Method for preparing diethoxymethane

A technology of diethoxymethane and dimethoxymethane, which is applied in the field of preparing diethoxymethane, can solve the problems of low output, high dosage, and limited output, and achieve less side reactions, good selectivity, and high product quality. simple effect

Inactive Publication Date: 2016-05-18
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The amount of dimethyl sulfoxide is large, the catalyst is unstable to acid and the yield is not high, which is not conducive to large-scale production
This method chloramphenicol by-product method is not conducive to large-scale production because of limited output

Method used

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  • Method for preparing diethoxymethane
  • Method for preparing diethoxymethane
  • Method for preparing diethoxymethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 30g of dimethoxymethane, 40g of ethanol and 3g of catalyst into a 200mL autoclave. The catalysts are sulfuric acid with a mass fraction of 98% (Shandong Jiuding), hydrochloric acid with a mass fraction of 38% (Hebei Yongfei), mass Nitric acid with a fraction of 50% (Hebei Yongfei), hydrofluoric acid with a mass fraction of 45% (Shandong Jiuding). use N 2 Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empty the gas in the kettle. Under the condition of ensuring no air leakage, the reaction was heated and heated. The stirring speed of the reactor was 500 rpm, the reaction temperature was 120 ° C, the reaction pressure was 3.0 MPa, and the reaction time was 6 hours. The results of controlling the catalyst type are shown in Table...

Embodiment 2

[0046] In a 200mL autoclave, the ratio of the amount of the raw material dimethoxymethane and ethanol is 2:1, 1:1, 1:2, 1:3, 1:4 and 3g hydrofluoric acid catalyst, at room temperature Next use N 2 Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empty the gas in the kettle. Under the condition of ensuring no air leakage, the temperature was raised under normal pressure, the stirring speed of the reactor was 500 rpm, the reaction temperature was 120°C, the reaction pressure was 3.0 MPa, and the reaction time was 6 hours. The results of controlling the ratio of raw materials are shown in Table 2.

[0047] Table 2. The effect of different raw material ratios on the reaction activity and product selectivity.

[0048]

[0049] As can be se...

Embodiment 3

[0051] Preparation of sulfuric acid with a mass fraction of 20% H 2 SO 4 / SiO 2 Supported catalyst, the preparation process is as follows: first put silica into a muffle furnace and roast at 500°C for 4 hours to remove the water adsorbed in silica, take 80g of silica after roasting as carrier; take 20g of 98% concentrated Sulfuric acid was diluted into 49% sulfuric acid solution, and 40g of the sulfuric acid solution was impregnated into 80g of silica carrier pores in an ultrasonic environment; ℃ roasting for 3 hours to produce H 2 SO 4 / SiO 2 supported catalyst. In 200mL autoclave, add 30g dimethoxymethane, 40g ethanol, 3gH 2 SO 4 / SiO 2 catalyst, at room temperature with N 2 Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empt...

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Abstract

The invention provides a method for preparing diethoxymethane, relating to a method for preparing methane. The method comprises the following step: by using dimethoxymethane and ethanol as raw materials, reacting at 0-160 DEG C under the reaction pressure of 0.1-10.0 MPa by using a liquid acid and a supported liquid acid as catalysts to generate diethoxymethane. The liquid acid catalyst is one or more of inorganic acids from sulfuric acid, hydrochloric acid, nitric acid and hydrofluoric acid. The mass percent of the sulfuric acid catalyst is 0-98%, the hydrochloric acid catalyst is a 0-38% hydrogen chloride water solution, the mass percent of the nitric acid catalyst is 0-95%, and the mass percent of the hydrofluoric acid catalyst is 0-55%. The reaction temperature is 0-160 DEG C, and the reaction pressure is 0.1-10.0 MPa. The method has the advantages of single product and high selectivity, and has favorable application prospects. The required raw materials are cheap and accessible, and the whole process is simple to operate and can not generate the environment-polluting chemical substances. Thus, the method belongs to an environment-friendly technical route.

Description

technical field [0001] The invention relates to a method for preparing methane, in particular to a method for preparing diethoxymethane. Background technique [0002] Diethoxymethane is an important chemical raw material, English name: dietoxymethan, abbreviated as DEM, structural formula: CH 3 CH 2 OCH 2 OCH 2 CH 3 . Diethoxymethane is a colorless, clear and volatile liquid with an odor similar to ether, with a melting point of -66.5°C and a boiling point of 89°C. It is soluble in benzene, ether, and ethanol, and slightly soluble in water. Diethoxymethane has the properties of low toxicity, high oxygen content, both hydrophilic and lipophilic properties, strong solubility, small surface tension and low heat of vaporization. Its application is mainly divided into two categories: one is used as a solvent, and the other is used as a reaction reagent. As a solvent, diethoxymethane is an aprotic solvent and can be used in some water-sensitive reactions without drying. Di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/30C07C41/50
CPCC07C41/50C07C43/30
Inventor 石磊赵佳姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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