Method for preparing sulfonic acid group-modified mesoporous material-loaded heteropolyacid catalyst and application thereof during esterification reaction
A technology for loading heteropolyacids and mesoporous materials, which is applied in catalytic reactions, preparation of organic compounds, preparation of carboxylate esters, etc., can solve the problems of easy dissolution and desorption of active components, and achieves simple preparation process, strong acidity, and large pores. the effect of
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[0025] Example 1
[0026] Dissolve 4g P123 in 120g 2mol / L hydrochloric acid solution, stir at 35°C for 3h to completely dissolve the template; heat up to 40°C, and add 8.42g ethyl orthosilicate (TEOS) dropwise to the above solution, Continue to stir for 60 minutes; add 3-mercaptopropyltrimethoxysilane (MPTMS), phosphotungstic acid (HPW) and hydrogen peroxide solution (30wt%) to the above solution in sequence, the molar component α=n(MPTMS) / n(MPTMS) +TEOS)=0.1, β=n(H 2 O 2 ) / n(MPTMS)=9, mass component γ=m(HPW / m(TEOS)=0.1, under nitrogen protection, continue to stir for 20h, then crystallize at 100℃ for 24h, filter, wash with ethanol and water solution respectively , Vacuum drying at 80°C for 12h, ethanol Soxhlet extraction for 24h, vacuum drying at 80°C for 12h, the resulting sample is denoted as HPW-SBA-15-SO 3 H (α=0.1, β=9, γ=0.1).
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[0027] Example 2
[0028] Application of a sulfonic acid group modified mesoporous material supported heteropolyacid catalyst in esterification reaction. Weigh 1.23g of sulfonic acid group modified ordered mesoporous material supported heteropoly acid catalyst HPW-SBA-15-SO 3 H (α=0.1, β=9, γ=0.1), weigh 8.21g cyclohexene and 13.81g formic acid into a 50ml three-necked flask, stir at 80℃ for 6h, cool to room temperature, use gas chromatography Analyzing the components of the reaction solution, the conversion of cyclohexene was 82%, and the selectivity of cyclohexyl formate was 99%.
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[0029] Example 3
[0030] Load the recycled sulfonic acid group modified mesoporous material with heteropolyacid catalyst HPW-SBA-15-SO 3 H (α=0.1, β=9, γ=0.1) was dried in vacuum at 100℃ for 12h, cooled to room temperature, weighed 1.23g, then weighed 8.21g cyclohexene and 13.81g formic acid into a 50ml three-necked flask, After stirring for 6 hours at 80°C and cooling to room temperature, the components of the reaction solution were analyzed by gas chromatography, and the conversion rate of cyclohexene was 83% and the selectivity of cyclohexyl formate was 99%.
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