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Purifying method for electronic-grade hexane

A purification method, n-hexane technology, applied in chemical instruments and methods, hydrocarbon purification/separation, adsorption purification/separation, etc., can solve the problem of low yield, achieve the effect of improving purity and ensuring yield

Inactive Publication Date: 2017-09-29
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN104744196A discloses a method for purifying high-purity organic solvent n-hexane. The method is specifically as follows: firstly add an oxidant and stir, then heat and distill out n-hexane; The dehydrating agent column carries out adsorption treatment, and the purity after purification is only 99.0wt%, and its yield is also low in addition

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a stirred reactor equipped with concentrated sulfuric acid (98.5 wt%) and N-methylpyrrolidone bisulfate with a volume ratio of 5:1, put industrial-grade n-hexane crude product (purity 95.0 %), and kept stirring, standing to separate layers, the upper layer is the treated crude n-hexane. This reaction was repeated three times.

[0038] The above treated crude n-hexane was passed through an adsorption column of 5A molecular sieve at 5 column volumes / hour to remove moisture.

[0039] Finally, the crude n-hexane from which moisture has been removed is added to an extractant that accounts for 1.5 volumes of the crude n-hexane to pass through the extractive distillation column. The extractant is a mixture of dimethyl phthalate and DMF at a volume ratio of 1:0.2. The upper part of the extractive distillation tower is fed with crude normal hexane at a flow rate of 2Kg / h, and the lower part of the extractive distillation tower is fed with dimethyl phthalate at a flow rate of...

Embodiment 2

[0041] In the stirred reactor equipped with concentrated sulfuric acid (92.5 wt%) and N-methylpyrrolidone bisulfate with a volume ratio of 9:1, put industrial-grade n-hexane crude product (purity 96 %), and kept stirring, standing to separate layers, the upper layer is the treated crude n-hexane. This reaction was repeated three times.

[0042] The above treated crude n-hexane was passed through an adsorption column of 5A molecular sieve at 15 column volumes / hour to remove moisture.

[0043] Finally, the crude n-hexane from which moisture has been removed is added to an extractant which accounts for 1.8 volumes of the crude n-hexane to pass through the extractive distillation column. The extractant is a mixture of dimethyl phthalate and DMF at a volume ratio of 1:0.25. The upper part of the extractive distillation tower is fed with crude normal hexane at a flow rate of 6Kg / h, and the lower part of the extractive distillation tower is fed with dimethyl phthalate at a flow rate...

Embodiment 3

[0045] In a stirred reactor equipped with concentrated sulfuric acid (95.5 wt%) and N-methylpyrrolidone bisulfate with a volume ratio of 5:1, put industrial-grade n-hexane crude product (purity 97 %), and kept stirring, standing to separate layers, the upper layer is the treated crude n-hexane. This reaction was repeated three times.

[0046] The above treated crude n-hexane was passed through an adsorption column of 5A molecular sieve at 15 column volumes / hour to remove moisture.

[0047] Finally, the crude n-hexane from which moisture has been removed is added to an extractant which accounts for 3 volumes of the crude n-hexane and passes through the extractive distillation column. The extractant is a mixture of dimethyl phthalate and DMF at a volume ratio of 1:0.30. The upper part of the extractive distillation tower is fed with crude normal hexane at a flow rate of 6Kg / h, and the lower part of the extractive distillation tower is fed with dimethyl phthalate at a flow rate ...

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PUM

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Abstract

The invention discloses a purifying method for electronic-grade hexane. The purifying method comprises the following steps: (1) reacting a crude hexane product with a decolorant; (2) allowing the crude hexane product treated in the step (1) to pass through a dehydrating agent; and (3) allowing the crude hexane product treated in the step (2) to pass through an extraction and rectification tower with a mixture of dimethyl phthalate and DMF in a volume ratio of 1: 0.2-0.5 as an extractant. According to the purifying method in the invention, the decolorant is used at first for removing macromolecular organic matters, ions and other impurities; then the dehydrating agent is used for removing moisture impurities; finally, the extraction and rectification tower is employed so as to allow hexane to be separated from other alkane impurities; so product purity is improved, and yield is guaranteed.

Description

technical field [0001] The invention relates to the technical field of n-hexane purification, in particular to an electronic-grade n-hexane purification method. Background technique [0002] The molecular formula for n-hexane is C 6 h 14 , belongs to straight chain alkanes, alias hexane. It is a colorless liquid with low toxicity and a faint special odor. Commonly used in wiping and cleaning operations in the production process of the electronic information industry, as well as crude oil leaching in the food manufacturing industry, propylene solvent recovery in the plastics manufacturing industry, extraction agents in chemical experiments (such as: phosgene experiments) and production of daily chemicals n-hexane is also used in industries such as floral solvent extraction at that time. If used improperly, it can easily cause occupational poisoning. [0003] In the prior art, there are many reports on the conventional treatment methods of n-hexane, but there are few disc...

Claims

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Application Information

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IPC IPC(8): C07C9/15C07C7/08C07C7/13
CPCC07C7/08C07C7/005C07C7/13C07C9/15
Inventor 王永旗王伟吕明
Owner TAICANG HUSHI REAGENT