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Process method for preparing high-purity methylal

A process method, methylal technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as poor results

Active Publication Date: 2020-06-09
KAIRUI ENVIRONMENTAL PROTECTION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, no matter whether polyhydric alcohol is used as the extractant or formaldehyde aqueous solution is used as the extractant, it is only effective for the removal of methanol, but not effective for the elution and extraction of formic acid and methyl formate.

Method used

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  • Process method for preparing high-purity methylal
  • Process method for preparing high-purity methylal
  • Process method for preparing high-purity methylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Laboratory device verification includes the following steps:

[0029] (1) The components of the methylal raw material (hereinafter referred to as the raw material) are: methylal 89.55% wt, methanol 7.85% wt, formic acid 0.35% wt, and methyl formate 2.25% wt.

[0030] (2) The components of the aqueous solution extractant containing alkali and salt formaldehyde (hereinafter referred to as the extractant) are: formaldehyde 32.55% wt, sodium hydroxide 2.55% wt, sodium formate 0.50% wt, and the rest being water.

[0031] (3) Put 100g each of the raw material and the extractant into a 1000ml four-neck flask 1-1, shake vigorously to mix the raw material and the extractant, and then figure 1 The rectification device is installed, the flask 1-1 is gradually heated by the heater 1-2, and the temperature at the top of the rectification column is controlled by the reflux inside the rectification column 1-3 to ≯45℃, and the vaporized methylal passes through the condenser 1-4 After condensi...

Embodiment 2

[0034] Laboratory device verification includes the following steps:

[0035] (1) The components of the methylal raw material (hereinafter referred to as the raw material) are: methylal 89.55% wt, methanol 7.85% wt, formic acid 0.35% wt, and methyl formate 2.25% wt.

[0036] (2) The components of the aqueous extractant containing alkali and salt formaldehyde (hereinafter referred to as the extractant) are: formaldehyde 6.85% wt, sodium hydroxide 0.6% wt, sodium formate 0.15% wt, and the rest is water.

[0037] (3) Put 100g each of the raw material and the extractant into a 1000ml four-neck flask 1-1, shake vigorously to mix the raw material and the extractant, and then figure 1 The rectification device is installed, the flask 1-1 is gradually heated by the heater 1-2, and the temperature at the top of the rectification column is controlled by the reflux inside the rectification column 1-3 to ≯45℃, and the vaporized methylal passes through the condenser 1-4 After condensing, it is coll...

Embodiment 3

[0040] A process method for preparing high-purity methylal. Extraction and rectification are performed simultaneously. figure 2 The shown device is carried out: the main body is the rectification tower 1, the upper middle of the tower wall is provided with an extractant inlet 2, the middle and lower middle is provided with a methylal raw material inlet 3, and the upper part of the other side of the tower wall is provided with a reflux port 4. It is provided with a discharge port I 5, and the tower kettle is provided with a discharge port II 6, wherein: the extractant inlet is connected to a device capable of supplying extractant; the methylal raw material inlet is connected to a device capable of supplying methylal The raw material device is connected; the outlet I 5 is connected with a condenser 7, and the outlet of the condenser is divided into two paths, one is connected to the return port, and the other is connected to the device for harvesting high-purity methylal The disc...

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Abstract

The invention discloses a process method for preparing high-purity methylal, which comprises the following step: by using a formaldehyde aqueous solution containing alkali and salt as an extractant, synchronously or stepwise extracting and rectifying the extractant and methylal, thereby removing impurities in the methylal raw material to obtain the high-purity methylal. According to the process method for preparing the high-purity methylal, methanol in the methylal is effectively removed, and meanwhile impurities such as formic acid and methyl formate in the methylal are removed. The formaldehyde extracting solution without impurities can be reused as a raw material for preparing methylal.

Description

Technical field [0001] The present invention relates to a process method for preparing high-purity methylal. An aqueous formaldehyde solution containing alkali and salt is used as an extractant to remove impurities such as methanol, formic acid, methyl formate and the like in the methylal to prepare high-purity methylal with a content of more than 99.95% wt. Purity methylal. The invention is suitable for the field of methylal preparation, and is especially suitable for preparing high-purity methylal without formic acid and methyl formate. Background technique [0002] Methylal, also known as formaldehyde dimethylacetal, dimethoxymethane. Structural formula CH 2 (OCH 3 ) 2 , Melting point: -104.8°C, boiling point: 42.3°C, density: 0.8593g / ml. [0003] Methylal is widely used in industry as an excellent solvent with lower toxicity and environmental protection. Methylal can be used for quantitative dissolution of grease, wax, nitrocellulose, synthetic resin, polystyrene, vinyl acet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/30C07C41/56C07C41/58
CPCC07C41/56C07C41/58C07C43/30Y02P20/10
Inventor 刘文飞张长胜曹红军毛进池
Owner KAIRUI ENVIRONMENTAL PROTECTION TECH