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Method for producing diethoxymethane by using paraformaldehyde

A diethoxymethane and paraformaldehyde technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of easy carbon deposition on the surface of the catalyst, difficulty in rectification, and difficulty in handling, and achieve accelerated Catalytic reaction rate, reduce production cost, save production cost effect

Pending Publication Date: 2022-07-15
甘肃美润新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because diethoxymethane is unstable under strong acidic conditions, it is easily decomposed into formaldehyde and ethanol. When the conventional process uses 37% formaldehyde for reaction, due to the large amount of water in the raw material, it is difficult to continue the conversion of the raw material after reaching the reaction equilibrium, resulting in The conversion rate of raw materials is low, and the waste water contains a large amount of unreacted formaldehyde, which is difficult to treat; the use of inorganic acid catalyzed reaction tends to produce a large amount of acidic waste water, which is gradually eliminated by heteropoly acid or solid organic acid catalyzed reaction
Using organic acid as a catalyst and adopting kettle reaction to rectify diethoxymethane, the process is simple, the operation is convenient, and the phenomenon is intuitive, but there are low conversion rate and poor selectivity in the preparation process, and the products generated during the reaction cannot be removed in time. Secondary reactions are prone to occur, which brings difficulty to subsequent rectification and affects product quality and yield; solid organic acid is used as catalyst, and diethoxymethane is prepared by reactor reaction rectification, which has uneven distribution of raw materials and catalysts, internal There are problems such as temperature difference and long contact time, and carbon deposits on the surface of the catalyst affect the conversion rate

Method used

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  • Method for producing diethoxymethane by using paraformaldehyde
  • Method for producing diethoxymethane by using paraformaldehyde
  • Method for producing diethoxymethane by using paraformaldehyde

Examples

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Embodiment 1

[0026] Example 1: Production of diethoxymethane using a preparation method comprising the following steps.

[0027] (1) Add 4500kg ethanol (volume fraction is 95%) in the depolymerization tank, then add 1000kg paraformaldehyde (content 96%), mix evenly so that paraformaldehyde is fully dispersed in ethanol; then add 0.3kg of 98% sulfuric acid , continue to mix evenly, at the same time, the temperature in the depolymerization tank is raised to 45 ° C and kept at normal pressure for 1 hour, so that paraformaldehyde is completely depolymerized into monomer formaldehyde and fully dissolved in ethanol to form a formaldehyde-ethanol solution.

[0028] (2) The formaldehyde-ethanol solution obtained in step (1) is subjected to continuous atmospheric-pressure catalytic reaction in a tubular fixed-bed catalytic reactor at atmospheric pressure at 45°C for 2 hours, and the reaction obtains that the content of diethoxymethane is greater than or equal to 50%, and the content of formaldehyde ...

Embodiment 2-5

[0034] The process parameters and all sample addition amounts of Examples 2-5 are consistent with those of Example 1. The only difference is that a depolymerizing agent different from Example 1 is used. The composition of the oxymethane finished product is shown in Table 1.

[0035] Depolymerization agent, consumption and product composition table that table 1 embodiment 2-5 adopts

[0036]

Embodiment 6-8

[0038] The process parameters of Examples 6-8 and all the sample addition amounts are consistent with those of Example 1, the only difference is that a different extraction agent from Example 1 was used, the type and amount of the specifically used extraction agent, and the final obtained diethoxyl The composition of the base methane product is shown in Table 2.

[0039] The extraction agent that table 2 embodiment 6-8 adopts, consumption and product composition table

[0040]

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Abstract

The invention discloses a method for producing diethoxymethane by using paraformaldehyde, which comprises the following steps: (1) dispersing paraformaldehyde in ethanol, adding a depolymerizing agent for depolymerization reaction, and dissolving the reaction product in ethanol to form a formaldehyde ethanol solution; (2) carrying out normal-pressure continuous catalytic reaction on the formaldehyde ethanol solution; (3) carrying out continuous catalytic distillation on the reaction product obtained in the step (2), and condensing and collecting fractions; (4) carrying out countercurrent continuous extraction on the fraction to obtain crude diethoxymethane; and (5) carrying out normal-pressure rectification on the crude diethoxymethane to obtain a diethoxymethane finished product. The raw material conversion rate of diethoxymethane produced by the method is high, less wastewater is generated in the production process and is easy to treat, and meanwhile, the tubular fixed bed catalytic reactor is adopted for reaction and the reaction distillation tower is adopted for continuous distillation, so that the production process is continuous and stable, and the production process is safe and environment-friendly.

Description

technical field [0001] The invention relates to the production technology field of diethoxymethane, in particular to a method for producing diethoxymethane by using paraformaldehyde. Background technique [0002] The boiling point of diethoxymethane is 88°C. As a solvent in organic synthesis, it has the following advantages: 1) suitable operating temperature range; 2) low viscosity, easy to operate and handle; 3) low solubility in water; 4) with water and ethanol It forms a ternary azeotrope, and forms a binary azeotrope with water and ethanol, which is beneficial to the purification of the product; 5) It has good stability, and can be used in strong bases such as hydroxide, sodium hydride and Grignard reagent and weak It is stable under acidic conditions, and it is not easy to form peroxides. These characteristics make diethoxymethane have important and extensive application value in organic synthesis. In recent years, its demand has increased exponentially, and it has rec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C41/58C07C43/30
CPCC07C41/56C07C41/58C07C43/30
Inventor 沈建成杨波王成城
Owner 甘肃美润新材料科技有限公司