CN103012051B - Chloroethane distillation separation method and system - Google Patents

Chloroethane distillation separation method and system Download PDF

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Publication number
CN103012051B
CN103012051B CN201310017375.4A CN201310017375A CN103012051B CN 103012051 B CN103012051 B CN 103012051B CN 201310017375 A CN201310017375 A CN 201310017375A CN 103012051 B CN103012051 B CN 103012051B
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monochloroethane
water
chloroethane
separation method
molecular sieve
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CN103012051A (en
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卢爱平
吕宇
徐睿
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JIANGSU YINZHU GROUP HAIBAI TECHNOLOGY CO., LTD.
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JIANGSU YINZHU CHEMICAL GROUP CO Ltd
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Abstract

The invention discloses a chloroethane distillation separation method and a system. The chloroethane distillation separation method comprises the steps that: the temperature of chloroethane is controlled to reduce the solubility of water in chloroethane according to different solubilities of water in chloroethane liquid under different temperatures, water microspheres in the chloroethane liquid is emulsified under low temperature to condense into snowflake solid water, and solid water is filtered by a micropore filter membrane and then absorbed by a molecular sieve to achieve the purpose of dehydrating and drying chloroethane. In addition, the method is low in use cost and simple, and well solves the problems that a large amount of dilute sulfuric acid containing ester compounds is produced during production of treating chloroethane in the prior art, the dilute sulfuric acid can not be recovered, the disposal difficult is large, not only are sources not reasonably utilized but also a large amount of contaminants is produced; and the end treatment cost is high, the chloroethane distillation separation method and the system have good application prospect.

