CN111647905A - Process control method for reducing damage of electrolytic cell shutdown to cathode chamber - Google Patents
Process control method for reducing damage of electrolytic cell shutdown to cathode chamber Download PDFInfo
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- CN111647905A CN111647905A CN202010540278.3A CN202010540278A CN111647905A CN 111647905 A CN111647905 A CN 111647905A CN 202010540278 A CN202010540278 A CN 202010540278A CN 111647905 A CN111647905 A CN 111647905A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
- C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
- C25B15/02—Process control or regulation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
- C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
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Abstract
The invention relates to a process control method for reducing damage of an electrolytic cell shutdown to a cathode chamber, which comprises an electrolytic cell (1), a brine head tank (2), an alkali head tank (3), a cathode circulating tank (4) and an anode circulating tank (5); the electrolytic cell gradually reduces the adding amount of the brine and the flow of 15 percent of the return brine in the process of reducing the current, and the electrolytic cell is stopped and then is connected with a power supply 2:1, adding a proper amount of liquid caustic soda into brine to ensure that hypochlorous acid and chlorine with strong oxidizing property in an anode chamber can be quickly generated into sodium hypochlorite with strong stability and weak oxidizing property after the electrolytic cell is stopped, thereby reducing the damage of the cathode chamber caused by stopping. The method has the characteristics of low cost, safety, reliability and simple process.
Description
Technical Field
The invention belongs to the technical field of chlor-alkali production, and particularly relates to a process control method for reducing damage of an electrolytic cell shutdown to a cathode chamber, which is particularly suitable for a bipolar type ionic membrane electrolytic cell.
Background
After decades of development, the multipole type ion membrane electrolytic cell has attracted attention in the aspects of energy saving, environmental protection and the like, and gradually becomes the standard allocation of the current chlor-alkali. The multi-pole type ion-exchange membrane electrolytic cell mainly comprises a unit cell and an ion-exchange membrane, wherein a metal composite partition plate divides the unit cell into a cathode chamber and an anode chamber. The brine after the second refining is electrolyzed and twice acid adding is carried out before the electrolysis, the first acid adding is used for removing carbonate ions which are excessively added during the first refining of the brine, the second acid adding is used for neutralizing hydroxide ions transferred from a cathode chamber, the purposes of inhibiting side reactions of the anode chamber and improving the purity of chlorine are achieved, and the in-tank brine during the operation of the electrolytic cell consists of refined brine and 15% returned brine from an anode circulating tank.
After the electrolytic cell is stopped, the brine in the anode chamber contains a certain amount of chlorine, and the ratio of the flow of the refined brine to the flow of the soft water is 2:1 weak brine (2: 1 brine for short) replaces the anode chamber of the electrolytic cell for a long time, and chlorine gas is discharged from the electrolytic cell. Chlorine in the brine reacts with water to generate hypochlorous acid and hydrochloric acid, so that the brine is acidic, the chemical properties of the hypochlorous acid and the chlorine are extremely active in an acidic environment, the oxidizability is extremely strong, and the anode chamber is extremely strong in electron-capturing capacity. When the electrolytic cell is operated, the chlorine ions in the anode chamber lose electrons under the action of electric field force, and the electrons enter the cathode chamber from the anode chamber through the metal composite partition plate. The direction of the electrons after the electrolytic cell is stopped is opposite to that of the electrons when the electrolytic cell is operated, so that the current generated after the electrolytic cell is stopped is called reverse current in the chlor-alkali industry. The chlorine and the hypochlorous acid in the brine can form reverse current after the electrolytic cell is stopped, and electrochemical corrosion can also be formed in the cathode chamber (because the reverse current and the power of the electrochemical corrosion formed in the cathode chamber are both from the hypochlorous acid and the chlorine in the brine, and are synchronous, so the chlor-alkali industry generally considers that the electrochemical corrosion formed in the cathode chamber is caused by the reverse current and is actually parallel. Particularly, the brine containing chlorine and hypochlorous acid can not be discharged in time under the condition of power loss of the whole plant, and the influence on the electrolytic cell and the ion exchange membrane is particularly serious.
