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Method for purifying high-purity organic solvent methanol

A purification method and organic solvent technology, applied in the field of chemical reagents, to achieve the effects of simple operation, high product purity and stable operation

Active Publication Date: 2012-05-02
天津市康科德科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] According to the search, there are very few domestic documents on the purification of high-purity methanol, so it is urgent to develop a purification method for high-purity methanol

Method used

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  • Method for purifying high-purity organic solvent methanol

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Embodiment 1

[0018] A method for purifying methanol, a high-purity organic solvent for scientific research. The purification steps are:

[0019] (1) Oxidation: drive 15kg of 99.5% raw material methanol into a 20L oxidation kettle, add 75g of oxidant hydrogen peroxide and 15g of acid medium sulfuric acid, reflux for 4h, and quickly distill the oxidized methanol;

[0020] (2) Reductive distillation: drive the oxidized methanol into a reduction kettle, add 30 g of calcium hydride as a reducing agent, and perform reductive distillation. Use heat-conducting oil to heat, control the temperature of the heat-conducting oil from 100℃ to 150℃, the temperature of methanol liquid in the distillation kettle from 70℃ to 78℃, the top temperature from 64℃ to 67℃, and control the reflux ratio of 10:4~5 (all displayed in the instrument control On the box), proper control of the distillation temperature and adjustment of the reflux ratio can control the moisture in the methanol effluent. The first distillate is ...

Embodiment 2

[0022] A method for purifying methanol, a high-purity organic solvent for scientific research. The purification steps are:

[0023] (1) Oxidation: drive 10kg of 99.5% raw material chromatographic methanol into a 20L oxidation kettle, add 100g of oxidant potassium permanganate and 4.5g of acid medium sulfuric acid, reflux for 4h, and quickly distill the oxidized methanol;

[0024] (2) Reductive distillation: Pour the oxidized methanol into the reducing distillation kettle, add 80g of the reducing agent calcium hydride, and carry out the reducing distillation, use heat transfer oil to heat, control the temperature of the heat transfer oil from 150 to 200°C, and put it in the distillation kettle The temperature of methanol liquid is 70℃~78℃, the top temperature is 64℃~67℃, and the reflux ratio is 10:4~5 (all displayed on the instrument control box). Properly controlling the distillation temperature and adjusting the reflux ratio can control the moisture in the methanol effluent. The ...

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Abstract

The invention relates to a method for purifying high-purity organic solvent methanol. The steps are as follows: through oxidation, reduction and rectification, and filtration; and the finished productof high-purity methanol can be obtained. The method adopts methanol of 99.5 percent as a raw material and utilizes the qualitative difference of impurities to purify the impurities containing a little unsaturated hydrocarbon and alcohol by the operations of oxidation, reduction and rectification, and impurity removal; and the product of pesticide residue grade and gradient elution grade chromatographic methanol with purity of more than 99.9 percent can be obtained, the yield coefficient is more than 95 percent, and the pesticide residue grade and gradient elution grade chromatographic pure methanol with purity of more than 90 percent is obtained.

Description

Technical field [0001] The invention belongs to the field of chemical reagents, and relates to a purification preparation method of a high-purity organic solvent, in particular a purification method of a high-purity organic solvent methanol for scientific research. Background technique [0002] The methods for preparing pesticide residue grade and gradient elution grade chromatographic methanol are rarely reported in China. Pesticide residue reagents are high-purity reagents used in pesticide residue detection, and their purity requirements are higher than ordinary chromatographic reagents. Due to the heavy dependence on pesticides in the production of agricultural products, the pesticide residues in agricultural products exceed the standard, which affects the food safety of consumers and the foreign trade of agricultural products. For this reason, the state has increased the intensity of pesticide residue testing, increased the types of pesticide testing, and improved the testi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/04C07C29/92C07C29/80
Inventor 宋金链张玉芝
Owner 天津市康科德科技有限公司
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