Method for preparing diethoxymethane by using active carbon supported solid acid catalyst

A technology of immobilizing acid and diethoxymethane on activated carbon, which is applied in chemical instruments and methods, preparation of organic compounds, chemical recovery, etc., can solve problems such as unfavorable large-scale production, difficulty in separation and recovery, and environmental pollution, and achieve Easy to separate, economical to prepare, and less corrosive to equipment

Active Publication Date: 2012-11-28
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Dimethyl sulfoxide is unstable to acid, and it will be decomposed by heating to generate formaldehyde, which will undergo addition reaction with ethanol to obtain diethoxymethane, which will produce SO as a by-product. 2 , which pollutes the environment and thus is not conducive to large-scale production
The classi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] Preparation of activated carbon-supported acid catalyst: wash 50 g of activated carbon with distilled water, dry it, activate it at 120 °C for 2 h, weigh 30 g of pretreated activated carbon and immerse it in 20 times the mass concentration of 60 mass% sulfuric acid, and immerse it at 120 °C under stirring 4h, suction filtration, washing to neutrality, drying at 120 °C in an oven to constant weight, and cooling to obtain 30 g of an activated carbon-supported acid catalyst with an acid loading of 15% by mass, for use.

example 2

[0024] Preparation of activated carbon-supported acid catalyst: wash 50 g of activated carbon with distilled water, dry it, activate it at 120 °C for 2 h, weigh 40 g of pretreated activated carbon and immerse it in 20 times the mass concentration of 98 mass% sulfuric acid, and immerse it at 120 °C under stirring 4h, suction filtration, washing to neutrality, drying at 120 °C in an oven to constant weight, and cooling to obtain 40 g of activated carbon-immobilized acid catalyst with an acid immobilization capacity of 22% by mass, for use.

example 3

[0026] In a 500ml three-necked flask equipped with a thermometer, a magnetic stirrer, a φ20×700 packed tower and a rectifying head, the concentration of 37% by mass formaldehyde solution 60g, 136g of dehydrated alcohol, and the activated carbon prepared by Example 1 were respectively added to immobilize H 2 SO 4 Catalyst 15.7g, stir and heat up until the tower kettle is in a boiling state, the total reflux to the top of the tower temperature is stable at 74 ° C, adjust the reflux ratio to 1:1, and collect the fraction with a top temperature of 74 to 76 ° C; as the top temperature rises, gradually Increase the reflux ratio. When the top temperature reaches 76 °C, the reflux ratio is increased to 4:1; when the top temperature is greater than 76 °C, the reflux ratio is controlled to 1:1, and the fractions with the top temperature less than 80 °C are switched and collected. After the reaction is completed, the temperature is lowered. . Collect 99g of diethoxymethane fraction, gas...

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Abstract

The invention relates to a method for preparing diethoxymethane by using an active carbon supported solid acid catalyst. The method is characterized in that formaldehyde and ethanol are used as raw materials and reacted under normal pressure under the action of a solid acid catalyst at the temperature of 70 to 100 DEG C, the reflux ratio is controlled to be 1:1-4:1, distillate of 74 to 76 DEG C is collected on the top of a tower, and the diethoxymethane product is obtained; after the aqueous solution in a tower kettle is filtered, the solid acid catalyst is recycled in the kettle; the molar ratio of the formaldehyde to the ethanol is 1:2-1:5, the formaldehyde raw material is a formaldehyde solution at the concentration of over 37 weight percent, and the ethanol raw material is absolute ethanol or an ethanol solution at the concentration of 75-95 weight percent; the solid acid catalyst is the active carbon supported solid acid catalyst, the active acid ingredient is sulfuric acid, and the acid solid capacity is 15 to 25 mass percent; and the consumption of the solid acid catalyst is 0.3 to 10 percent of the total mass of the reactants. The method has the advantages that the catalyst is economic in preparation, easy to separate from the product and low in equipment corrosion, and the waste catalyst is easy and convenient to reclaim and treat.

Description

technical field [0001] The invention relates to a method for preparing diethoxymethane by an activated carbon-supported acid catalyst; diethoxymethane is also called formaldehyde diethyl acetal, and the structural formula is: CH 3 CH 2 OCH 2 O CH 2 CH 3 ; belongs to the technical field of organic chemical industry. Background technique [0002] Diethoxymethane, is a colorless transparent liquid, the molecular formula is C 5 H 12 O 2 , the molecular weight is 104.15, the pure product has a boiling point of 88 °C, a melting point of -66.50 °C, and a solubility of 9% (wt) in water at 20 °C. It has good properties and can be used in organic synthesis and extraction, dilution, recrystallization and other solvents. [0003] As a solvent in organic synthesis, diethoxymethane is an aprotic solvent with low affinity for water, insoluble in water and non-hygroscopic, so it can be directly used in some water-repellent compounds without further drying. Sensitive reactions such...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/56
CPCY02P20/584
Inventor 朱新宝李迪王筠翔王传柱彭春睿胡明华
Owner NANJING FORESTRY UNIV
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