The prior art method for inhibiting electrochemical corrosion of cathode chamber: (1) UPS polarized power supply: after the electrolytic cell is stopped, the UPS is used for supplying power to the electrolytic cell, so that the electrolytic cell operates at low current (100A), a large amount of 2:1 saline water is supplied to the electrolytic cell, the content of chlorine and hypochlorous acid in the saline water of the anode chamber is halved, the electrochemical corrosion of the cathode chamber is inhibited, and the damage of the chlorine and the hypochlorous acid to the ion exchange membrane is reduced. The method has the advantages of safety and reliability, and has the disadvantage of high equipment cost; (2) the application of the C-DCDS direct current knife switch comprises the following steps: the electrolyzer is an electricity-consuming device during operation, and the electrolyzer after shutdown is converted into a primary battery pack with a complex structure by the electricity-consuming device. After the electrolytic cell is stopped, the C-DCDS direct current knife switch in the middle of the electrolytic cell is disconnected, and the electrolytic cell is changed into two independent grounding paths from one grounding path, so that the back electromotive force is halved. The method has the advantages of low equipment cost and the defect that the damage of hypochlorous acid and chlorine gas in the brine of the anode chamber to the ion exchange membrane cannot be quickly reduced.
In conclusion, chlorine and hypochlorous acid in the brine can form reverse current after the electrolytic cell is stopped, and electrochemical corrosion can also be formed in the cathode chamber, so that the coating of the cathode chamber falls off, and the metal nickel loses electrons and is converted into nickel ions. The coating falls off and is attached to the ion exchange membrane to increase the cell voltage, the power consumption is increased, the service life of the protective cell frame without the coating can be rapidly reduced, and therefore, a large amount of capital is required to be invested in chlor-alkali production to effectively reduce the damage of the shutdown of the electrolytic cell to the cathode chamber.
Disclosure of Invention
The invention is suitable for a bipolar type ion membrane electrolytic cell, and aims to reduce the oxidability of an anode chamber after the bipolar type ion membrane electrolytic cell is stopped, inhibit the damage of electrochemical corrosion to a cathode chamber, prolong the service life of a cell frame and an ion exchange membrane and reduce the influence of coating falling on the ion exchange membrane.
The invention adopts the following technical scheme: a process control method for reducing damage of an electrolytic cell shutdown to a cathode chamber comprises an electrolytic cell (1), a brine head tank (2), an alkali head tank (3), a cathode circulating tank (4) and an anode circulating tank (5); an anode part: the secondary refined brine (a) enters a brine head tank and automatically flows into an anode chamber of an electrolytic cell (1) through a refined brine header pipe (12) under the action of head difference, the secondary refined brine is electrolyzed in the anode chamber under the action of direct current to generate chlorine and light brine, the light brine automatically flows into an anode circulating tank (5), 15% of the light brine is returned to a brine pipe through 15% of the water pipe to be introduced into the refined brine header pipe of the electrolytic cell to protect a titanium pipe; a cathode portion: the catholyte enters the alkali elevated tank (3) and is automatically fed to an outlet pipe (15) of the alkali elevated tank from a catholyte header pipe under the action of the elevation difference and then enters the cathode chamber; electrolyzing in a cathode chamber to generate hydrogen and 32% liquid caustic soda, and feeding the 32% liquid caustic soda into a cathode circulating tank (4); a 2:1 brine pipeline (13) is arranged on the refined brine main pipe (12); introducing soft water (a) into a 2:1 brine pipeline (13) through a soft water pipeline, arranging a 2:1 brine and alkali adding pipeline (14) on an outlet pipe (15) of the alkali elevated tank, connecting an inlet of the 2:1 brine and alkali adding pipeline (14) with the outlet pipe (15) of the alkali elevated tank, and connecting an outlet with the 2:1 brine pipeline (13); after the electrolytic cell is shut down, the electrolytic cell is switched to a 2:1 brine alkali adding pipeline (14) to supply the brine alkali solution to the electrolytic cell in a volume ratio of 2:1, adding a proper amount of liquid alkali into the saline water to ensure that the anode outlet of each electrolytic cell can quickly display alkalinity.
