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A kind of method for preparing acrolein

A technology of acrolein and glycerin, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of easy carbon deposition and deactivation of catalysts, low yield of acrolein, high reaction temperature, etc. Possibility, increase of reaction yield, effect of mild reaction conditions

Active Publication Date: 2020-12-01
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the glycerin dehydration catalytic system is mainly a gas phase and a liquid phase system. The gas phase has the advantages of high yield and continuous production. frequent challenges
Glycerol can also be converted into acrolein at a lower temperature (lower than the boiling point of glycerol). At this time, glycerin is in a liquid state, and the liquid phase reaction of glycerol to generate acrolein has the advantages of low reaction temperature and mild conditions, but in the liquid phase reaction The yield of acrolein from glycerol is low, and a large amount of humus is produced as a by-product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Mix 5ml of glycerin, 5ml of water, and 0.1g of concentrated sulfuric acid thoroughly, add 0.5g of silicon dioxide powder with a contact angle of 95 degrees and 5ml of decahydronaphthalene, and stir for two minutes under mechanical stirring at 2000 rpm to make a uniform Water-in-oil emulsion; heat the emulsion to 180°C, and collect the acrolein formed by the reaction until no liquid condenses and drops out. After nuclear magnetic detection, the conversion rate of glycerin reached 92%. The collected liquid was analyzed and the yield of acrolein was 25%. The reaction system was centrifuged, the supernatant was poured out and recovered by distillation to obtain decalin, and the paste Dissolve the substance in hot water, filter, wash the filter cake 3-5 times, dry it, and reuse it as emulsifier silicon dioxide powder.

Embodiment 2

[0033] Mix 4ml of glycerin, 6ml of water, and 0.5g of concentrated hydrochloric acid thoroughly, add 0.1g of silicon dioxide powder with a contact angle of 150 degrees and 8ml of decahydronaphthalene, and stir for 10 minutes under mechanical stirring at 1600 rpm to make a uniform Water-in-oil emulsion; heat the emulsion to 140°C, and collect the acrolein formed by the reaction until no liquid condenses and drops out. After nuclear magnetic detection, the conversion rate of glycerin reached 94%. The collected liquid was analyzed and the yield of acrolein was 28%. The reaction system was centrifuged, the supernatant was poured out and recovered by distillation to obtain decahydronaphthalene. The liquid-like substance is dissolved in hot water, filtered, the filter cake is washed 3-5 times, dried, and can be reused as an emulsifier.

Embodiment 3

[0035] Mix 3ml of glycerin, 7ml of water, and 0.8g of concentrated phosphoric acid thoroughly, add 0.2g of titanium dioxide powder with a contact angle of 105°C and 10ml of Fischer-Tropsch wax with a boiling range of 180-200°C, and stir under mechanical stirring at 800 rpm for 30 Minutes to make a uniform water-in-oil emulsion; heat the emulsion to 160°C, and collect the acrolein generated by the reaction until no liquid condenses and drops out. After nuclear magnetic detection, the conversion rate of glycerin reached 90%. The collected liquid was analyzed and the yield of acrolein was 33%. The reaction system was centrifuged, the supernatant was poured out and recovered by distillation to obtain decahydronaphthalene. The liquid-like substance is dissolved in hot water, filtered, the filter cake is washed 3-5 times, dried, and can be reused as an emulsifier.

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Abstract

The invention discloses a method for preparing acrolein. The method includes the steps: sufficiently and uniformly mixing catalysts, glycerin and water to prepare glycerin water catalysis reaction solution; adding low-pole organic solvents and Pickering emulsifying agents into the glycerin water catalysis reaction solution, and stirring and emulsifying mixture to prepare a Pickering emulsion reaction system; heating the Pickering emulsion reaction system to reach the reaction temperature, condensing and collecting acrolein generated by reaction, recycling the acrolein, and performing catalyticreaction on the recycled acrolein. The method has the advantages of low reaction temperature, high acrolein yield and good reaction selectivity.

Description

technical field [0001] The invention relates to a method for preparing acrolein by dehydrating glycerin in a water-in-oil Pickering emulsion system. [0002] technical background [0003] Acrolein is an important chemical intermediate, which can be used to synthesize important chemical products such as picoline, glutaraldehyde, acrylic acid, etc. These chemicals can be widely used in the fields of medicine, food and cosmetics. At present, the main source of acrolein is prepared by catalytic oxidation of propylene with air and water vapor. The main sources of propylene are the petroleum industry and the coal chemical industry. With the serious shortage of petrochemical resources, the output of propylene is in short supply and the price is expensive. Therefore, people wish to find a raw material for the production of acrolein with a wider source. Biomass resources are the only renewable carbon-containing resources on the earth, and have the potential to supplement and replace...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/22C07C45/52
CPCC07C45/52C07C47/22
Inventor 邓天昇张姣姣侯相林柴琳王英雄齐永琴贾时宇
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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