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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The boiling point and PODE of these hydrolysis products 3-8 approach, PODE 3-8 The hydrolysis not only reduces the yield of the product, but also makes the separation of the product difficult

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

Embodiment 1

[0042] Such as figure 1 Shown, the synthesis method of the present embodiment is:

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

Embodiment 2

[0052] Such as figure 1 Shown, the synthesis method of the present embodiment is:

[0053] Step 1, methanol condensation to prepare methylal: according to the ratio of the molar ratio of methanol to formaldehyde of 3.0:1, methanol and dilute formaldehyde with a mass concentration of 20% are mixed and then sent to the reactor 1 filled with a catalyst for condensation reaction. The reaction temperature of the condensation reaction is 70°C, the reaction pressure is 5.0MPa, and then the material after the condensation reaction is sent to the first reactive distillation tower 2, and the number of sieve plates at the top of the first reactive distillation tower 2 is 20 , the number of sieve trays at the bottom of the tower is 20, the number of layers of the packed bed is 5 layers, the pressure at the top of the first reactive distillation tower 2 is controlled to be 30kPa, the temperature at the top of the tower is 45°C, and the temperature at the bottom of the tower is 108°C. The ...

Embodiment 3

[0062] Such as figure 1 Shown, the synthesis method of the present embodiment is:

[0063]Step 1, methanol condensation to prepare methylal: according to the ratio of the molar ratio of methanol to formaldehyde of 3.5:1, methanol and dilute formaldehyde with a mass concentration of 45% are mixed and then sent to the reactor 1 filled with a catalyst for condensation reaction. The reaction temperature of the condensation reaction is 60°C, the reaction pressure is 2.0MPa, and then the material after the condensation reaction is sent to the first reactive distillation tower 2, and the number of sieve trays on the top of the first reactive distillation tower 2 is 5 , the number of sieve trays at the bottom of the tower is 5, the number of layers of the packed bed is 2, the top pressure of the first reactive distillation tower 2 is controlled to be 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 ...

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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

technical field [0001] The invention belongs to the technical field of oil additive preparation, and in particular relates to a method for synthesizing polyoxymethylene dimethyl ether through condensation, oxidation, polycondensation and etherification of methanol. Background technique [0002] In recent years, with the development of the world economy, the demand for main fuel oils such as gasoline and diesel is also increasing day by day, especially the situation that the supply of diesel oil is in short supply. The contradiction between the tight supply and demand of diesel oil reflects the great demand for diesel oil in the world, but Exhaust gas from diesel combustion pollutes the environment and has become a major source of urban air pollution. Increasing production, reducing fuel consumption, and reducing pollution are the main directions for the development of clean diesel. A relatively simple, economical, effective and easy method is to add oxygen-containing compon...

Claims

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Application Information

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IPC IPC(8): C07C41/56C07C43/30B01J31/08
CPCC07C41/50C07C41/56C07C45/37C07C43/30C07C47/04Y02P20/10
Inventor 刘红喜陈华卢建华郁刘军
Owner XIAN SHANGHUA TECH DEV CO LTD
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