In-situ preparation method for acidic aluminum chlorate ionic liquid loaded SBA-15 catalyst and application

An ionic liquid, in-situ preparation technology, applied in the field of mesoporous materials, can solve the problems of single way of immobilizing ionic liquid, high viscosity of ionic liquid, difficult post-processing process, etc., and achieve cost reduction, easy separation and reduction of ionic liquid loss. Effect

Inactive Publication Date: 2017-07-18
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are three commonly used methods for immobilizing ionic liquids, direct impregnation method, covalent bonding method, sol-gel method, and the method of immobilizing ionic liquids is relatively simple.
At the same time, these commonly used methods are all designed to the synthesis and post-treatment process of ionic liquids, but due to the generally high viscosity of ionic liquids, the post-processing process is difficult and the operation is complicated.

Method used

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  • In-situ preparation method for acidic aluminum chlorate ionic liquid loaded SBA-15 catalyst and application
  • In-situ preparation method for acidic aluminum chlorate ionic liquid loaded SBA-15 catalyst and application
  • In-situ preparation method for acidic aluminum chlorate ionic liquid loaded SBA-15 catalyst and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First prepare SBA-15, and then according to the way of in-situ loading, highly disperse the reaction raw materials of ionic liquid methylimidazole and n-chlorobutane on the inner surface of SBA-15, and control the temperature, directly on the inner surface of SBA-15 Synthesis containing 1-methyl-3-butyl imidazolium chloride salt. The content of 1-methyl 3-butyl imidazolium chloride was measured by thermogravimetry, and the SBA-15 loaded with the acidic chloroaluminate ionic liquid could be obtained after being treated with aluminum chloride. The specific method is as follows: Weigh 5g of SBA-15 into a 250ml three-neck flask, add 50ml of ethyl acetate, stir magnetically, add 4.1g (0.05mol) of methylimidazole, heat to 80-85°C, and stir for 2 ~3 hours. After that, 4.63 g (0.05 mol) of n-chlorobutane was added and reacted for 48 h under nitrogen atmosphere. After the reaction, the excess ethyl acetate was evaporated, washed three times with ether, and dried in vacuum at 8...

Embodiment 2

[0036]According to the method of Example 1, corresponding materials were prepared as catalysts for the reaction of cyclohexanone and ethylene glycol ketal. The corresponding catalytic conditions were changed, and the orthogonal test was carried out to obtain the maximum yield of cyclohexanone ethylene glycol of 85.3% under the following conditions. Cyclohexanone (9.3ml): ethylene glycol = 1:1.5, temperature: 120°C-125°C, reaction time: 75min, cyclohexane: 15ml. The catalyst was recycled four times, and the catalytic efficiency decreased from 85.3% to 81.3%, as Figure 7 . The shading rate of the product n D 20 =1.4586 (standard shading rate n D 20 = 1.4583). Infrared analysis of the product as Figure 8 , it can be seen that the hydroxyl peak completely disappears and the carbonyl peak is also very small, while the 1163cm -1 、1103cm -1 There are two large C-O-C absorption peaks, which prove that the obtained product is the cyclohexanone ethylene glycol ketal product w...

Embodiment 3

[0038] According to the method of Example 1, keep other conditions unchanged, change the amount of aluminum chloride, respectively with aluminum chloride: 1-methyl-3-butyl imidazolium salt=1:1,1.5:1,2:1, 3:1 (molar ratio) of aluminum chloride to treat the intermediate product A. The obtained catalysts were named as C1, C2, C3, and C4, respectively. And use these catalysts to catalyze the reaction of cyclohexanone and ethylene glycol ketal, the conditions are the same as in Example 2. The result is as Figure 9 , proving that the maximum catalytic effect can be achieved when aluminum chloride: 1-methyl-3-butyl imidazolium salt = 2:1, and the conversion rate of cyclohexanone increases little if the amount of aluminum chloride continues to increase.

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Abstract

The invention provides an in-situ preparation method for an acidic aluminum chlorate ionic liquid loaded SBA-15 catalyst and an application. The preparation method comprises the following steps: 1) preparing SBA-15; and 2) preparing an acidic aluminum chlorate ionic liquid loaded SBA-15 catalyst: adding SBA-15 into ethyl acetate, uniformly stirring, adding methylimidazole, heating to 80-85 DEG C and stirring; slowly adding n-butyl chloride and reacting under an inert gas condition; after the ending of reaction, evaporating the excessive ethyl acetate and washing with diethyl ether, thereby acquiring an intermediate product; adding aluminum chloride into the intermediate product, thereby acquiring the acidic aluminum chlorate ionic liquid loaded SBA-15 catalyst. According to the invention, the immobilization for the ionic liquid is performed in the manner of in-situ compounding and the purifying process of the ionic liquid is changed, so that the problems of operation difficulty, complex post-processing process and serious loss caused by excessive ionic liquid viscosity in the purifying process can be reduced.

Description

technical field [0001] The present invention relates to a kind of using mesoporous molecular sieve SBA-15 as carrier, using 1-methylimidazole, n-chlorobutane as raw material, ethyl acetate as dispersant, through the method of in-situ synthesis, directly ionic liquid chlorine The 1-methyl-3-butylimidazolium salt is supported on the mesoporous molecular sieve SBA-15, and finally treated with aluminum chloride to obtain an acidic mesoporous material. The invention belongs to the technical field of inorganic nanocomposite materials. Background technique [0002] In recent years, the research on ionic liquids has become increasingly active and has attracted widespread attention at home and abroad. Countries have successively invested a large amount of funds to fund research. Ionic liquids also have "zero vapor pressure", high thermal stability and highly designable catalytic applications, which make them replace traditional highly volatile, toxic, flammable and explosive organi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26B01J31/02C07D317/72
CPCB01J31/26B01J31/0295C07D317/72
Inventor 赵谦代黎明姜廷顺李迎迎方明兰
Owner JIANGSU UNIV
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