The process control method for reducing the damage of the shutdown of the electrolytic cell to the cathode chamber comprises the steps that a refined brine header pipe (12) is provided with a tank brine stop valve (11), a 2:1 brine stop valve (10) is arranged on a 2:1 brine pipeline (13), a 2:1 brine pure water flow regulating valve (7) is arranged on a soft water pipeline, a 2:1 brine alkali adding flow regulating valve (8) is arranged on a 2:1 brine alkali adding pipeline (14), and when the electrolytic cell is shut down, the tank brine stop valve (11) is closed, the 2:1 brine stop valve (10) is opened, and the 2:1 brine pure water flow regulating valve (7) and the 2:1 brine alkali adding flow regulating valve (8) are opened simultaneously.
According to the process control method for reducing damage of the shutdown of the electrolytic cell to the cathode chamber, an anode outlet pH monitor (6) is arranged on a 15% return brine pipeline and is in linkage control with a 2:1 brine alkalinity adding flow regulating valve (8).
In the process control method for reducing the damage of the shutdown of the electrolytic cell to the cathode chamber, when the pH value of the anode outlet of the process control method is more than 8, the 2:1 saline water and alkali adding flow regulating valve (8) is closed; the addition of base to the 2:1 brine was stopped and the replacement of the anode compartment with 2:1 brine was continued until the hypochlorite ion content was low.
The process control method for reducing the damage of the electrolytic bath shutdown to the cathode chamber adopts a DCS method to carry out automatic control. Acid addition flow (6) of refined brine, acid addition flow (14) of brine entering a tank, 15% return brine flow (10), 2:1 saline water alkali addition flow (8), 2: the 1 saline water alkali adding duration, the 2:1 saline water flow and the 2:1 saline water replacement duration are all automatically controlled by the DCS
Adjusting the pH value of the anode chamber to inhibit electrochemical corrosion and damage to the membrane: chlorine and hypochlorous acid in the brine are neutral in electricity, the electrolysis bath can move towards the cathode chamber together with hypochlorous acid and migration water after stopping, damage is caused to the membrane on the ion exchange membrane, the chlorine and the hypochlorous acid with strong oxidizing property in the brine can quickly generate sodium hypochlorite with relatively stable chemical property by adding alkali to the anode chamber, the damage of electrochemical corrosion to the cathode chamber can be effectively inhibited, the hypochlorite shows negative electricity to the outside, the membrane has the effect of repelling anions, and the damage of the hypochlorite to the membrane is inhibited. The method has the advantages of low equipment cost, safety and reliability, can quickly reduce the oxidization of the brine in the anode chamber, can quickly reduce the damage of the shutdown to the electrolytic cell and the ion exchange membrane particularly under the condition of power loss of the whole plant,
the invention has the beneficial effects that: after the electrolytic cell is stopped, the hypochlorous acid with strong oxidizing property and the chlorine gas in the anode chamber are quickly generated into the sodium hypochlorite with strong stability and weak oxidizing property, so that the electrochemical corrosion of the cathode chamber is effectively inhibited, the service lives of the electrolytic cell frame and the ion exchange membrane are prolonged, the influence of the falling of the coating on the operation of the ion membrane is reduced, the power consumption is reduced, and the production cost is saved.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
In fig. 1: an electrolytic cell 1, a brine head tank 2, an alkali head tank 3, a cathode circulating tank 4, an anode circulating tank 5, an anode outlet pH monitor 6, a 2:1 brine pure water flow regulating valve 7, a 2:1 brine alkali addition flow regulating valve 8, a 2:1 brine alkali addition flow meter 9, a 2:1 brine stop valve 10, an in-tank brine stop valve 11, a refined brine header pipe 12, a 2:1 brine pipe 13, a 2:1 brine alkali addition pipe 14, an alkali head tank outlet pipe 15, a secondary refined brine, b refined brine acid, c soft water and d in-tank brine acid.
