阅读说明：本技术 一种生产纯度高且水分含量少的液氯的方法 (Method for producing liquid chlorine with high purity and low moisture content ) 是由 张家清 于 2020-07-02 设计创作，主要内容包括：本发明公开了一种生产纯度高且水分含量少的液氯的方法,步骤如下：步骤1：所述缓冲罐对电解后的干燥氯气去除杂质和酸沫,并重新进行气化处理；步骤2：所述分配台对干净的氯气进行再分配,将去液化的氯气进行下一步的热交换处理；步骤3：所述螺杆机组循环提供液态氟利昂,作为反应物参与反应；步骤4：所述液化器将氯气与液态氟利昂进行热交换,液态氟利昂气化成气态氟利昂,大部分氯气液化成液氯,部分氯气重新处理；步骤5：所述回螺杆机组将气态氟利昂重新液化,循环利用。本发明解决了电解后的氯气直接液化,纯度不够高,且未液化的氯气直接排出存在浪费现象的问题。(The invention discloses a method for producing liquid chlorine with high purity and low moisture content, which comprises the following steps: step 1: the buffer tank removes impurities and acid foam from the electrolyzed dry chlorine and carries out gasification treatment again; step 2: the distribution table redistributes the clean chlorine and carries out the next heat exchange treatment on the chlorine subjected to liquefaction removal; and step 3: the screw machine set circularly provides liquid Freon which is used as a reactant to participate in the reaction; and 4, step 4: the liquefier exchanges heat between chlorine and liquid Freon, the liquid Freon is gasified into gaseous Freon, most of the chlorine is gasified into liquid chlorine, and part of the chlorine is reprocessed; and 5: the screw returning unit re-liquefies the gaseous Freon for recycling. The invention solves the problems that the electrolyzed chlorine is directly liquefied, the purity is not high enough, and the unliquefied chlorine is directly discharged to cause waste.)

1. A method for producing liquid chlorine with high purity and low moisture content is characterized by comprising the following steps:

step 1: the buffer tank removes impurities and acid foam from the electrolyzed dry chlorine and carries out gasification treatment again;

step 2: the distribution table redistributes the clean chlorine and carries out the next heat exchange treatment on the chlorine subjected to liquefaction removal;

and step 3: the screw machine set circularly provides liquid Freon which is used as a reactant to participate in the reaction;

and 4, step 4: the liquefier exchanges heat between chlorine and liquid Freon, the liquid Freon is gasified into gaseous Freon, most of the chlorine is gasified into liquid chlorine, and part of the chlorine is reprocessed;

and 5: the screw returning unit re-liquefies the gaseous Freon for cyclic utilization;

step 6: the distribution table redistributes the non-liquefied chlorine gas;

and 7: the filling is to pump the liquid chlorine in the liquid chlorine storage tank to a filling distribution table by a magnetic pump for filling.

2. The method for producing liquefied chlorine with high purity and low moisture content as claimed in claim 1, wherein the treatment of chlorine gas in the buffer tank in step 1 is as follows:

step 1-1: the ultra-low temperature cooler is used for liquefying the electrolyzed dry chlorine gas, and the theoretical cooling temperature of the ultra-low temperature cooler is-10 ℃ to-152 ℃;

step 1-2: the chlorine bottle is used for temporarily storing the liquid chlorine, the chlorine bottle can deflect in actual use, the too large deflection angle can cause insufficient gasification space of the liquid chlorine, and the deflection angle is calculated according to the volume of the buffer tank and is related to the inner diameter and the length of the chlorine bottle;

step 1-3: the copper pipe is used as a conveying tool of liquid chlorine, and an anti-corrosion layer is arranged on the inner surface of the copper pipe;

step 1-4: the jar body has certain gasification space when liquid chlorine gasification, the volume of the jar body should satisfy actual gasification requirement:

the standard chlorine bottle can contain 500kg of liquid chlorine, the inner diameter is 600mm, the length is 1800mm, the relative density of the liquid chlorine is 1.47, the filling coefficient of the chlorine bottle is 1.2kg/L, when the chlorine bottle is filled with 500kg of liquid chlorine, the volume of the liquid chlorine is 326L, the filling volume accounts for 81 percent of the inner part of the chlorine bottle, the gas volume is 19 percent, and the inflow volume of the liquid chlorine acceptable by the tank body is 78L;

step 1-5: the vacuum regulator gasifies the liquid chlorine containing impurities in the tank body to convert the liquid chlorine into chlorine;

step 1-6: the filter material can capture impurities and liquid drops in the chlorine gas and discharge clean chlorine gas;

step 1-7: the glass wool is the main material of the filter material, and the impurities in the glass wool are removed by replacing the glass wool.

