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Purification method of high-purity organic solvent methanol

A technology of organic solvent and purification method, which is applied in the purification of high-purity organic solvent methanol for scientific research and the purification and preparation of high-purity organic solvent, which can solve the problems of high cost, achieve simple operation, be suitable for large-scale production, and reduce raw material costs Effect

Pending Publication Date: 2022-04-12
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this patent application must be made of high-concentration methanol, which is expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of purification method of high-purity organic solvent methanol, the step of purification is:

[0018] (1) impurity removal: the purity of the raw material is 90% methanol raw material 15kg to remove impurities by nano-silicon adsorption to obtain refined methanol;

[0019] (2) Oxidation: Pour the refined methanol prepared in step (1) into a 20L oxidation kettle, add 75g of oxidant hydrogen peroxide, 15g of acid medium sulfuric acid, reflux for 4 hours, and quickly evaporate the oxidized methanol;

[0020] (3) Reductive rectification: put the oxidized methanol into the reduction kettle, add 30 g of reducing agent calcium hydride, and carry out reductive rectification. Use heat conduction oil to heat, control heat conduction oil temperature 100℃~150℃, methanol liquid temperature in rectification kettle 70℃~78℃, top temperature 64℃~67℃, control reflux ratio 10:4~5 (all displayed on instrument control box), proper control of the rectification temperature and adjustm...

Embodiment 2

[0022] A kind of purification method of high-purity organic solvent methanol, the step of purification is:

[0023] (1) impurity removal: the purity of the raw material is 90% methanol raw material 10kg to remove impurities by nano-silicon adsorption to obtain refined methanol;

[0024] (2) Oxidation: Put 10 kg of chromatographic methanol with a content of 99.5% into a 20L oxidation kettle, add 100 g of oxidant potassium permanganate, 4.5 g of acidic medium sulfuric acid, reflux for 4 hours, and quickly steam out the oxidized methanol;

[0025] (3) Reductive rectification: put the oxidized methanol into the reducing rectification kettle, add 80g of calcium hydride as a reducing agent, carry out reductive rectification, use heat-conducting oil to heat, control the temperature of the heat-conducting oil at 150°C to 200°C, and put it in the rectifying kettle The methanol liquid temperature is 70°C-78°C, the top temperature is 64°C-67°C, and the reflux ratio is controlled at 10:4-...

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PUM

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Abstract

The invention discloses a method for purifying high-purity organic solvent methanol. The method comprises the following steps: (1) impurity removal: adsorbing a methanol raw material with the purity of 90% through nano silicon to remove impurities so as to obtain refined methanol; (2) oxidizing and pumping the refined methanol obtained in the step (1) into a reaction kettle, adding an oxidizing agent and sulfuric acid, refluxing for 2-4 hours, and distilling out methanol; and (3) reduction rectification: pumping the distilled methanol into a reduction rectification kettle, adding a reducing agent for reduction rectification, heating by using heat conduction oil, controlling the temperature of the heat conduction oil to be 100-200 DEG C, the temperature of methanol liquid in the rectification kettle to be 70-78 DEG C, the top temperature to be 64-67 DEG C and the reflux ratio to be 10: (4-5), removing primary fractions, and filtering distillate to obtain a high-purity methanol finished product. The methanol with the content of 90% is used as the raw material, so that the cost of the raw material is reduced.

Description

technical field [0001] The invention belongs to the field of chemical reagents, and relates to a method for purifying and preparing a high-purity organic solvent, in particular to a method for purifying methanol, a high-purity organic solvent 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 the detection of pesticide residues, and their purity requirements are higher than ordinary chromatographically pure reagents. Due to the heavy reliance 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 detection, increased the types of pesticide detecti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C29/76C07C29/80C07C29/88C07C31/04
Inventor 王伟王永旗吕明李定发
Owner TAICANG HUSHI REAGENT