron ratios of 30 and 10 were prepared according to the steps of Example 1, and the obtained composite catalyst was used to catalyze the reaction of cyclohexanone and ethylene glycol ketal.

[0051] According to the molar ratio of ketone to alcohol is 1:1.8, add 1.96g cyclohexanone to the flask, the reaction temperature is 85℃, the amount of catalyst is 0.25g, and the reaction time is 3h. The effect of different B doping amount on the catalytic performance of the composite catalyst is investigated. The experiment shows When the ratio of silicon to boron is 30, the conversion rate of cyclohexanone is 93.01% and the yield of ketal is 78.39%. When the ratio of silicon to boron is 10, the conversion rate of cyclohexanone is 90.49% and the yield of ketal is 84.24%. This result shows that when the ratio of silicon to boron is 15, the obtained composite catalyst has the best catalytic effect.

Embodiment 3

[0053] According to the steps of Example 1, by changing the loading amount of the ionic liquid, a solid-supported ionic liquid with a loading amount of 0.8 g and 1.5 g was prepared, and the effect on the catalytic reaction of cyclohexanone and ethylene glycol ketal was investigated.

[0054] According to the ketone alcohol molar ratio of 1:1.8, 1.96g cyclohexanone was added to the flask, the reaction temperature was 85°C, the amount of catalyst was 0.25g, and the reaction time was 3h. The results showed that when the loading amount of ionic liquid was 0.8g, the conversion rate of cyclohexanone was 90.94% and the yield of ketal was 66.41%; and when the loading amount of ionic liquid was 1.5g, the conversion rate of cyclohexanone was 91.09. %, the ketal yield is 69.05%. Therefore, the optimal load of ionic liquid per gram of B-SBA-16 is 1.2g.

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Abstract

The invention belongs to the field of inorganic nanometer composite material, and discloses a preparation method and applications of a B-SBA-16 loaded silicotungstic acid type ionic liquid composite catalyst. The preparation method comprises following steps: 1, two-step method is adopted to prepare B-SBA-16; 2, silicotungstic acid ionic liquid is prepared; and 3, ionic liquid immobilizing loadingis carried out. According to the preparation method, catalytic performance is studied taking reaction of cyclohexanone and glycol ketal reaction as a model. It is shown by experiment results that thesynthesized immobilized ionic liquid is excellent in catalytic performance, stability, and reusability, and is an excellent green catalyst, and green chemistry ideas are satisfied.

Description

Technical field [0001] The invention belongs to the field of inorganic nano composite materials, and relates to a silicotungstic acid type solid-supported ionic liquid composite catalyst synthesized by an impregnation method. Background technique [0002] In the past few decades, ionic liquids have continued to become a hot topic and focus of chemistry researchers. Because ionic liquids are environmentally friendly, they are often referred to as green solvents or green catalysts. They have many advantages, such as high viscosity and low viscosity. Vapor pressure, strong solubility, wide operating temperature range, good anion and cation settable and adjustable acidity, are widely used in gas adsorption, catalysis, solvents and other fields. Traditional ionic liquids are usually prepared by acidification with sulfuric acid, chloroaluminate, etc. The synthesized ionic liquids have slightly lower activity, while heteropoly acid is an environmentally friendly multifunctional acid wit...

Claims

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Application Information

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IPC IPC(8): B01J31/26B01J37/02B01J31/18B01J35/10C07D317/72
CPCB01J31/0295B01J31/0298B01J37/0201B01J27/188C07D317/72B01J35/61
Inventor 谢英杰姜廷顺任玥玥赵谦
Owner JIANGSU UNIV
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