3. The method of claim 1, wherein the liquefied chlorine gas is treated by the liquefier in step 4 as follows:

step 4-1: the heat exchange device carries out heat exchange on the liquefied chlorine and the liquid Freon, the liquefied chlorine and the liquid Freon are respectively conveyed by two pipelines, a heat exchange wall is arranged between the two pipelines, the temperature of the liquid Freon is below zero DEG C, the boiling point of the liquid Freon is-29.8 ℃, the temperature of the chlorine is higher than-29.8 ℃, when the liquid Freon is contacted with the chlorine through the heat exchange wall, the liquid Freon is boiled to be gasified, the chlorine is liquefied after being subjected to low temperature, and the gasification temperature cannot be reached after the liquid chlorine is liquefied because the gasification temperature of the liquid chlorine is 80 ℃, the liquid state is always kept, and for improving the heat transfer efficiency, a split-path partition plate is arranged in the heat exchange device to divide a tube path into two paths, four paths, six paths, eight paths and the like, so that the flow section of the heat exchanger is reduced, the flow rate;

step 4-2: the gas-liquid separation device separates the gas-liquid mixture of chlorine after heat exchange and discharges chlorine gas and liquid chlorine respectively.

4. The method for producing liquefied chlorine having high purity and low moisture content as claimed in claim 3, wherein the treatment of the deliquified chlorine gas by the liquefier in step 4-2 is as follows:

step 4-2-1: the fractionating tower is used for fractionating a gas-liquid mixture, liquid chlorine at the bottom end of the fractionating tower is directly discharged, and gas at the upper end of the fractionating tower is subjected to next-step treatment;

step 4-2-2: the refrigerator is arranged at the top end of the fractionating tower, the suction temperature of the refrigerator is-32-5 ℃, and demisting treatment is carried out on tail chlorine which is not completely heat-exchanged by the heat exchange device;

step 4-2-3: the gas washing tower is provided with multiple stages, and part of freon gas mixed in tail chlorine is washed by water and removed.

5. The method for producing liquid chlorine with high purity and low moisture content according to claim 1, wherein the screw returning process in step 5 is as follows:

step 5-1: the cooling compressor is used for cooling and compressing gaseous Freon, the condition that the Freon is converted from the gaseous state into the liquid state is low temperature or high pressure, and the cooling compressor can be used for liquefying the Freon at high efficiency;

step 5-2: and the screw machine set is the screw machine set in the step 3, wherein the liquid Freon is recycled.

Technical Field

The invention relates to the field of liquid chlorine preparation, in particular to a method for producing liquid chlorine with high purity and low moisture content.

Background

The liquid chlorine is yellow green oily liquid, is toxic, boils at minus 34.6 ℃ under the standard condition, is stored in a steel cylinder with 0.5-1.0 t if the liquid chlorine has strong corrosivity to steel in case of water, and is stored in a dry, light-proof and fireproof place. The liquid chlorine is gasified to become chlorine and is added into water by a chlorine adding device. The chlorine is an active substance and can react with most elements (or compounds), whether the alkali is prepared by electrolysis by an ion membrane method or by electrolysis by a metal anode method, the co-produced chlorine always has certain impurities, and for some application occasions, the chlorine with higher purity is needed, and the dried raw material chlorine cannot meet the requirement. In the chlorine liquefaction process, most of chlorine is condensed, non-condensable gas is discharged as tail gas, the purity of liquid chlorine is improved, the volume of the chlorine is greatly reduced after the chlorine is liquefied, the density of the chlorine is 3.2kg/m3, the density of the liquid chlorine can reach 13-16kg/m3, and the chlorine is convenient to transport and store. Liquid chlorine is a basic chemical raw material, can be used in industries such as metallurgy, textile, papermaking and the like, and is a raw material for synthesizing hydrochloric acid, polyvinyl chloride, plastics and pesticides.

The electrolyzed chlorine gas is directly liquefied, although most of the chlorine gas is condensed, the non-condensable gas is discharged as tail gas, the purity of the liquid chlorine is improved, but the content of impurities in the liquid chlorine is still high and the purity is not enough, and the non-liquefied chlorine gas and the non-condensable gas are discharged as the tail gas together, so that a large chlorine gas waste phenomenon exists in the process of preparing the liquid chlorine; therefore, the market is urgently in need of developing a method for producing liquid chlorine with high purity and low moisture content to help people to solve the existing problems.

Disclosure of Invention

The invention aims to provide a method for producing liquid chlorine with high purity and low moisture content, which aims to solve the problems that the chlorine gas after electrolysis is directly liquefied, the purity is not high enough, and the chlorine gas which is not liquefied is directly discharged to cause waste.

