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Purification method of chromatographic pure 1,4-dioxane

A technology of dioxane and purification method, applied in the direction of organic chemistry, etc., can solve the problems such as failure to achieve purification effect, poor treatment effect, incomplete reaction, etc., to prevent iron impurities, complete reaction, and high safety. Effect

Inactive Publication Date: 2019-03-08
天津康科德医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the purification method of 1,4-dioxane generally uses ferrous sulfate or cuprous chloride as the reducing agent to remove the peroxide impurity, but due to the incomplete reaction of these two reducing agents, the treatment effect is not good. good, long-term deposition at the bottom of the kettle is difficult to clean, etc., and the ideal purification effect cannot be achieved

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  • Purification method of chromatographic pure 1,4-dioxane

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Embodiment 1

[0045] A kind of purification method of 1,4-dioxane, the steps are as follows:

[0046] 1) Hydrolysis: put 1,4-dioxane raw material with a content of 98.0% into the reactor, add a strong acidic cation exchange resin with a mass fraction of 0.02% to 0.05% into the reactor, and heat to 100 to 150°C , reflux for 1 to 2 hours, and hydrolyze the 2-methyl-1,3-dioxolane impurity in the raw material.

[0047] 2) Adsorption: Put the hydrolyzed 1,4-dioxane raw material into the cation exchange resin adsorption column, in which the adsorption column is 1.6m high and 4.2cm in diameter, and the height of the cation exchange resin product inside is 4 / 5 of the column height. Adsorption and filtration of some aldehyde impurities in the 1,4-dioxane raw material is carried out through a cation exchange resin adsorption column, and the filtration flow rate is 300-500mL / min;

[0048] 3) The raw materials adsorbed by cation exchange resin are then adsorbed by an activated carbon filter column. Th...

Embodiment 2

[0056] A kind of purification method of 1,4-dioxane, the steps are as follows:

[0057] 1) Hydrolysis: put 1,4-dioxane raw material with a content of 98.0% into the reactor, add a strong acidic cation exchange resin with a mass fraction of 0.02% to 0.05% into the reactor, and heat to 100 to 150°C , Reflux reaction for 1.5-2h, 2-methyl-1,3-dioxolane impurity in the raw material.

[0058] 2) Adsorption: Put the hydrolyzed 1,4-dioxane raw material into the cation exchange resin adsorption column, in which the adsorption column is 1.6m high and 4.2cm in diameter, and the height of the cation exchange resin product inside is 4 / 5 of the column height. Adsorption and filtration of some aldehyde impurities in the 1,4-dioxane raw material is carried out through a cation exchange resin adsorption column, and the filtration flow rate is 500-800mL / min;

[0059] 3) The raw material adsorbed by cation exchange resin is then adsorbed by an activated carbon column. The activated carbon colum...

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Abstract

The invention provides a purification method of chromatographic pure 1,4-dioxane. The method comprises the following steps of (1) eliminating 2-methyl-1,3-dioxolame impurities through hydrolysis; (2)performing adsorption: injecting the hydrolyzed 1,4-dioxane raw materials into a serially connected cation exchange resin adsorption column and active carbon adsorption column; adsorbing some aldehydes impurities in the 1,4-dioxane raw materials; (3) removing peroxides through the adsorption by a lithium aluminum hydride adsorption column; (4) performing drying and dewatering by a 4A molecular sieve; (5) performing rectification. According to the method, 1,4-dioxane industrial products with the content being 98.0 percent are used as raw materials; some adsorbable impurities can be eliminated through hydrolysis, the cation exchange resin adsorption column and the active carbon adsorption column; then, through heating treatment, the peroxides in the products are eliminated through the entering into a lithium aluminum hydride filling column. The method has the advantages that the reaction is complete; the safety is high. After the rectification, the final product content reaches 99.9 percent or higher; the moisture is less than or equal to 0.02 percent.

Description

technical field [0001] The invention belongs to the field of chemical reagents and relates to a method for purifying 1,4-dioxane. Background technique [0002] 1,4-Dioxane, also known as dioxane in Chinese, is a colorless transparent liquid with a boiling point of 101.1°C (101.35kPa), a melting point of 11.8°C, a relative density of 1.0336 (20 / 4°C), and a refractive index of 1.4224 (25°C). . It is an important organic solvent, which is used as solvent, reaction medium and extraction agent in the manufacture of special fine chemicals such as medicine, cosmetics and spices, as well as in scientific research. Secondly, it is widely used as a reaction solvent for polyurethane synthetic leather and amino acid synthetic leather. The product has a strong dissolving ability, which is similar to that of dimethylformamide and stronger than that of tetrahydrofuran. Therefore, the product is widely used. [0003] At present, the purification method of 1,4-dioxane generally uses ferro...

Claims

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Application Information

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IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 刘岩宋金链
Owner 天津康科德医药化工有限公司
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