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Method for synthesizing trioxymethylene by methanol through condensation, oxidation and polycondensation

A trioxymethylene and methylal technology, which is applied in organic chemistry, chemical industry, climate sustainability, etc., can solve the problems of high equipment material requirements, low trioxymethylene yield, and large recovery volume, and achieves reduction in concentration. The effect of energy consumption, improving one-way conversion rate, and reducing residence time

Inactive Publication Date: 2016-12-28
XIAN SHANGHUA TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But no matter what type of catalyst is used above, the biggest problem of these methods for synthesizing paraformaldehyde based on aqueous formaldehyde solution is that the formaldehyde solution needs to be concentrated to more than 65%, and the paraformaldehyde yield in the reaction phase is very low (under the above conditions When sulfuric acid and ionic liquid are used as catalysts, the equilibrium concentration of paraformaldehyde in the reaction kettle liquid is only about 1.8% and 2.5% respectively (mass percentage), and formic acid, methyl formate, etc. are generated at the same time, so it must be produced by reactive distillation process Paraformaldehyde
This type of process also generally has the problem of recovery and treatment of dilute formaldehyde. The recovery of dilute formaldehyde basically adopts a distillation scheme, which has a large recovery volume, high energy consumption, high requirements for equipment materials, and large investment.

Method used

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  • Method for synthesizing trioxymethylene by methanol through condensation, oxidation and polycondensation

Examples

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Effect test

Embodiment 1

[0034] As shown in Figure 1, the synthesis method of this embodiment is:

[0035] Step 1, methanol condensation to prepare methylal: according to the molar ratio of methanol and formaldehyde of 2.0:1, methanol and dilute formaldehyde with a mass concentration of 5% are mixed and then sent to 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 at 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. Ratio is 3.0, including product ...

Embodiment 2

[0041] As shown in Figure 1, the synthesis method of this embodiment is:

[0042] Step 1, methanol condensation to prepare methylal: according to the molar ratio of methanol and formaldehyde of 3.0:1, methanol and dilute formaldehyde with a mass concentration of 20% are mixed and then sent to 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 trays 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 top pressure of the first reactive distillation tower 2 is controlled to be 30kPa, the temperature of the top of the tower is 45°C, and the temperature of the bottom of the tower is 108°C. Ratio is 2.0, the product methylal and...

Embodiment 3

[0048] As shown in Figure 1, the synthesis method of this embodiment is:

[0049] Step 1, methanol condensation to prepare methylal: according to the molar ratio of methanol and formaldehyde of 3.5:1, methanol and dilute formaldehyde with a mass concentration of 45% are mixed and then sent to 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 at 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 temperature of the top of the tower is 42.3°C, the temperature of the bottom of the tower is 100°C, the reflux ratio is 1.0, the material after the co...

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Abstract

The invention relates to a method for synthesizing trioxymethylene by methanol through condensation, oxidation and polycondensation. According to the invention, methanol and dilute formaldehyde with concentration of 5-30% separated from a trioxymethylene apparatus are taken as raw materials to synthesize methylal with concentration of 85-99.9%; methylal and air are subjected to catalyst oxidation to generate formaldehyde through an iron molybdenum method, through refining water and methylal unit tower waste water absorption, a formaldehyde aqueous solution with concentration of 70% is generated; high-concentration formaldehyde is introduced into a trioxymethylene synthetic tower, and the trioxymethylene is synthesized under existence of a strong-acid cation exchange resin catalyst, and trioxymethylene with content of 99.9% can be obtained through steps of rectification and concentration, extraction, rectification, and purifying. The method solves the problems of low conversion rate, selectivity and low yield during a trioxymethylene production process, solves the problems of low catalyst reaction efficiency and corrosivity, and solves the problems of complex technology and high energy consumption. The method provides good raw materials for producing PODE, and realization of industrialization of PODE can solve the problem of excess production capacity of methanol in our country.

Description

technical field [0001] The invention relates to a method for synthesizing trioxane with methanol through condensation, oxidation and polycondensation processes. In particular, it relates to a catalyst using a strongly acidic styrene-based cation exchange resin. It belongs to the technical field of chemical synthesis. Background technique [0002] Paraformaldehyde (TOX) and many related industries are extremely important links in the carbon-one chemical industry chain. First of all, paraformaldehyde is the raw material for preparing polyoxymethylene (POM) engineering plastics. POM is one of the three major engineering plastics in the world, and the domestic demand is increasing day by day. At the same time, paraformaldehyde can replace formaldehyde and is widely used in the preparation of bulk chemicals and fine chemicals, including disinfectants, antibacterials, fumigants, insecticides, and adhesives. The raw material can also be used to synthesize isooctyl thioglycolate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D323/06
CPCC07D323/06Y02P20/10
Inventor 陈华刘宗强郁刘军
Owner XIAN SHANGHUA TECH DEV CO LTD
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