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Method for preparing dibutoxymethane from dimethoxymethane and n-butyl alcohol

A technology for dimethoxymethane and dibutoxymethane, which is applied in the field of preparing dibutoxymethane, can solve the problems of difficult product separation, high energy consumption, short reaction time and the like, and achieves good application prospects and simple process operation. , the effect of high selectivity

Inactive Publication Date: 2016-07-27
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acid-catalyzed method is simple to operate, short in reaction time and high in yield, but the aqueous solution of formaldehyde in this method contains a large amount of water, the product is difficult to separate, and the energy consumption is high

Method used

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  • Method for preparing dibutoxymethane from dimethoxymethane and n-butyl alcohol
  • Method for preparing dibutoxymethane from dimethoxymethane and n-butyl alcohol
  • Method for preparing dibutoxymethane from dimethoxymethane and n-butyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 30g of dimethoxymethane, 64g of n-butanol and 3g of catalysts into a 200mL autoclave. The catalysts are KAD302 (Beijing Kairui Environmental Protection), KC107 (Tianjin Yunkai), NKC-9 (Tianjin Bohong), DA -330 (Jiangsu Tehua), D009B (Dandong Pearl), Amberlyst-15 (Jiangsu Sekesaisi), D072H (Tianjin Yunkai). 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 1.

[0039] Table 1. Effects of differe...

Embodiment 2

[0043] In a 200mL autoclave, the ratio of the amount of raw material dimethoxymethane and n-butanol is 2:1, 1:1, 1:2, 1:3, 1:4 and 3gAmberlyst-15 catalyst, at room temperature Next use N 2Replace 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.

[0044] Table 2. The effect of different raw material ratios on the reaction activity and product selectivity.

[0045]

[0046] As can be seen from T...

Embodiment 3

[0048] In 200mL autoclave, add 30g dimethoxymethane, 64g n-butanol, 3gAmberlyst-15 catalyst, use N at room temperature 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, heat up under normal pressure, the stirring speed of the reactor is 500 rpm, the reaction time is 6 hours, the reaction pressure is 3.0MPa, and the reaction temperatures are 25°C, 40°C, 60°C, and 80°C respectively , 100°C, 120°C, 130°C, 140°C, 150°C, 160°C, the reaction results under different reaction temperature conditions are shown in Table 3.

[0049] Table 3. Effect of Amberlyst-15 catalyst on the reactivity and product selectivity of dimethoxymethane and n-butanol at different reaction temp...

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Abstract

The invention provides a method for preparing dibutoxymethane from dimethoxymethane and n-butyl alcohol and relates to a method for preparing dibutoxymethane. The method comprises steps as follows: dimethoxymethane and n-butyl alcohol which serve as raw materials are subjected to a reaction in the presence of catalysts, namely, liquid acid and supported liquid acid, at the reaction temperature of 0-160 DEG C under the reaction pressure of 0.1-10.0 MPa, and dibutoxymethane is produced in a high-selective manner; a resin catalyst is one or more of KAD302, KC107, NKC-9, DA-330, D009B, Amberlyst-15, D072H and the like which contain sulfonic acid functional groups; the reaction temperature is 0-160 DEG C and the reaction pressure is 0.1-10.0 MPa. According to the method, a single product is produced, the selectivity is high, required raw materials are low in price and easy to obtain, the operation is simple in the whole procedure, no chemical substances polluting the environment are produced, and the method is an environment-friendly technological process.

Description

technical field [0001] The invention relates to a method for preparing dibutoxymethane, in particular to a method for preparing dibutoxymethane by using dimethoxymethane and n-butanol as raw materials. Background technique [0002] Dibutoxymethane (also known as butyral) is an important chemical raw material, English name: dibutoxymethane, structural formula: CH 3 (CH 2 ) 3 OCH 2 O(CH 2 ) 3 CH 3 . Dibutoxymethane is a colorless transparent liquid with a mild, fruity odor. Boiling point 180°C, density 0.84g / cm 3 , Flash point 60°C. Slightly soluble in water, stable in nature, need to avoid contact with oxidants, thermal decomposition temperature is 300°C. Its application is mainly divided into two categories: one is used as a solvent, and the other is used as a reaction raw material. As a solvent, dibutoxymethane is an excellent solvent for core aggregates and binders. As a fuel additive, it can effectively reduce the emission of particles during the combustion of...

Claims

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Application Information

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IPC IPC(8): C07C41/50C07C43/30
CPCC07C41/50C07C43/30
Inventor 石磊李朕权姚杰赵佳
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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