Unlock instant, AI-driven research and patent intelligence for your innovation.

Refinement method of 1,4-dioxane

A refining method, the technology of dioxane, applied in the direction of organic chemistry, can solve the problems of high risk and cumbersome operation, and achieve the effect of high risk, cumbersome operation and stable product quality

Active Publication Date: 2015-02-11
SINOPHARM CHEM REAGENT
View PDF4 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the above-mentioned problems, the purpose of the present invention is to provide a method for refining 1,4-dioxane, which avoids the use of ferrous sulfate and sodium metal, and overcomes the use of ferrous sulfate and sodium metal in the prior art. The defect of high risk and cumbersome operation, at the same time, use strong acid resin dehydrating agent to dehydrate to obtain refined 1,4-dioxane, which has a water content of 0.02-0.03% and a purity of 99.5-99.8wt%.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 1000g of industrial 1,4-dioxane in a reaction vessel equipped with a reflux condenser, an agitator, and a thermometer, then add 20mL of a concentration of 5wt% cuprous chloride solution, heat to reflux, and simultaneously feed nitrogen for 6 Cool to room temperature after 1 hour, add solid potassium hydroxide under stirring until the solid potassium hydroxide is no longer dissolved, divide the water layer, and dry the organic layer with 300g 4A molecular sieve for 12 hours, then filter the solid, and add Amberlyst15 strong acid to the filtrate Resin dehydrating agent 100g, after refluxing for 6 hours, collect fractions at 101-102°C to obtain 858g of 1,4-dioxane with a purity of 99.5%. After testing, its water content is 0.02%.

Embodiment 2

[0028] Add 1000g of industrial 1,4-dioxane in a reaction vessel equipped with a reflux condenser, an agitator, and a thermometer, then add 50mL of a concentration of 10wt% cuprous chloride solution, heat to reflux, and simultaneously feed nitrogen for 8 Cool to room temperature after 1 hour, add solid potassium hydroxide under stirring, until solid potassium hydroxide is no longer dissolved, divide water layer, organic layer is dried 24 hours with 100g solid potassium hydroxide, then filter solid, add Amberlyst15 in the filtrate 200g of strong acidic resin dehydrating agent, after refluxing for 8 hours, collect fractions at 101-102°C to obtain 886g of 1,4-dioxane with a purity of 99.8%. After testing, its water content is 0.03%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a refinement method of 1,4-dioxane, which comprises the following steps: by using industrial 1,4-dioxane as the raw material, adding a cuprous chloride solution, introducing nitrogen in a reflux state, cooling, adding solid potassium hydroxide until the potassium hydroxide is not dissolved any longer, separating out the water layer, drying the organic layer with solid potassium hydroxide, and refluxing the filtrate in the presence of a strongly-acidic resin dehydrating agent to obtain the refined 1,4-dioxane. The water content of the 1,4-dioxane obtained by the method is less than 0.05%, and the purity is 99.5-99.8 wt% and conforms to the analytical purity requirement for 1,4-dioxane in Standard HG / T3499-2004. Compared with the prior art, the method disclosed by the invention avoids using ferrous sulfate and sodium metal, can recycle the strongly-acidic resin dehydrating agent, has stable product quality, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for refining 1,4-dioxane. Background technique [0002] 1,4-Dioxane is used as a 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. This product forms a coordination compound with sulfur trioxide, which can be used as a sulfating agent in the synthesis of many compounds; it can be used for the extraction of medicines and pesticides, and the dewaxing of petroleum products; it can be used as a dispersant for dyes and wood colorants. agent and solvent for oil-soluble dyes; used as a high-purity metal surface treatment agent, etc. 1,4-dioxane can be freely mixed with water, and usually contains a small amount of diethanol acetal and water. Long-term storage of 1,4-dioxane also contains peroxide, which affects its application performance. [0003] In the prior art, the refining method of 1,4-dioxane is comm...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D319/12
Inventor 凌芳王伟倪传宏曹丽丽郑琦
Owner SINOPHARM CHEM REAGENT