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Method for producing high-purity ether used for HPLC

A pure ether, high performance liquid chromatography technology, applied in the field of high-purity ether, can solve the problems of limited removal capacity, long time period, large amount of impurity removal reagents, etc., and achieve the effect of reducing the loss of extractant

Active Publication Date: 2013-04-03
ANQING FULLTIME CHEM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are: the process is cumbersome, the time period is too long, and the amount of impurity removal reagents is large, so it is only suitable for laboratory applications
Disadvantages: There are certain requirements for the specifications of crude methyl tert-butyl ether raw materials, and the ability to remove alkenes, ketones and ion impurities is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] In a 100L all-glass reaction still, add 70Kg of raw material industrial-grade tetrahydrofuran, and add 70Kg of ionic liquid 1-butyl-3-methylimidazole chloride with a quality of 10% of raw material industrial-grade tetrahydrofuran, and 70Kg of raw material industrial-grade tetrahydrofuran with a quality of 10‰ Sodium borohydride 700g. After total reflux for 0.5h, adjust the reflux ratio to 4, carry out THF extraction, remove 15% of the head and leave it for later use. The middle of extraction is 50.3Kg of product THF, and the distillate after the tower top temperature exceeds 66.3°C is combined and separated with the next raw material. After obtaining refined tetrahydrofuran, continue to extract water from the top of the tower, and keep the ionic liquid in the tower kettle for next use. The product is analyzed by GC, and the content is 99.9%; the water content is measured by Karl Fischer method, and the water content is 0.03%; the absorbance at 280nm is 0.0238, and the a...

Embodiment 2

[0044] In a 100L all-glass reactive still, add 70Kg raw material industrial grade 1,4-dioxane, and add 1,4-dioxane mass% ionic liquid 1-butyl-3-methyl chloride 35Kg of imidazole, 70g of sodium borohydride with a mass of 1‰ of 1,4-dioxane. After total reflux for 0.5h, adjust the reflux ratio to 6, carry out 1,4-dioxane extraction, pull out 15% of the head and leave it for later use, the middle of the extraction is 55.1Kg of product 1,4-dioxane, and the top of the tower The fraction after the temperature exceeds 102.5°C will be combined and separated with the next raw material. The product is analyzed by GC, and the content is 99.7%; the water content is measured by Karl Fischer method, and the water content is 0.04%; the absorbance at 280nm is 0.0358, and the absorbance at 250nm is 0.2411.

Embodiment 3

[0046] In a 100L all-glass reaction still, add 70Kg raw material industrial grade methyl tert-butyl ether, and add 700g of ionic liquid 1-butyl-3-methylimidazole bromide with 1% raw material quality, and 0.50‰ boron with raw material quality Sodium hydride 35g. After total reflux for 0.5h, adjust the reflux ratio to 10, carry out the extraction of methyl tert-butyl ether, remove 15% of the head and leave it for later use, the middle of the extraction is the product methyl tert-butyl ether 49.4Kg, and the temperature at the top of the tower exceeds 56.5°C Afterwards, the rear fraction is taken out and combined with the next raw material for separation. The product is analyzed by GC, and the content is 99.5%; the water content is measured by Karl Fischer method, and the water content is 0.01%; the absorbance at 280nm is 0.0182, and the absorbance at 254nm is 0.0910.

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Abstract

The invention discloses a method by using all-glass reaction rectification equipment to enable industrial ether (tetrahydrofuran, 1,4-dioxane or MTBE) to react with certain proportion of ionic liquid and reducing agent to be rectified so as to remove the impurities of water, organic substances, ions and the like contained in the industrial ether to obtain high-purity ether used for HPLC.

Description

technical field [0001] The invention relates to a method for purifying industrial-grade ethers (respectively including tetrahydrofuran, 1,4-dioxane and methyl tert-butyl ether) into high-purity ethers for HPLC, belonging to the chemical industry field. Background technique [0002] Tetrahydrofuran, also known as 1,4-epoxybutane, or tetrahydrofuran for short, is a valuable organic solvent with excellent performance. It is widely used in chemical and pharmaceutical production. It is often used as a reactive solvent and is known as "universal solvent". [0003] Now domestic and foreign production of tetrahydrofuran generally adopts furan hydrogenation, furfural method, Reppe method (that is, acetylene hydrogenation method), maleic anhydride (MAH) hydrogenation method, butadiene acetyl oxidation method and butadiene nitriding method . However, the crude products obtained after rectification of these reaction products all contain a small amount of water and a small amount of per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/12C07D307/08C07C43/04C07C41/42
Inventor 周沛
Owner ANQING FULLTIME CHEM INDAL