Description

A kind of method and system of monochloroethane rectifying separation
Technical field
The invention belongs to chemical technology field, particularly relate to a kind of method and system of monochloroethane rectifying separation.
Background technology
In monochloroethane production process, monochloroethane drying and dehydrating all adopts the first vitriol oil to absorb the organic species such as monochloroethane mixed gas alcohol ether simultaneously, also absorb moisture wherein, after re-using 4A molecular sieve adsorption, cooling condensation produces monochloroethane finished product, thus produce the dilute sulphuric acid of a large amount of ester-contaning compounds, these dilute sulphuric acids cannot be recycled, and dispose difficulty comparatively large, neither utilize resource rational utilization, produce again a large amount of pollutent, end treatment cost is larger.
Summary of the invention
The object of the invention is to utilize a kind of monochloroethane distillation and separation method and system, be intended to solve the dilute sulphuric acid of a large amount of ester-contaning compounds of the generation that exists in existing process monochloroethane production process, dilute sulphuric acid cannot be recycled, dispose difficulty larger, neither utilize resource rational utilization, produce again a large amount of pollutent, the problem that end treatment cost is larger.
The object of the present invention is to provide a kind of monochloroethane distillation and separation method, described monochloroethane distillation and separation method comprises the following steps: according to the different solubility in monochloroethane liquid of water under differing temps, control monochloroethane temperature, reduce water in monochloroethane solubleness, water particulate at low temperatures in emulsification monochloroethane liquid, condenses into flakes solid water, through millipore filtration membrane filtration solid water wherein, again through molecular sieve adsorption, reach the object that monochloroethane dehydrates.
Further, described monochloroethane distillation and separation method specifically comprises the following steps:
Rectification process is carried out to monochloroethane;
At dehydration tower, carry out the dehydration of monochloroethane;
Solid fraction water is filtered by millipore filter;
4A molecular sieve adsorption moisture.
Further, described millipore filter filters solid fraction water, and monochloroethane water content is lower than 200ppm.
Further, described solid water is through 4A molecular sieve adsorption.
Further, described low temperature monochloroethane reclaims after cold through heat exchange and enters 4A molecular sieve adsorption solvability moisture content, and water-content is lower than 100ppm.
Another object of the present invention is to provide a kind of monochloroethane rectifying separation system, described monochloroethane rectifying separation system comprises:
Monochloroethane dehydration tower;
Strainer, is connected with bottom described monochloroethane dehydration tower, for filter solid water;
Vacuum unit, is connected with described strainer, for controlling the pressure of monochloroethane dehydration tower;
Interchanger, is connected with described strainer, for lowering the temperature to monochloroethane.
Further, described monochloroethane dehydration tower adopts vacuum unit by pressure at 20Kpa--90Kpa.
tool of the present invention has the following advantages:
Monochloroethane distillation and separation method provided by the invention and system, by by monochloroethane rectification process, achieve the high purity of monochloroethane, monochloroethane dewatering unit of the present invention can be arranged according to industrial scale, implement device maximizes, for plant automation operation provides basic guarantee, physics dehydration does not have chemical reaction, a consumption of power and heating power, do not use sulfuric acid, the chemical substances such as caustic soda, no longer produce dilute sulphuric acid, waste lye, do not bring out new environmental pollution factors, the monochloroethane product water content that rectifying separation goes out is low, water content can reach below 100ppm, meet the safety requirements using monochloroethane both at home and abroad, in addition, the inventive method is simple, use cost is low, preferably resolve the dilute sulphuric acid of a large amount of ester-contaning compounds of the generation that exists in existing process monochloroethane production process, dilute sulphuric acid cannot be recycled, dispose difficulty larger, neither utilize resource rational utilization, produce again a large amount of pollutent, the problem that end treatment cost is larger, there is good application prospect.
Accompanying drawing explanation
Fig. 1 is the realization flow figure of the monochloroethane distillation and separation method that the embodiment of the present invention provides.
Fig. 2 is the structured flowchart of the monochloroethane rectifying separation system that the embodiment of the present invention provides.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide a kind of monochloroethane distillation and separation method, this monochloroethane distillation and separation method comprises the following steps: according to the different solubility in monochloroethane liquid of water under differing temps, control monochloroethane temperature, reduce water in monochloroethane solubleness, water particulate at low temperatures in emulsification monochloroethane liquid, condenses into flakes solid water, through millipore filtration membrane filtration solid water wherein, again through molecular sieve adsorption, reach the object that monochloroethane dehydrates.
As a prioritization scheme of the embodiment of the present invention, monochloroethane distillation and separation method specifically comprises the following steps:
Rectification process is carried out to monochloroethane;
At dehydration tower, carry out the dehydration of monochloroethane;
Solid fraction water is filtered by millipore filter;
4A molecular sieve adsorption moisture.
As a prioritization scheme of the embodiment of the present invention, millipore filter filters solid fraction water, and monochloroethane water content is lower than 200ppm.
As a prioritization scheme of the embodiment of the present invention, solid water is through 4A molecular sieve adsorption.
As a prioritization scheme of the embodiment of the present invention, low temperature monochloroethane reclaims after cold through heat exchange and enters 4A molecular sieve adsorption solvability moisture content, and water-content is lower than 100ppm.
Referring to accompanying drawing 1, embodiment of the present invention monochloroethane distillation and separation method and system are described in further detail.
As shown in Figure 1, the monochloroethane distillation and separation method of the embodiment of the present invention comprises the following steps:
S101: monochloroethane is carried out rectifying separation;
S102: through dehydration tower, the water-setting that monochloroethane is separated out forms flakes solid fraction water;
S103: enter millipore filter, elimination solid fraction water;
S104: monochloroethane enters 4A molecular sieve adsorption dissolved water.
Workflow of the present invention is as follows: according to the different solubility in monochloroethane liquid of water under differing temps, control monochloroethane temperature, reduce water in monochloroethane solubleness, be emulsified in the water particulate in monochloroethane liquid simultaneously at low temperatures, condense into flakes solid water, then through millipore filtration membrane filtration solid water wherein, in monochloroethane, moisture content is lower than 200PPM, again through 4A molecular sieve adsorption, in monochloroethane, water content is lower than 100PPM, thus reaches the object that monochloroethane dehydrates.Do not use sulfuric acid to dewater, no longer produce a large amount of spent acid solution, technical solution of the present invention is: arrange monochloroethane dehydration tower 1, vacuum unit 11, strainer 12, interchanger 13, the pressure of monochloroethane dehydration tower 1 is controlled at 20Kpa--90Kpa (absolute pressure root by vacuum unit 11, monochloroethane after rectifying first carries out in monochloroethane dehydration tower 1 after indirect heat exchange cooling, instant vaporization is absorbed heat and lowers the temperature, the solubility with temperature of water in monochloroethane reduces and reduces, the water of separating out forms micro-and is blended in monochloroethane or forms monochloroethane--water-in-oil emulsion, water DEG C at easily condense, now separate out water very quick setting become flakes because of shape water, solid fraction water is filtered through millipore filter 12, monochloroethane water content reduces below 200ppm, low temperature monochloroethane reclaims after cold through heat exchange and enters 4A molecular sieve adsorption solvability moisture content wherein, and control wherein water-content lower than 100ppm, specific embodiment of the present invention is as follows: control monochloroethane dehydration tower 1 pressure at 20Kpa--90Kpa by vacuum unit 11, monochloroethane after rectifying separation reclaims after cold through heat exchange and enters monochloroethane dehydration tower 1 top, while dehydration tower column plate flows downward, the water-setting that monochloroethane is separated out forms flakes solid fraction water, draw from tower bottom, enter millipore filter 12, elimination solid fraction water, in saturated monochloroethane, water content is reduced to below 200ppmm, be pumped to monochloroethane interchanger 13 and reclaim cold, then enter 4A molecular sieve adsorption dissolved water wherein again, monochloroethane water content control is at below 100ppm, after millipore filter 12 inlet and outlet pressure difference rises to 500Kpa, enable another millipore filter for subsequent use 12, add solid fraction water in thermal evolution strainer 12 by chuck and discharge for subsequent use, the monochloroethane gas that vacuum unit 11 is extracted out, still gets back to system through cooling condensation post liquefaction.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (2)