Detailed Description
The first embodiment is as follows: to describe the present invention in more detail, the following specific method is described with reference to the accompanying drawings: when the current is larger than 6.0KA in the process of reducing the current of the electrolytic cell (1), the acid adding flow regulating valve of the refined brine, the acid adding flow regulating valve of the in-cell brine and the 15 percent return brine flow regulating valve are adjusted in time according to process indexes, and the acid adding flow of the refined brine, the acid adding flow of the in-cell brine and the 15 percent return brine flow are reduced according to the process indexes. When the current of the electrolytic cell is reduced to 6.0KA, the refined brine acid adding flow regulating valve, the in-cell brine acid adding flow regulating valve and the 15% return brine flow regulating valve are closed. And (3) under the low-current operation of the electrolytic cell, waiting for the stop of the electrolytic cell after the indication of the PH monitoring meter (6) at the anode outlet is stable. After the electrolytic cell is shut down, a proper amount of liquid caustic soda is passed through a 2:1 saline water alkali adding flow regulating valve (7) and 2:1 adding saline water into a saline water alkali adding flow meter, and adding 2:1, in the brine, the anode outlet of the electrolytic cell is enabled to rapidly show alkalinity. When the anode outlet of each electrolytic cell shows alkalinity, the addition of the alkali to the 2:1 saline is stopped, and the 2:1 saline is continuously used for replacing the anode chamber until the hypochlorite ion content is lower.
Example two: a process control method for reducing damage of an electrolytic cell shutdown to a cathode chamber comprises an electrolytic cell (1), a brine head tank (2), an alkali head tank (3), a cathode circulating tank (4) and an anode circulating tank (5); an anode part: the secondary refined brine (a) enters a brine head tank and automatically flows into an anode chamber of an electrolytic cell (1) through a refined brine header pipe (12) under the action of head difference, the secondary refined brine is electrolyzed in the anode chamber under the action of direct current to generate chlorine and light brine, the light brine automatically flows into an anode circulating tank (5), 15% of the light brine is returned to a brine pipe through 15% of the water pipe to be introduced into the refined brine header pipe of the electrolytic cell to protect a titanium pipe; a cathode portion: the catholyte enters the alkali elevated tank (3) and is automatically fed to an outlet pipe (15) of the alkali elevated tank from a catholyte header pipe under the action of the elevation difference and then enters the cathode chamber; electrolyzing in a cathode chamber to generate hydrogen and 32% liquid caustic soda, wherein the 32% liquid caustic soda enters a cathode circulating tank (4); a 2:1 brine pipeline (13) is arranged on the refined brine main pipe (12); introducing soft water (a) into a 2:1 brine pipeline (13) through a soft water pipeline, arranging a 2:1 brine and alkali adding pipeline (14) on an outlet pipe (15) of the alkali elevated tank, connecting an inlet of the 2:1 brine and alkali adding pipeline (14) with the outlet pipe (15) of the alkali elevated tank, and connecting an outlet with the 2:1 brine pipeline (13); after the electrolytic cell is shut down, the electrolytic cell is switched to a 2:1 brine alkali adding pipeline (14) to supply the brine alkali solution to the electrolytic cell in a volume ratio of 2:1, adding a proper amount of liquid alkali into the saline water to ensure that the anode outlet of each electrolytic cell can quickly display alkalinity. A refined brine main pipe (12) is provided with a tank brine stop valve (11), a 2:1 brine stop valve (10) is arranged on a 2:1 brine pipeline (13), a 2:1 brine pure water flow regulating valve (7) is arranged on a soft water pipeline, a 2:1 brine alkali adding flow regulating valve (8) is arranged on a 2:1 brine alkali adding pipeline (14), and when the current of an electrolytic tank is reduced to 0KA, the tank brine stop valve (11) is closed, the 2:1 brine stop valve (10) is opened, and the 2:1 brine pure water flow regulating valve (7) and the 2:1 brine alkali adding flow regulating valve (8) are opened at the same time. An anode outlet pH monitoring meter (6) is arranged on an anode circulation tank outlet dilute brine pipeline and is in linkage control with a 2:1 brine alkali adding flow regulating valve (8). When the anode outlet pH monitoring meter (6) shows that the value is 10, the 2:1 saline alkali adding flow regulating valve (8) is closed; the addition of base to the 2:1 brine was stopped and the replacement of the anode compartment with 2:1 brine was continued until the hypochlorite ion content was low. The process adopts a DCS method for automatic control.
