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Method for synthesizing methylal

A synthesis method, methylal technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as environmental pollution, high cost, equipment corrosion, etc., and achieve cost reduction, low cost, and equipment less corrosive effect

Active Publication Date: 2014-05-21
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the mature synthesis method of methylal is the condensation reaction of methanol and formaldehyde under the action of acid catalysis. Although the conversion rate of liquid inorganic acid in the catalyst used is high, the equipment is severely corroded and cannot be recycled, resulting in a large amount of acidic waste water , which pollutes the environment; although resin catalysts are easy to separate, they have poor temperature resistance, are prone to lose activity, and are relatively expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In the reactor, formaldehyde and methanol were reacted at 40°C for 240min under the action of a solid acid catalyst with a molar ratio of 1:1.5, and the reflux ratio was controlled to be 1:1, and the fraction at the top of the tower was collected at 40°C. Analysis shows that the methylal content is 73%, wherein the solid acid catalyst is acidified aluminum pillared montmorillonite, the dosage is 2% of the total mass of methanol and formaldehyde, and the loading capacity of the main active component sulfuric acid is 30wt%.

[0021] The preparation of acidified aluminum pillared montmorillonite comprises the following steps:

[0022] (1) Preparation of columnar agent: AlCl 3 ·6H 2 Add NaOH solution dropwise into the O aqueous solution, after the dropwise addition is completed, stir at constant temperature for 1 hour, and age for 16 hours to obtain a columnar agent, in which NaOH and AlCl 3 ·6H 2 The molar ratio of O is 1:1, AlCl 3 ·6H 2 The molar concentration of the...

Embodiment 2

[0026] In the reactor, formaldehyde and methanol were reacted at 70°C for 190min under the action of a solid acid catalyst at a molar ratio of 1:2.7, and the reflux ratio was controlled to be 1:1.8. The fraction at the top of the tower was collected at 43°C, and the reaction product was analyzed by gas chromatography. Analysis showed that the methylal content was 76%. Among them, the solid acid catalyst was acidified aluminum pillared montmorillonite, the dosage was 15% of the total mass of methanol and formaldehyde, and the loading amount of sulfuric acid, the main active component, was 5 wt %.

[0027] The preparation of acidified aluminum pillared montmorillonite comprises the following steps:

[0028] (1) Preparation of columning agent: AlCl 3 ·6H 2 Add NaOH solution dropwise into the O aqueous solution, after the dropwise addition is completed, stir at constant temperature for 3 hours, and age for 24 hours to obtain a columnar agent, in which NaOH and AlCl 3 ·6H 2 The ...

Embodiment 3

[0032]In the reactor, formaldehyde and methanol reacted at 60°C for 140min under the action of a solid acid catalyst with a molar ratio of 1:3, and the reflux ratio was controlled to be 1:2.7. The fraction at the top of the tower was collected at 47°C, and the reaction product was analyzed by gas chromatography. Analysis shows that the methylal content is 78%. Among them, the solid acid catalyst is acidified aluminum pillared montmorillonite, the dosage is 8% of the total mass of methanol and formaldehyde, and the loading amount of sulfuric acid, the main active component, is 10 wt%.

[0033] The preparation of acidified aluminum pillared montmorillonite comprises the following steps:

[0034] (1) Preparation of columnar agent: AlCl 3 ·6H 2 Add NaOH solution dropwise into the O aqueous solution, after the dropwise addition, stir at constant temperature for 2 hours, and age for 8 hours to obtain a columnar agent, in which NaOH and AlCl 3 ·6H 2 The molar ratio of O is 1.7:1, ...

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Abstract

The invention relates to a method for synthesizing methylal. Methanal and methanol in the mole ratio of 1:1.5-4.5 are reacted under the effect of a solid-acid catalyst at the temperature of 40-100 DEG C for 40-240min, the reflux ratio is controlled to be 1:1-3.5, and fractions at the temperatures of 40-55 DEG C on the top of the tower are collected to obtain the methylal, wherein the solid-acid catalyst is a home-made acid activated pillared montmorillonite catalyst. The catalyst used in the method is a strong solid-acid catalyst which provides an acidic condition for the synthesis of the methylal, liquid acid catalysis is replaced for synthesizing the methylal, and the catalyst is easy to separate from a reaction system, has small corrosivity on equipment and is easy to recycle; the methylal is high in yield, and low in circulation volume and energy consumption; and the raw material of the catalyst is cheap, is easy to obtain, and is low in cost.

Description

technical field [0001] The invention relates to a method for synthesizing methylal, in particular to a method for synthesizing methylal by using a self-made acidified pillared montmorillonite solid acid catalyst. Background technique [0002] Methylal (DMM), also known as dimethoxymethane, molecular formula structure CH 3 O-CH 2 -OCH 3 , is a colorless, transparent, volatile and flammable liquid, and is one of the downstream products of methanol. Methylal is the simplest member of acetal. It is not only easy to synthesize, but also the cheapest. The raw materials for synthesizing methylal are methanol and formaldehyde, and high-purity formaldehyde can be prepared in turn. The "acetal method" uses formaldehyde As a formaldehyde source, acetal can be extended to produce polyoxymethylene, phenolic resin, polymethoxymethylal and other products, and more high value-added chemicals can be obtained, which can become an important non-petroleum route. [0003] Methylal has excell...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/30C07C41/56
Inventor 白君君牟庆平马韵升史庆苓栾波张建林高洪奎
Owner CHAMBROAD CHEM IND RES INST CO LTD