1. a monochloroethane distillation and separation method, it is characterized in that, described monochloroethane distillation and separation method comprises the following steps: according to the different solubility in monochloroethane liquid of water under differing temps, control monochloroethane temperature, reduce water in monochloroethane solubleness, the water particulate at low temperatures in emulsification monochloroethane liquid, condense into flakes solid water, through millipore filtration membrane filtration solid water wherein, then through molecular sieve adsorption, reach the object that monochloroethane dehydrates;
Described monochloroethane distillation and separation method specifically comprises the following steps:
Rectification process is carried out to monochloroethane;
At dehydration tower, carry out the dehydration of monochloroethane;
Solid fraction water is filtered by millipore filter;
4A molecular sieve adsorption moisture;
Described millipore filter filters solid fraction water, and monochloroethane water content is lower than 200ppm;
Described solid water is through 4A molecular sieve adsorption;
Described low temperature monochloroethane reclaims after cold through heat exchange and enters 4A molecular sieve adsorption solvability moisture content, and water-content is lower than 100ppm.
2. a monochloroethane rectifying separation system, is characterized in that, described monochloroethane rectifying separation system comprises:
Monochloroethane dehydration tower;
Strainer, is connected with bottom described monochloroethane dehydration tower, for filter solid water;
Vacuum unit, is connected with described strainer, for controlling the pressure of monochloroethane dehydration tower;
Interchanger, is connected with described strainer, for lowering the temperature to monochloroethane;
Described monochloroethane dehydration tower adopts vacuum unit by pressure at 20Kpa--90Kpa.
CN201310017375.4A 2013-01-17 2013-01-17 Chloroethane distillation separation method and system Active CN103012051B (en)

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CN104892351B (en) * 2015-05-22 2016-07-06 连云港瑞威化工有限公司 A kind of separation method of high-purity chloro ethane
CN108863711B (en) * 2018-08-07 2021-02-19 中化蓝天霍尼韦尔新材料有限公司 Dehydration device and method for 1,1,1,3, 3-pentafluoropropane

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CN202427326U (en) * 2011-12-20 2012-09-12 迈克斯(如东)化工有限公司 Thidiazuron freeze drying kettle
CN102417435A (en) * 2011-12-26 2012-04-18 天津市康科德科技有限公司 Method for purifying chromatographic grade organic solvent 1,2-dichloroethane
CN102586058A (en) * 2012-03-19 2012-07-18 青岛朱雀蓝莓研究技术开发有限公司 Brewing process of blueberry wine base
CN102850178A (en) * 2012-08-24 2013-01-02 江苏振方医药化工有限公司 Method for synthesizing ethyl chloride by using gas phase hydrogen chloride and ethanol

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Application publication date: 20130403

Assignee: Nanjing, Hongze spices company limited

Assignor: Jiangsu Yinzhu Chemical Group Co., Ltd.

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Denomination of invention: Chloroethane distillation separation method and system

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Address after: 223100 No. 20 people's North Road, Hongze County, Jiangsu, Huaian

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Address after: 223100 No. 20 people's North Road, Hongze County, Jiangsu, Huaian

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