Claims (5)
1. A process control method for reducing damage of an electrolytic cell shutdown to a cathode chamber is characterized by comprising an electrolytic cell (1), a brine head tank (2), an alkali head tank (3), a cathode circulating tank (4) and an anode circulating tank (5); an anode part: the secondary refined brine (a) enters a brine head tank and automatically flows into an anode chamber of an electrolytic cell (1) through a refined brine header pipe (12) under the action of head difference, the secondary refined brine is electrolyzed in the anode chamber under the action of direct current to generate chlorine and light brine, the light brine automatically flows into an anode circulating tank (5), 15% of the light brine is returned to a brine pipe through 15% of the water pipe to be introduced into the refined brine header pipe of the electrolytic cell to protect a titanium pipe; a cathode portion: the catholyte enters the alkali elevated tank (3) and is automatically fed to an outlet pipe (15) of the alkali elevated tank from a catholyte header pipe under the action of the elevation difference and then enters the cathode chamber; electrolyzing in a cathode chamber to generate hydrogen and 32% liquid caustic soda, wherein the 32% liquid caustic soda enters a cathode circulating tank (4); a 2:1 brine pipeline (13) is arranged on the refined brine main pipe (12); introducing soft water (a) into a 2:1 brine pipeline (13) through a soft water pipeline, arranging a 2:1 brine and alkali adding pipeline (14) on an outlet pipe (15) of the alkali elevated tank, connecting an inlet of the 2:1 brine and alkali adding pipeline (14) with the outlet pipe (15) of the alkali elevated tank, and connecting an outlet with the 2:1 brine pipeline (13); after the electrolytic cell is shut down, the electrolytic cell is switched to a 2:1 brine alkali adding pipeline (14) to supply the brine alkali solution to the electrolytic cell in a volume ratio of 2:1, adding a proper amount of liquid alkali into the saline water to ensure that the anode outlet of each electrolytic cell can quickly display alkalinity.
2. A process control method for reducing damage of an electrolyzer shutdown to cathode chambers according to claim 1, characterized in that an in-tank brine shut-off valve (11) is provided on a refined brine header pipe (12), a 2:1 brine shut-off valve (10) is provided on a 2:1 brine pipeline (13), a 2:1 brine pure water flow regulating valve (7) is provided on a soft water pipeline, a 2:1 brine alkali addition flow regulating valve (8) is provided on a 2:1 brine alkali addition pipeline (14), and when the electrolyzer is shutdown, the in-tank brine shut-off valve (11) and the 2:1 brine shut-off valve (10) are closed, and the 2:1 brine pure water flow regulating valve (7) and the 2:1 brine alkali addition flow regulating valve (8) are opened.
3. A process control method to reduce damage to the cathode compartment from electrolyzer shutdowns as claimed in claim 2 characterized in that an anode outlet pH monitor (6) is placed on the 15% return brine line and is interlocked with a 2:1 brine make-up flow control valve (8).
4. A process control method to reduce cell shut down damage to the cathode compartment as claimed in claim 3 wherein the anode outlet pH monitor (6) indicates a value greater than 8 and the 2:1 brine plus base flow regulator valve (8) is closed; the addition of base to the 2:1 brine was stopped and the replacement of the anode compartment with 2:1 brine was continued until the hypochlorite ion content was low.
5. A process control method for reducing damage to the cathode compartment from cell shutdowns according to any one of claims 1 to 4, wherein the process is automatically controlled by DCS method.
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Application publication date: 20200911 |