Preparation method of high-purity halogenated hydrocarbon used for liquid chromatogram

A technology of liquid chromatography and pure halogenated hydrocarbons, which is applied in the field of preparation of high-purity halogenated hydrocarbons for liquid chromatography, to achieve the effects of reducing costs, reducing process steps, and easy recovery

Active Publication Date: 2010-07-21
ANQING FULLTIME CHEM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Halogenated hydrocarbons for liquid chromatography have higher requirements for purity, none of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 5 kg of industrial grade dichloromethane through preliminary rectification was added to the reaction distillation still, and 0.25 kg of 5% sulfuric acid aqueous solution was added at the same time, the temperature of the reaction kettle was 25° C., and the reaction was carried out for 2 hours. Start extraction and rectification, and after 1 hour of total reflux, start to extract the overhead fraction. After the top product is separated by liquid phase, all the water phase is refluxed, and the oil phase is partially refluxed. The total reflux ratio is 7. Extract the fraction below 37.8°C and put it back into the raw material storage tank, extract 4.86 kg of the fraction at 37.8-38.4°C, pass through the drier equipped with 3A molecular sieve at a space velocity of 1 / hour, and obtain 4.48 kg of product dichloromethane, which enters the second extraction Distillation tower. Add 0.224 kilograms of toluene in the second extractive distillation column, and after full reflux fo...

Embodiment 2

[0029]5.0 kg of industrial grade chloroform through preliminary rectification was added to the reactive distillation still, and 1.5 kg of 1% sulfuric acid aqueous solution was added simultaneously, and the temperature of the reaction still was 25° C., and reacted for 2 hours. Start extraction and rectification, and after 1 hour of total reflux, start to extract the overhead fraction. After the top product is separated by liquid phase, all the water phase is refluxed, and the oil phase is partially refluxed. The total reflux ratio is 2. Extract the fraction below 57.8°C and put it back into the raw material storage tank, extract 4.87 kg of the fraction at 57.8-56.4°C, pass through the drier equipped with 3A molecular sieve at a space velocity of 2 / hour, and obtain 4.43 kg of product chloroform, which enters the second extractive distillation tower. The second tower adds 0.443 kilograms of toluene, and after full reflux for 1 hour, the overhead fraction begins to be extracted. A...

Embodiment 3

[0031] Add 5.0 kilograms of industrial grade carbon tetrachloride through preliminary rectification to the reaction distillation kettle, add 0.10 kilograms of 15% sulfuric acid aqueous solution simultaneously, the reaction kettle temperature is 25 ℃, reacts 2 hours. Start extraction and rectification, and after 1 hour of total reflux, start to extract the overhead fraction. After the top product is separated by liquid phase, all the water phase is refluxed, and the oil phase is partially refluxed. The total reflux ratio is 5. Extract 4.79 kg of 65.7~66.3°C distillate, pass through the drier equipped with 4A molecular sieve at a space velocity of 1 / hour to obtain 4.39 kg of product carbon tetrachloride, and enter the second extractive distillation tower. Add 2.40 kilograms of toluene to the second tower, after full reflux for 1 hour, begin to extract the overhead fraction. The distillate below 76.4°C from the top of the tower is put back into the raw material storage tank, 4.18...

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Abstract

The invention relates to a method for producing high-purity halogenated hydrocarbon used for liquid chromatogram by primarily rectified industrial halogenated hydrocarbon. The method comprises the following steps: eliminating unsaturated compounds by sulphuric acid, using water for extractive distillation to remove oxidizable substances, alcohols and high-hydrophilicity impurities with the similar boiling point to the halogenated hydrocarbon; using molecular sieves for water removal through absorption; and using toluene for extractive distillation to remove hydrocarbon with the similar boiling point to the halogenated hydrocarbon.

Description

technical field [0001] The invention relates to a process for preparing high-purity halogenated hydrocarbons for liquid chromatography. Background technique [0002] Halogenated hydrocarbons are compounds in which hydrogen atoms in hydrocarbon molecules are replaced by halogens (fluorine, chlorine, bromine, iodine). There are not many types of naturally occurring halogenated hydrocarbons, and most of them are synthetic products. Halogenated hydrocarbons are generally represented by RX (X=F, Cl, Br, I), and halogen atoms are functional groups of halogenated hydrocarbons. [0003] Dichloromethane is a colorless transparent volatile liquid. Has a pungent ether-like odor. Soluble in about 50 times of water, soluble in phenol, aldehyde, ketone, glacial acetic acid, triethyl phosphate, ethyl acetoacetate, cyclohexylamine. Compatible with other chlorinated hydrocarbon solvents, ethanol, ether and N,N-dimethylformamide. The relative density is 1.3266 (20 / 4°C), the melting point...

Claims

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Application Information

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IPC IPC(8): C07C17/38C07C19/03C07C19/04C07C19/041
Inventor 周沛
Owner ANQING FULLTIME CHEM INDAL
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