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Method for separating acidic dichloroethane mixture

A dichloroethane, separation and treatment technology, applied in ether separation/purification, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc., can solve the problems of difficult treatment, high treatment cost, waste of resources, etc. , to achieve the effect of eliminating environmental pollution, low treatment cost and high production efficiency

Active Publication Date: 2013-12-04
SHAOXING EASTLAKE HIGH TECH CO LTD
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  • Claims
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Problems solved by technology

But utilize this method to process the acidic dichloroethane mixture to have the following problems: (1) need a large amount of lye to go neutralization, cause treatment cost higher; High content, high COD, and containing halogenated hydrocarbons that are difficult to biochemically treat, it is very difficult to handle; (3) hydrogen chloride, 2-chloroethyl phosphonate and dichloroethyl ether cannot be effectively separated in the mixture, which is a serious waste of resources; (4) There is a lot of residual liquid in rectification, and the product recovery rate is low

Method used

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  • Method for separating acidic dichloroethane mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 1000 liters (1260 kg) of acidic dichloroethane mixture at a flow rate of 500 liters per hour through the side line into the first-stage atmospheric rectification tower. The rectification tower is equipped with ceramic corrugated packing, the diameter of the tower is 500 mm, and the total height of the tower is 9 meters , the total height of the packing layer is 8 meters, of which the height of the packing layer in the upper rectifying section from the side feed inlet to the top of the tower is 5 meters (theoretical plate number is 20), and the height of the packing layer in the stripping section below the side feed inlet is 3 meters (theoretical The number of trays is 12), the temperature at the top of the tower is 83-85 °C to obtain a mixture of hydrogen chloride and dichloroethane with a low boiling point, and the temperature at the bottom of the tower is 110-115 °C to obtain dichloroethyl ether and 2-chloroethyl phosphonate with a high boiling point; The hydrogen ...

Embodiment 2

[0027]Put 2000 liters (2520 kg) of acidic dichloroethane mixture at a flow rate of 500 liters per hour through the side line into the first-stage atmospheric rectification tower. The rectification tower is equipped with ceramic corrugated packing. The diameter of the tower is 500 mm and the total height of the tower is 9 meters. , the total height of the packing layer is 8 meters, of which the height of the packing layer in the upper rectifying section from the side feed inlet to the top of the tower is 5 meters (theoretical plate number is 20), and the height of the packing layer in the stripping section below the side feed inlet is 3 meters (theoretical The number of trays is 12), the temperature at the top of the tower is 83-85 °C to obtain a mixture of hydrogen chloride and dichloroethane with a low boiling point, and the temperature at the bottom of the tower is 110-115 °C to obtain dichloroethyl ether and 2-chloroethyl phosphonate with a high boiling point; The hydrogen c...

Embodiment 3

[0029] Put 3000 liters (3780 kg) of acidic dichloroethane mixture into the first-stage atmospheric rectification tower through the side line at a flow rate of 500 liters per hour. The rectification tower is equipped with ceramic corrugated packing. The diameter of the tower is 500 mm and the total height of the tower is 9 meters. , the total height of the packing layer is 8 meters, of which the height of the packing layer in the upper rectifying section from the side feed inlet to the top of the tower is 5 meters (theoretical plate number is 20), and the height of the packing layer in the stripping section below the side feed inlet is 3 meters (theoretical The number of trays is 12), the temperature at the top of the tower is 83-85 °C to obtain a mixture of hydrogen chloride and dichloroethane with a low boiling point, and the temperature at the bottom of the tower is 110-115 °C to obtain dichloroethyl ether and 2-chloroethyl phosphonate with a high boiling point; The hydrogen ...

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Abstract

The invention discloses a method for separating an acidic dichloroethane mixture. The acidic dichloroethane mixture is a mixture of dichloroethane, hydrogen chloride, 2-chloroethyl phosphonate and dichloroether. The method comprises the following steps of: adding the acidic dichloroethane mixture into a one-level normal-pressure rectifying tower in a way of side line and controlling the temperature of the tower top to be between 80 and 86 DEG C and the temperature of the tower bottom to be between 110 and 120 DEG C to obtain a tower top fraction 1 and a tower bottom fraction 1; adding the tower top fraction 1 into a two-level normal-pressure rectifying tower in the way of side line, and controlling the temperature of the tower top to be between 80 and 83 DEG C and the temperature of the tower bottom to be between 83 and 86 DEG C to obtain a tower top fraction 2 which is a hydrogen chloride gas and a tower bottom fraction 2 which is dichloroethane; and adding the tower bottom fraction 1 into a three-level normal-pressure rectifying tower in the way of side line, and controlling the tower reflux ratio to be between 1 and 1.5, the relative vacuum degree to be between 0.09 and 0.095MPa, the temperature of the tower top to be between 100 and 110 DEG C and the temperature of the tower bottom to be between 120 and 130 DEG C to obtain a tower top fraction 3 which is dichloroether and a tower bottom fraction 3 which is 2-chloroethyl phosphonate. By the method, the mixing components in the acidic dichloroethane can be completely separated out; the purity of the separated products is high; and the economic benefit is relatively good.

Description

technical field [0001] The invention relates to a method for separating and treating an acidic dichloroethane mixture, in particular to a method for separating and treating a by-product acidic dichloroethane mixture obtained in the production of a plant growth regulator ethephon. Background technique [0002] Dichloroethane, colorless and transparent liquid, boiling point 83.5 ℃, melting point -35.3 ℃, relatively stable in nature, used as a solvent for fats, oils, waxes, rubber, tar, pitch, resins, ethyl cellulose, etc., also used in organic Synthesis and paint manufacturing. [0003] The last step of the acid hydrolysis production process of the plant growth regulator ethephon is to pass hydrogen chloride gas into 2-chloroethyl phosphonate, and the reaction produces ethephon and a large amount of acidic dichloroethane at the same time. The reaction equation is as follows: [0004] . [0005] According to above-mentioned reaction, hydrogen chloride gas excess is more in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/045C07C17/383C07C43/12C07C41/42C07F9/40C01B7/01
Inventor 张国富季国炎丁成荣葛铭季国尧季小英
Owner SHAOXING EASTLAKE HIGH TECH CO LTD
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