Preparation method of dibutoxy methane

A technology of dibutoxymethane and formaldehyde is applied in the field of preparation of industrial grade dibutoxymethane, which can solve the problems of high equipment requirements, cumbersome operation, influence on product stability, etc., and achieves low equipment corrosion, easy separation, Handling easy effects

A technology of dibutoxymethane and formaldehyde is applied in the field of preparation of industrial grade dibutoxymethane, which can solve the problems of high equipment requirements, cumbersome operation, influence on product stability, etc., and achieves low equipment corrosion, easy separation, Handling easy effects

CN102241571AActive Publication Date: 2011-11-16NANJING FORESTRY UNIV +1
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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] Preparation of activated carbon-supported acid catalyst: wash 50g of activated carbon with distilled water, dry it, activate it at 120°C for 2h, weigh 15g of pretreated activated carbon and immerse it in sulfuric acid with a mass concentration of 20 times of 60% by mass, and impregnate it at 120°C under stirring After 4 hours, filter with suction, wash until neutral, dry in an oven at 120°C to constant weight, and obtain 15 g of activated carbon-immobilized acid catalyst with an acid-immobilized capacity of 15% by mass after cooling, and set aside.

example 2

[0026] Wash 50g of activated carbon with distilled water, dry it, activate it at 120°C for 2h, weigh 15g of pretreated activated carbon and immerse it in 20 times the mass concentration of 98% by mass sulfuric acid, immerse it under stirring at 120°C for 4h, filter it with suction, and wash to medium properties, dried in an oven at 120°C to constant weight, and after cooling, 15 g of activated carbon-supported acid catalyst with an acid-loaded capacity of 22% by mass was obtained for future use.

example 3

[0028] Into a 500 mL three-neck flask equipped with a thermometer, a constant speed stirrer, and a water separator (with a condenser on the top), 78.4 g of a formaldehyde solution with a concentration of 37% by mass, 187.4 g of n-butanol, and 1.3 g of HZSM-5 catalyst were respectively added. , stirred and heated up, the initial reaction temperature was 90 °C, and the reaction was continuously raised until the reaction was completed at 130 °C, and the reaction time was 3 h; during the reaction process, the raw materials and by-product water were continuously separated from the reaction system through a water separator. After the reaction was completed, the reactant was filtered to obtain 196.5 g of a colorless crude product of dibutoxymethane, the content of dibutoxymethane was 58.7% according to gas chromatography, and the content of n-butanol was 33.3%; of dibutoxymethane.

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Abstract

The invention relates to a preparation method of dibutoxy methane. The preparation method is characterized by comprising the following step of: undergoing a normal-pressure gap type aldol condensation reaction on formaldehyde and n-butyl alcohol under the action of a solid acid catalyst by taking n-butyl alcohol as an azeotropic dehydrating agent in a reactor with a stirrer, a condenser and a water knockout vessel to obtain the dibutoxy methane, wherein the molar ratio of the formaldehyde to the n-butyl alcohol is 1:2-1:4, the concentration of a formaldehyde solution is more than or equal to 25 percent by mass, the reaction temperature is 60-140 DEG C, the reaction time is 0.5-8 hours, the solid catalyst is an HZSM-5 molecular sieve or an active carbon immobilized sulfuric acid catalyst, the active ingredient of the active carbon immobilized sulfuric acid catalyst is sulfuric acid, the immobilized quantity of acid is 15-25 percent by mass, and the using amount of the solid acid catalyst is 0.1-8 percent of the total mass of reactants. The method has the advantages of easiness in separation of the solid acid catalyst from a product, small corrosion to equipment and catalyst recyclability, and is a novel, efficient and environmentally-friendly production method.

Description

technical field [0001] The present invention relates to a preparation method of industrial grade dibutoxymethane. Dibutoxymethane is also known as formaldehyde dibutylacetal, and its structural formula is: CH 3 (CH 2 ) 3 OCH 2 O(CH 2 ) 3 CH 3 . It belongs to the field of organic chemical technology. Background technique [0002] Dibutoxymethane is a colorless transparent liquid with a mild, fruity odor. Boiling point 180 ℃, density 0.84 g / cm 3 , flash point 60 ℃. Slightly soluble in water, stable in nature, need to avoid contact with oxidants, thermal decomposition temperature is 300 ℃. [0003] Dibutoxymethane can be used as a good solvent for casting core aggregates and binders, and can also effectively reduce the emission of particles during the combustion of diesel fuel, and can increase the cetane number of diesel. Dibutoxymethane is also used as a raw material for the preparation of polyoxymethylene dialkyl ether, a diesel additive. [0004] Dibutoxymethan...

Claims

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Application Information

Patent Timeline
16 Nov 2011
Publication
CN102241571A
IPC
C07C43/30; C07C41/56
CPC
Y02P20/584
Inventors
朱新宝; 彭春睿