In order to achieve the purpose, the invention provides the following technical scheme: a method for producing liquid chlorine with high purity and low moisture content comprises the following steps:

step 1: the buffer tank removes impurities and acid foam from the electrolyzed dry chlorine and carries out gasification treatment again;

step 2: the distribution table redistributes the clean chlorine and carries out the next heat exchange treatment on the chlorine subjected to liquefaction removal;

and step 3: the screw machine set circularly provides liquid Freon which is used as a reactant to participate in the reaction;

and 4, step 4: the liquefier exchanges heat between chlorine and liquid Freon, the liquid Freon is gasified into gaseous Freon, most of the chlorine is gasified into liquid chlorine, and part of the chlorine is reprocessed;

and 5: the screw returning unit re-liquefies the gaseous Freon for cyclic utilization;

step 6: the distribution table redistributes the non-liquefied chlorine gas;

and 7: the filling is to pump the liquid chlorine in the liquid chlorine storage tank to a filling distribution table by a magnetic pump for filling.

Preferably, the treatment of the buffer tank on the chlorine gas in the step 1 is specifically as follows:

step 1-1: the ultra-low temperature cooler is used for liquefying the electrolyzed dry chlorine gas, and the theoretical cooling temperature of the ultra-low temperature cooler is-10 ℃ to-152 ℃;

step 1-2: the chlorine bottle is used for temporarily storing the liquid chlorine, the chlorine bottle can deflect in actual use, the too large deflection angle can cause insufficient gasification space of the liquid chlorine, and the deflection angle is calculated according to the volume of the buffer tank and is related to the inner diameter and the length of the chlorine bottle;

step 1-3: the copper pipe is used as a conveying tool of liquid chlorine, and an anti-corrosion layer is arranged on the inner surface of the copper pipe;

step 1-4: the jar body has certain gasification space when liquid chlorine gasification, the volume of the jar body should satisfy actual gasification requirement:

the standard chlorine bottle can contain 500kg of liquid chlorine, the inner diameter is 600mm, the length is 1800mm, the relative density of the liquid chlorine is 1.47, the filling coefficient of the chlorine bottle is 1.2kg/L, when the chlorine bottle is filled with 500kg of liquid chlorine, the volume of the liquid chlorine is 326L, the filling volume accounts for 81 percent of the inner part of the chlorine bottle, the gas volume is 19 percent, and the inflow volume of the liquid chlorine acceptable by the tank body is 78L;

step 1-5: the vacuum regulator gasifies the liquid chlorine containing impurities in the tank body to convert the liquid chlorine into chlorine;

step 1-6: the filter material can capture impurities and liquid drops in the chlorine gas and discharge clean chlorine gas;

step 1-7: the glass wool is the main material of the filter material, and the impurities in the glass wool are removed by replacing the glass wool.

Preferably, the treatment of the deliquified chlorine gas by the liquefier in the step 4 is specifically as follows:

step 4-1: the heat exchange device carries out heat exchange on the liquefied chlorine and the liquid Freon, the liquefied chlorine and the liquid Freon are respectively conveyed by two pipelines, a heat exchange wall is arranged between the two pipelines, the temperature of the liquid Freon is below zero DEG C, the boiling point of the liquid Freon is-29.8 ℃, the temperature of the chlorine is higher than-29.8 ℃, when the liquid Freon is contacted with the chlorine through the heat exchange wall, the liquid Freon is boiled to be gasified, the chlorine is liquefied after being subjected to low temperature, and the gasification temperature cannot be reached after the liquid chlorine is liquefied because the gasification temperature of the liquid chlorine is 80 ℃, the liquid state is always kept, and for improving the heat transfer efficiency, a split-path partition plate is arranged in the heat exchange device to divide a tube path into two paths, four paths, six paths, eight paths and the like, so that the flow section of the heat exchanger is reduced, the flow rate;

step 4-2: the gas-liquid separation device separates the gas-liquid mixture of chlorine after heat exchange and discharges chlorine gas and liquid chlorine respectively.

Preferably, the treatment of the deliquified chlorine gas by the liquefier in the step 4-2 is as follows:

step 4-2-1: the fractionating tower is used for fractionating a gas-liquid mixture, liquid chlorine at the bottom end of the fractionating tower is directly discharged, and gas at the upper end of the fractionating tower is subjected to next-step treatment;

step 4-2-2: the refrigerator is arranged at the top end of the fractionating tower, the suction temperature of the refrigerator is-32-5 ℃, and demisting treatment is carried out on tail chlorine which is not completely heat-exchanged by the heat exchange device;

step 4-2-3: the gas washing tower is provided with multiple stages, and part of freon gas mixed in tail chlorine is washed by water and removed.

