Method for synthesizing PODE through condensation, oxidation, polycondensation and etherification of methyl alcohol

A polyoxymethylene dimethyl ether, chemical synthesis technology, applied in the direction of chemical instruments and methods, preparation of organic compounds, carbon-based compounds, etc., can solve the problems of reducing product yield, product separation difficulties, etc., to improve the purity And yield, reduce hydrolysis reaction, strong selectivity effect

Active Publication Date: 2014-09-24
XIAN SHANGHUA TECH DEV CO LTD
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The boiling point and PODE of these hydrolysis products 3-8 approach, PODE 3-8 The hydrolysis

Method used

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  • Method for synthesizing PODE through condensation, oxidation, polycondensation and etherification of methyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 1

[0042] Such as figure 1 As shown, the synthesis method of this embodiment is:

[0043] Step 1. Methanol condensation to prepare methylal: Mix methanol and dilute formaldehyde with a mass concentration of 5% according to the molar ratio of methanol to formaldehyde at a ratio of 2.0:1 and then send them to the reactor 1 filled with catalyst for condensation reaction. The reaction temperature of the condensation reaction is 90°C, the reaction pressure is 8.0MPa, and then the materials after the condensation reaction are sent to the first reactive distillation tower 2. The number of sieve plates on the top of the first reactive distillation tower 2 is 30 , The number of sieve plates at the bottom of the tower is 30, the number of layers of the packed bed is 8, and the top pressure of the first reactive distillation tower 2 is controlled to 50kPa, the top temperature is 47℃, the bottom temperature is 115℃, reflux The ratio is 3.0. The materials after the condensatio...

Example Embodiment

[0051] Example 2

[0052] Such as figure 1 As shown, the synthesis method of this embodiment is:

[0053] Step 1. Methanol condensation to prepare methylal: Mix methanol and dilute formaldehyde with a mass concentration of 20% in a ratio of 3.0:1 in the molar ratio of methanol to formaldehyde, and then send them to reactor 1 filled with catalyst for condensation reaction. The reaction temperature of the condensation reaction is 70°C, the reaction pressure is 5.0MPa, and then the materials after the condensation reaction are sent to the first reactive distillation tower 2, and the number of sieve plates on the top of the first reactive distillation tower 2 is 20 , The number of sieve plates at the bottom of the tower is 20, the number of packed beds is 5, and the top pressure of the first reactive distillation tower 2 is controlled to 30kPa, the top temperature is 45℃, the bottom temperature is 108℃, and the reflux The ratio is 2.0. The materials after the condensation reaction in...

Example Embodiment

[0061] Example 3

[0062] Such as figure 1 As shown, the synthesis method of this embodiment is:

[0063] Step 1. Methanol condensation to prepare methylal: Mix methanol and dilute formaldehyde with a mass concentration of 45% according to the ratio of methanol to formaldehyde at a molar ratio of 3.5:1, and then send them to reactor 1 filled with catalyst for condensation reaction. The reaction temperature of the condensation reaction is 60°C, the reaction pressure is 2.0MPa, and then the materials after the condensation reaction are sent to the first reactive distillation tower 2. The number of sieve plates on the top of the first reactive distillation tower 2 is 5 , The number of sieve plates at the bottom of the tower is 5, the number of packed beds is 2, and the top pressure of the first reactive distillation tower 2 is controlled to 5kPa, the top temperature is 42.3°C, the bottom temperature is 100°C, and the reflux ratio Is 1.0, the material after the condensation reaction ...

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Abstract

The invention discloses a method for synthesizing PODE through condensation, oxidation, polycondensation and etherification of methyl alcohol. The method includes the steps that firstly, methylal with the mass purity of 85%-99.9% is prepared through a reaction of the methyl alcohol and diluted methanal; secondly, the methylal and air are catalyzed and oxidized by iron-molybdenum catalysts to prepare methanal with the mass purity of not less than 70%; thirdly, the methanal is subjected to polycondensation and then is refined to obtain triformol with the mass purity of not less than 99.9%; fourthly, the methylal and the triformol are subjected to etherification, reactive distillation and dehydration and are refined to obtain PODE3-8 with the mass purity of over 99%. By the adoption of the method, the single-pass yield of the PODE is increased from 40%-50% to 95%, the yield of the PODE3-8 is increased from 20% to 90%, product distribution is more reasonable, and the product purity is improved from 50% to 99%. The PODE is wide in application prospect and remarkable in economic, social and environmental benefit.

Description

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Claims

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Application Information

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Owner XIAN SHANGHUA TECH DEV CO LTD
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