Preparation method for carbon tetrachloride

A technology of carbon tetrachloride and carbon disulfide, applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve problems such as improper handling of by-products, low purity of finished products, and low investment, so as to improve sufficiency and improve reaction Efficiency, the effect of improving purity

Inactive Publication Date: 2017-03-08
王显权
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has less investment, and the product is easy to purify, but due to improper handling of by-products, it causes relatively serious waste and pollution; simultaneously in the preparation process of carbon tetrachloride, due to the defects of temperature and steps, iron needs to be added as Catalyst, resulting in lower purity of the finished product

Method used

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  • Preparation method for carbon tetrachloride

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Effect test

Embodiment 1

[0020] Such as figure 1 A kind of preparation method of carbon tetrachloride shown, comprises the following steps:

[0021] Step 1: Tube chlorination: Mix carbon disulfide with a purity of 98% and chlorine solution with a purity of 99% at a weight ratio of 1:2, and then add it to a coiled tube reactor for reaction. The coiled tube reactor is placed in water, and the water temperature is controlled at 100°C , the reaction vapor after the reaction is generated and introduced into the fractionation tower to carry out a fractionation;

[0022] Step 2: Fractionation tower one fractionation: Fractionation temperature is 85 ℃, collects a distillate carbon tetrachloride at the top of the fractionation tower, and a distillate is dried through a solid alkali drier to obtain low-purity carbon tetrachloride, a fractionation tower Store liquid disulfide dichloride for tower chlorination;

[0023] Step 3: tower chlorination: the fractionation tower is fully refluxed, and an excess of 25% ...

Embodiment 2

[0029] The difference between Example 2 and Example 1 is that the purity of carbon disulfide in step 1 is 97%, and the water temperature is 95°C; the fractionation temperature in step 2 is 83°C; the fractionation temperature in step 6 is 80°C.

Embodiment 3

[0031] The difference between embodiment 3 and embodiment 1 is that the water temperature in step one is 98°C; the fractionation temperature in step two is 80°C; the fractionation temperature in step six is ​​82°C.

[0032] Compared with the carbon disulfide chlorination method adopted in the background technology, the purity of the carbon tetrachloride prepared by the present invention is increased by 4 to 5 percentage points, and the by-products are fully utilized simultaneously, greatly reducing the pollution to the environment.

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Abstract

The invention discloses a preparation method for carbon tetrachloride in the field of preparation of carbon tetrachloride. The preparation method comprises the following steps: step 1, metering carbon disulfide and a chlorine liquid, carrying out mixing, then adding the obtained mixture into a coiled reactor and carrying out a reaction, introducing reaction steam into a fractionating tower, and carrying out first fractionation; step 2, during fractionation of the reaction steam, collecting a first fractionated liquid carbon tetrachloride located at the top of the tower, and carrying out drying so as to prepare an industrial product; step 3, subjecting the tower liquid in the fractionating tower to full reflux, adding excessive carbon disulfide, allowing disulfur dichloride to chlorinate carbon disulfide; step 4, cooling the chlorinated liquid in the tower to 20 DEG C, carrying out crystallization so as to precipitate sulfur, and recycling the precipitated sulfur; step 5, adding a tower parent liquid into a chlorine introduction column, and introducing the chlorine liquid into the chlorine introduction column, and chlorinating excessive carbon disulfide so as to obtain a column chlorinated liquid; step 6, pressing the column chlorinated liquid into the fractionating tower, carrying out fractionation, evaporating a secondary fractionated liquid, and allowing the evaporated secondary fractionated liquid to enter a decomposing tank; and step 7, adding slaked lime into the decomposing tank, decomposing the disulfur dichloride in the secondary fractionated liquid, and subjecting the decomposed decomposition liquid to drying and rectification so as to obtain high-purity carbon tetrachloride. With a scheme provided by the invention, the purity of the carbon tetrachloride is improved; meanwhile, the recycling of by-products is realized.

Description

technical field [0001] The invention relates to the technical field of carbon tetrachloride preparation, in particular to a preparation method of carbon tetrachloride. Background technique [0002] Carbon tetrachloride is a colorless poisonous liquid that can dissolve fat, paint and other substances. It is a volatile liquid with a slightly sweet smell of chloroform. The molecular weight is 153.84, the density at normal temperature and pressure is 1.595g / cm³ (20°C), the boiling point is 76.8°C, the vapor pressure is 15.26kPa (25°C), and the vapor density is 5.3g / L. At the same time, carbon tetrachloride is an ozone-depleting substance, which is a product that needs to be phased out gradually. However, because carbon tetrachloride is inert to the chlorination reaction, it will not bring the chlorination product of the solvent into the product; its boiling point (78 ° C) is compatible with the temperature required by most chlorination reactions, and is convenient for recovery ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/093C07C17/383C07C19/041
CPCC07C17/093C07C17/383
Inventor 王显权
Owner 王显权
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