Preferably, the screw returning unit in the step 5 is specifically processed as follows:

step 5-1: the cooling compressor is used for cooling and compressing gaseous Freon, the condition that the Freon is converted from the gaseous state into the liquid state is low temperature or high pressure, and the cooling compressor can be used for liquefying the Freon at high efficiency;

step 5-2: and the screw machine set is the screw machine set in the step 3, wherein the liquid Freon is recycled.

Compared with the prior art, the invention has the beneficial effects that:

1. the method comprises the steps of firstly liquefying electrolyzed chlorine gas to obtain liquid chlorine containing impurities, converting the liquid chlorine into the liquid chlorine, regasifying the liquid chlorine, conveniently controlling the internal volume of the whole buffer tank, directly discharging gas into the buffer tank, not easily controlling the gas discharge speed and the tank body volume, regasifying the liquid chlorine in the buffer tank, and then removing the impurities and acid foam from the liquid chlorine containing the impurities, wherein the glass wool is fluorine silicon oil demisting glass wool, only liquid drops and the impurities in the glass wool are captured, and the impurities are removed by replacing the glass wool.

2. After the gas-liquid separation device is used for separating chlorine from liquid chlorine, the separation operation is carried out through the fractionating tower, the tail chlorine is retreated, the Freon gas in the tail chlorine is washed away, the clean chlorine is retreated through the heat exchange device to obtain the liquid chlorine, and the waste phenomenon that the chlorine is directly discharged is avoided.

3. The invention removes impurities from the electrolyzed chlorine gas through continuous gasification and liquefaction processes, so that the purity of the finally filled liquid chlorine is high and is more than 99.6 percent, wherein the moisture content is less than 400ppm, and the requirement of high-purity liquid chlorine is met.

Drawings

FIG. 1 is a process flow diagram of a method of producing liquid chlorine having high purity and low moisture content in accordance with the present invention;

FIG. 2 is a process flow diagram of buffer tank gasification according to the present invention;

FIG. 3 is a process flow diagram of the heat exchange of the liquefier of the present invention;

FIG. 4 is a flow chart of the separation process of the gas-liquid separation apparatus according to the present invention;

fig. 5 is a diagram of the working steps of the screw returning unit of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

Referring to fig. 1-5, an embodiment of the present invention is shown: a method for producing liquid chlorine with high purity and low moisture content comprises the following steps:

step 1: the buffer tank removes impurities and acid foam from the electrolyzed dry chlorine gas, and the dry chlorine gas is gasified again to remove the impurities, so that the purity of the finally prepared liquid chlorine is ensured;

step 2: the distribution table redistributes the clean chlorine, carries out the next heat exchange treatment on the liquefied chlorine, liquefies the chlorine after being subjected to low temperature through the heat exchange with liquid Freon, and keeps the chlorine in a liquid state all the time due to high gasification temperature;

and step 3: the screw machine set circularly provides liquid Freon which is used as a reactant to participate in the reaction, and the liquid Freon can be repeatedly utilized, so that the production cost in the production process is saved;

and 4, step 4: the liquefier exchanges heat between chlorine and liquid Freon, the liquid Freon is gasified into gaseous Freon, most of the chlorine is gasified into liquid chlorine, and part of the chlorine is reprocessed;

and 5: the screw returning unit re-liquefies the gaseous Freon for recycling, and the liquefied Freon enters the screw unit again;

step 6: the distribution table redistributes the chlorine which is not liquefied, the chlorine which is not liquefied can continuously participate in the reaction, the waste of the chlorine which is electrolyzed is avoided, and only part of the chlorine with more content is converted into liquid chlorine finally;

and 7: the filling is that liquid chlorine in the liquid chlorine storage tank is pumped to a filling distribution table by a magnetic pump to be filled, and the content of filled chlorine bottles is 0.5-1.0 t.

