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A kind of method for preparing dibutoxymethane with dimethoxymethane and n-butanol as raw material

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

Inactive Publication Date: 2018-06-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of method for preparing dibutoxymethane with dimethoxymethane and n-butanol as raw material
  • A kind of method for preparing dibutoxymethane with dimethoxymethane and n-butanol as raw material
  • A kind of method for preparing dibutoxymethane with dimethoxymethane and n-butanol as raw material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 30 g of dimethoxymethane, 64 g of n-butanol and 3 g of catalysts into a 200 mL autoclave. The catalysts are KAD302 (Beijing Kairui Environmental Protection), KC107 (Tianjin Yunkai), NKC-9 (Tianjin Bo Hong), DA-330 (Jiangsu Tehua), D009B (Dandong Pearl), Amberlyst-15 (Jiangsu Sekesaisi), D072H (Tianjin Yunkai). use N 2 Under the condition of 1.0 MPa, replace the air in the kettle three times, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. 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 types are shown in Table 1.

[0041] Table 1. Effects of d...

Embodiment 2

[0045] In 200 mL autoclave, the ratio of the amount of substance that adds raw material dimethoxymethane and n-butanol is 2:1, 1:1, 1:2, 1:3, 1:4 and 3 g Amberlyst-15 catalyst, at room temperature with N 2Under the condition of 1.0 MPa, replace the air in the kettle three times, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Under the condition of ensuring no air leakage, heating was carried out 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.

[0046] Table 2. The effect of different raw material ratios on the reaction activity and product selectivity.

[0047]

[0048] As c...

Embodiment 3

[0050] Add 30 g of dimethoxymethane, 64 g of n-butanol, and 3 g of Amberlyst-15 catalyst in a 200 mL autoclave, and use N 2 Under the condition of 1.0 MPa, replace the air in the kettle three times, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. 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 3.0 MPa, and the reaction temperatures are 25 ℃, 40 ℃, 60 ℃, 80 ℃ 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.

[0051] Table 3. Effect of Amberlyst-15 catalyst on the reactivity and product selectivity of dimethoxymethane and n-butanol at different react...

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Abstract

A method for preparing dibutoxymethane using dimethoxymethane and n-butanol as raw materials, relates to a method for preparing dibutoxymethane, the method includes the following process: using dimethoxymethane and n-butanol as raw materials , using liquid acid and supported liquid acid as catalysts, reacting at a reaction temperature of 0-160°C and a reaction pressure of 0.1-10.0 MPa to generate dibutoxymethane with high selectivity; the resin catalyst is KAD302 containing sulfonic acid functional groups, One or more resin catalysts such as KC107, NKC‑9, DA‑330, D009B, Amberlyst‑15, D072H; the reaction temperature is 0-160°C, and the reaction pressure is 0.1-10.0 MPa. The product of the method of the invention is relatively single, the selectivity is high, the required raw materials are cheap and easy to obtain, the whole process is simple to operate, no chemical substances polluting the environment are produced, and it belongs to an environmentally friendly process path.

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 smell. 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 ℃. 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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