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Preparation method of heteropolyacid ionic liquid-loaded Sn-SBA-15 catalyst and application of catalyst

A technology of sn-sba-15 and ionic liquid, which is applied in the field of preparation of Sn-SBA-15 catalyst, can solve problems such as catalytic activity to be optimized, and achieve the effects of improving utilization rate, overcoming recovery difficulties, and good thermal stability

Active Publication Date: 2019-01-11
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the pure silica molecular sieve has few defects in the framework network, and the catalytic activity needs to be optimized.

Method used

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  • Preparation method of heteropolyacid ionic liquid-loaded Sn-SBA-15 catalyst and application of catalyst
  • Preparation method of heteropolyacid ionic liquid-loaded Sn-SBA-15 catalyst and application of catalyst
  • Preparation method of heteropolyacid ionic liquid-loaded Sn-SBA-15 catalyst and application of catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Firstly, the heteropolyacid ionic liquid and Sn-SBA-15 were prepared respectively, and the ionic liquid was combined with the carrier by impregnation method to obtain the supported heteropolyacid ionic liquid catalyst. The specific method is as follows:

[0037] 1. Preparation of Sn-SBA-15

[0038] Weigh 1.5g of P123 and dissolve in 70ml of deionized water, add 1.18g of NaCl solid, and stir mechanically at 35-40°C until clear. Slowly drop 4.2g of TEOS at 35°C for 4h in advance. Add 0.35g of SnCl 4 ·5H 2 O The white solid (Si / Sn=20) continued to be mechanically stirred for 24h, forming a white cloudy liquid. The reaction mixture was transferred to polytetrafluoroethylene for hydrothermal crystallization for 24h. Suction filtration, washing and drying. Put it in a tube furnace, raise the temperature to 500°C at a heating rate of 1°C / min, and calcine in air for 12 hours to remove the template agent, and obtain the Sn-SBA-15 mesoporous material.

[0039] Step 2. Prep...

Embodiment 2

[0050] According to the reaction conditions of Step 1 and Step 2 in Example 1, keep the other conditions of Step 3 unchanged, and change the reflux reaction temperature to 60°C.

[0051] Gained catalyst is applied in the esterification reaction of acetic acid and benzyl alcohol, reaction temperature is 100 ℃, acetic acid 6.0g, benzyl alcohol 8.1g, catalyzer 0.4g, the relation of acetic acid conversion rate and time is as follows Figure 7 As shown, the reaction can reach equilibrium in 5h, and the maximum conversion rate of acetic acid can reach 85.68%. It can be seen that when the reflux reaction temperature is 60°C, the catalytic activity of the obtained catalyst is slightly lower than that of the catalyst prepared at 50°C. Considering the energy loss problem, we take the reflux reaction temperature as 50°C. Example 3

Embodiment 3

[0052] After determining the ideal temperature for the composite of the carrier and the ionic liquid, continue to explore the influence of the doping amount of the ionic liquid in the carrier Sn-SBA-15 on the catalyst activity. According to the method of steps 1 and 2 in Example 1, keep other conditions unchanged. change, respectively by m SWIL / m Sn-SBA-15 =0.8, 1, 1.2, 1.4 mass ratio to treat the catalyst, and the obtained catalysts are respectively named as C1, C2, C3, and C4. And use these catalysts to catalyze the esterification reaction of acetic acid and benzyl alcohol, the conditions are the same as in Example 1, and the conversion rate of acetic acid is as follows: Figure 8 As shown, prove that the equivalent m SWIL / m Sn-SBA-15 =1.2, the conversion of acetic acid reaches the maximum. Continuing to increase the doping amount of ionic liquid, the conversion rate decreased slightly.

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Abstract

The invention belongs to the field of inorganic nanometer composite materials and discloses a preparation method of a heteropolyacid ionic liquid-loaded Sn-SBA-15 catalyst and application of the catalyst. The preparation method comprises the following steps: preparing a Sn-SBA-15 mesoporous molecular sieve; preparing heteropolyacid ionic liquid; and preparing the heteropolyacid ionic liquid-loadedSn-SBA-15 catalyst. According to the preparation method, the ionic liquid bound with organic cations and heteropoly anions is loaded on a metal atom modified mesoporous material, and the heteropolyacid ionic liquid is bound with a mesoporous material Sn-SBA-15, so that the advantages of the heteropolyacid ionic liquid and the mesoporous material are integrated, the disadvantages of the heteropolyacid ionic liquid and the mesoporous material are overcome, the problem that the ionic liquid is difficult to be treated due to high viscosity is solved, and the acidity, activity and repeated utilization rate of an acid catalyst are greatly increased.

Description

technical field [0001] The invention belongs to the field of inorganic nanocomposite materials, and relates to a preparation method and application of a Sn-SBA-15 catalyst supported by a heteropolyacid ionic liquid. Background technique [0002] Ionic liquids are salts composed of organic cations and inorganic or organic anions, which are in a liquid state at or near room temperature. Because of its low vapor pressure, wide liquid range, good electrical and thermal conductivity, and adjustable solubility, it fully meets the requirements of green chemistry and can gradually replace traditional inorganic acids, showing good application prospects. Taking advantage of the unique advantage that ionic liquids have the configurability of anions and cations, the acidity of ionic liquids can be adjusted by changing the types of anions and cations. [0003] Heteropolyacids, as highly active, multifunctional, and environmentally friendly inorganic acids, have received more and more at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/34B01J27/188C07C67/08C07C69/157
CPCB01J27/188B01J31/34B01J2231/49C07C67/08C07C69/157
Inventor 姜廷顺谢英杰方明兰
Owner JIANGSU UNIV
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