Further, the treatment of the buffer tank on the chlorine gas in the step 1 is specifically as follows:

step 1-1: the ultra-low temperature cooler is used for liquefying the electrolyzed dry chlorine, the theoretical cooling temperature of the ultra-low temperature cooler is-10 ℃ to-152 ℃, the chlorine is rapidly liquefied, and the chlorine is completely liquefied;

step 1-2: the chlorine bottle is used for temporarily storing the liquid chlorine, the chlorine bottle can deflect in actual use, the too large deflection angle can cause insufficient gasification space of the liquid chlorine, and the deflection angle is calculated according to the volume of the buffer tank and is related to the inner diameter and the length of the chlorine bottle;

step 1-3: the copper pipe is used as a conveying tool of liquid chlorine, and the inner surface of the copper pipe is provided with an anti-corrosion layer;

step 1-4: the jar body has certain gasification space when liquid chlorine gasification, prevents that liquid chlorine from because of the jar body explosion that volume inflation leads to when the gasification, and the volume of the jar body should satisfy the gasification requirement of reality:

the standard chlorine bottle can be filled with 500kg of liquid chlorine, the inner diameter is 600mm, the length is 1800mm, the relative density of the liquid chlorine is 1.47, the filling coefficient of the chlorine bottle is 1.2kg/L, when the chlorine bottle is filled with 500kg of liquid chlorine, the volume of the liquid chlorine is 326L, the filling volume accounts for 81 percent of the inner part of the chlorine bottle, the gas volume is 19 percent, the inflow volume of the liquid chlorine acceptable by the tank body is 78L, and certain pressure can be caused to the tank body when the inflow liquid chlorine exceeds the volume, so that the service time of the tank body is shortened;

step 1-5: the vacuum regulator gasifies the liquid chlorine containing impurities in the tank body, the gasification efficiency is high, the liquid chlorine is converted into chlorine, and the conversion rate almost reaches 100%;

step 1-6: the filter material can capture impurities and liquid drops in the chlorine gas, and the filter material is replaceable and discharges clean chlorine gas side by side;

step 1-7: the glass wool is the main material of the filter material, and the impurities in the filter material are removed by replacing the glass wool.

Further, the treatment of the deliquified chlorine gas by the liquefier in step 4 is specifically as follows:

step 4-1: the heat exchange device carries out heat exchange on the liquefied chlorine and the liquid Freon, the liquefied chlorine and the liquid Freon are respectively conveyed by two pipelines, the two pipelines do not need to be connected, the two substances respectively flow in the pipelines, a heat exchange wall is arranged between the two pipelines to play a role of heat conduction, the temperature of the liquid Freon is below zero DEG centigrade, the boiling point is-29.8 ℃, the temperature of the chlorine is higher than-29.8 ℃, when the liquid Freon is contacted with the chlorine through the heat exchange wall, the liquid Freon is boiled to be gasified, the chlorine is liquefied after being subjected to low temperature, the gasification temperature of the liquid chlorine is 80 ℃, so that the gasification temperature can not be reached after the liquid chlorine is liquefied, the liquid state is kept all the time, and for improving the heat transfer efficiency, a split-path partition plate is arranged in the heat exchange device to divide a tube path into two paths, four paths, six paths, eight paths and the like, the flow cross section of the heat exchanger is reduced, the flow, the heat exchange efficiency is increased;

step 4-2: the gas-liquid separation device separates the gas-liquid mixture of chlorine after heat exchange, and discharges chlorine gas and liquid chlorine respectively, wherein the liquid chlorine is a finished product required by the reaction, and the chlorine gas also needs to be subjected to subsequent treatment.

Further, the treatment of the deliquified chlorine gas by the liquefier in the step 4-2 is specifically as follows:

step 4-2-1: the fractionating tower is used for fractionating a gas-liquid mixture, liquid chlorine at the bottom end of the fractionating tower is directly discharged, a discharged pipeline has strong corrosion resistance, the discharged pipeline extends into the fractionating tower, the joint is sealed, the liquid chlorine is prevented from leaking, the liquid chlorine has certain toxicity, and gas at the upper end of the fractionating tower is subjected to next treatment;

step 4-2-2: the refrigerator is arranged at the top end of the fractionating tower, chlorine gas flows upwards due to the property of the chlorine gas, namely, the chlorine gas enters the refrigerator, the suction temperature of the refrigerator is-32-5 ℃, and demisting treatment is carried out on tail chlorine which is not completely heat exchanged by the heat exchange device;

step 4-2-3: the gas washing tower is provided with multiple stages, and part of freon gas mixed in tail chlorine is washed by water and removed, so that the purity of the discharged chlorine is ensured, and unnecessary substances are not contained.

Further, the screw returning unit in the step 5 is specifically processed as follows:

step 5-1: the cooling compressor is used for cooling and compressing the gaseous Freon, the condition that the Freon is converted from the gaseous state into the liquid state is low temperature or high pressure, the cooling compressor can be used for liquefying the Freon at high efficiency, and the Freon can be reused for heat exchange treatment through the liquefying treatment of the Freon;

step 5-2: the screw machine set is the screw machine set in the step 3, wherein the liquid Freon is recycled, and no extra substance is lost in the whole heat exchange device.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.