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Magnetic solid acid catalyst, preparation method and application tehreof

A magnetic solid acid and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve environmental pollution, low yield, difficulty in separation and recovery, etc. problem, achieve the effect of reducing production cost, large specific surface area and high catalytic efficiency

Inactive Publication Date: 2011-09-14
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Traditional synthetic acetal and ketal processes mostly use homogeneous catalysts such as inorganic strong acids, such as H 2 SO 4 , HCl, H 3 PO 4 etc., there are many problems such as long catalytic reaction time, many side reactions, low yield, serious equipment corrosion, large discharge of acidic wastewater, serious environmental pollution, etc.
At present, there are also excellent catalysts for the synthesis of acetals using ion exchange resins, solid superacids, acidic molecular sieves, heteropolyacids or ionic liquids, but these catalysts have disadvantages such as low activity, difficult separation and recovery, and complicated post-treatment processes. Area for industrial use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] a. Preparation of Magnetic Nanoparticles

[0018] Take 400ml of 0.18mol / l ferric nitrate solution and 0.12mol / l ferrous sulfate solution and mix them, quickly add 96ml of ammonia water with a concentration of 25wt% at 40°C, stir and mix for 15 minutes, then raise the temperature to 60°C and stir for 5 minutes , with a stirring speed of 1000 rpm, and then magnetically separated, washed with deionized water several times, and vacuum-dried at 80°C for 5 hours to obtain a superparamagnetic Fe 3 o 4 Nanoparticles.

[0019] b. Modification of magnetic nanoparticles

[0020] Take the magnetic Fe prepared above 3 o 4 Add 6g of nanoparticles into a solution of 29.8g 3-chloropropyltrimethoxysilane, 47.2g triphenylphosphine and 416g toluene, stir and disperse at a speed of 1000 r / min, reflux for 48 hours, and perform magnetic separation after the reaction. isolated magnetic Fe 3 o 4 The nanoparticles were washed with absolute ethanol several times and then dried in vacuum a...

Embodiment 2

[0026] a. Preparation of Magnetic Nanoparticles

[0027] Get 500ml of ferric nitrate solution of 0.18mol / l and 500ml of ferrous sulfate solution of 0.12mol / l and mix, add 120ml of 25wt% ammonia water rapidly at 40°C, stir at 1000rpm for 15 minutes and then heat up to 60°C ℃ and then stirred for 5 minutes, then magnetically separated and washed with deionized water for several times, and vacuum-dried at 80℃ for 5 hours to obtain superparamagnetic magnetic Fe 3 o 4 Nanoparticles.

[0028] b. Modification of magnetic nanoparticles

[0029] Take the magnetic Fe prepared above 3 o 4 Add 4g of nanoparticles into a solution of 29.8g 3-chloropropyltrimethoxysilane, 47.2g triphenylphosphine and 416g toluene, stir and disperse at a speed of 1000 rpm, reflux for 48 hours, and magnetically separate after the reaction. Magnetic Fe 3 o 4 The nanoparticles are washed with absolute ethanol several times and then vacuum-dried at 80°C for 10 hours to prepare the magnetic nanoparticles mo...

Embodiment 3

[0035] The magnetic solid acid catalyst prepared in above-mentioned embodiment 1 is used for synthesizing benzaldehyde ethylene glycol acetal reaction, in 100ml reactor, add 3.18g benzaldehyde successively, 5.58g ethylene glycol, 0.06g magnetic solid acid catalyst, 15.6 g cyclohexane, refluxing cyclohexane with water at 82°C, stirred and reacted at 800 rpm for 0.5h, then cooled to room temperature, magnetically separated the magnetic solid acid catalyst and then carried out atmospheric distillation, collected at 80-82°C The distillate reclaims cyclohexane, and then collects the distillate that boiling range is 220~228 ℃, promptly makes benzaldehyde ethylene glycol acetal, and its yield is 58.5%, and the catalyst after separation can be deionized water washing, drying recycle.

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PUM

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Abstract

The invention discloses a magnetic solid acid catalyst, a preparation method and application thereof, and is characterized in that the catalyst takes magnetic nanometer particles as carrier and is prepared sequentially through triphenylphosphine-methoxy silane ionic liquid modification and gaseous phase sulfonation, the catalyst is used for the acetal (ketone) synthesis catalytic reaction, the weight ratio of the catalyst, the benzaldehyde, glycol and water aqua is 0.02-0.08:1.59-6.36:2.79-11.2. compared with prior art, the invention has simple method, convenient preparation, high catalytic efficiency, good selectivity, even distribution of magnetic nanometer particles, high specific surface area, easy separation with products, can be used repeatedly and further reduces the production cost.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a magnetic solid acid catalyst and its preparation method and application. Background technique [0002] Acetal (ketone) is a class of important compounds, often used in the protection of aldehydes or ketones, is an important intermediate in the chemical industry, and even as a solvent for special reactions, it has a floral and fruity aroma that is superior to the parent carbonyl compound. In recent years, As a new high-grade spice, it is widely used in daily chemical and food industries. [0003] Traditional synthetic acetal and ketal processes mostly use homogeneous catalysts such as inorganic strong acids, such as H 2 SO 4 , HCl, H 3 PO 4 etc., there are many problems such as long catalytic reaction time, many side reactions, low yield, serious equipment corrosion, large acid wastewater discharge, and serious environmental pollution. At present, there are also ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/24C07D317/12
CPCY02P20/584
Inventor 单永奎孔爱国王平王文娟朱海燕单冲冲张新华
Owner EAST CHINA NORMAL UNIV