Device for measuring acidity of electrolyte of fluorine-making electrolytic cell

By setting an electrolytic protective sleeve and an acidity measurement electrode in the electrolytic fluorine-making device, the electrolytic resistance value is automatically converted to the acidity signal, which solves the problem of inaccurate measurement of electrolytic acidity, and achieves safe and environmentally friendly electrolytic acidity measurement and electrolytic cell efficiency improvement.

CN223139504UActive Publication Date: 2025-07-22PERIC SPECIAL GASES CO LTD
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Patent Information

Application Number
CN202421446331.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-06-24
Publication Date
2025-07-22
Estimated Expiration
2034-06-24

AI Technical Summary

Technical Problem

In the prior art, real-time measurement of the acidity of the electrolyte is not possible during the electrolytic fluorine production process, resulting in inaccurate HF replenishment, which may damage the carbon plate anode. HF dissipation is harmful to workers' health and affects the efficiency of the electrolytic cell.

Method used

A device for measuring the acidity of the electrolyte of the fluorine electrolyte is designed, including an electrolytic protective sleeve, a potential protection sleeve, an acidity measurement electrode and a signal converter. By measuring the electrolyte resistance value, it is automatically converted into an acidity signal, and automatic control is achieved.

Benefits of technology

It realizes safe, environmentally friendly, and sustainable and reliable electrolyte acidity measurement, avoids HF dissipation and carbon plate damage, and improves the operating efficiency of the electrolyte cell and the safety of workers.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the technical field of electrolytic fluorine production, in particular to a device for measuring the acidity of electrolyte in a fluorine-making electrolytic bath, which comprises the fluorine-making electrolytic bath, an electrolytic protective sleeve, a potential protective sleeve, two acidity measuring electrodes, a signal converter and a fastener, the fluorine-making electrolytic cell is installed at the electrolytic material adding port, the upper ends of the electrolytic protective sleeve, the potential protective sleeve and the two acidity measuring electrodes are fixed above the fluorine-making electrolytic cell through fasteners, the fluorine-making electrolytic cell is filled with electrolyte, and the lower ends of the acidity measuring electrodes and the potential protective sleeve are immersed below the electrolyte level. The potential protection sleeves are arranged on the inner sides of the acidity measuring electrodes, the upper ends of the acidity measuring electrodes are protected by the electrolysis protection sleeves, the signal converter is connected between the two acidity measuring electrodes through the electrode connecting wire, and the signal converter is positioned above the fluorine-making electrolytic bath. The device is safe, environment-friendly, continuous and reliable in measurement of the acidity of the electrolyte in the fluorine-making electrolytic cell.
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Description

Technical Field

[0001] The utility model relates to the technical field of electrolytic fluorine production, in particular to a device for measuring the acidity of electrolyte in a fluorine production electrolytic cell. Background Technique

[0002] As the most important raw material for fluorine chemical industry, with the development of fluorine chemical technology, electrolytic fluorine production technology has been paid more and more attention by fluorine chemical enterprises. However, when measuring the acidity of electrolyte in electrolytic fluorine production, manual sampling is still carried out using a copper rod under the condition of opening the fluorine production electrolytic cell, and then titration is carried out, which has many disadvantages: ① It cannot be measured in real time. When supplementing HF, it can only be supplemented according to the theoretically calculated consumption, and it cannot be displayed in real time. If too much HF is supplemented, it will cause irreversible damage to the carbon plate anode and even cause carbon plate pulverization; ② HF will escape, which causes great harm to the workers sampling the electrolyte and also increases the labor intensity; ③ It is not conducive to continuous HF supplementation without real-time monitoring; ④ The electrolytic cell needs to be shut down and purged with nitrogen, which affects the efficiency of the fluorine production electrolytic cell. Content of the Utility Model

[0003] The purpose of the utility model is to provide a safe, environmentally friendly, continuous and reliable device for measuring the acidity of electrolyte in a fluorine production electrolytic cell.

[0004] To achieve the above purpose, the utility model provides the following technical solutions:

[0005] A device for measuring the acidity of electrolyte in a fluorine production electrolytic cell, comprising a fluorine production electrolytic cell, an electrolytic protection sleeve, a potential protection sleeve, two acidity measurement electrodes, a signal converter and a fastener;

[0006] The fluorine production electrolytic cell is installed at the electrolytic material adding port. The upper ends of the electrolytic protection sleeve, the potential protection sleeve and the two acidity measurement electrodes are fixed above the fluorine production electrolytic cell through fasteners. The fluorine production electrolytic cell is filled with electrolyte. The lower ends of the acidity measurement electrodes and the potential protection sleeve are both immersed below the electrolytic liquid level. The potential protection sleeve is arranged inside the acidity measurement electrodes. The upper ends of the acidity measurement electrodes are protected by the electrolytic protection sleeve. The two acidity measurement electrodes are connected to the signal converter through electrode connection wires. The signal converter is located above the fluorine production electrolytic cell.

[0007] Preferably, a fluorine production electrolytic cell cover is arranged on the fluorine production electrolytic cell.

[0008] Preferably, the signal converter is in signal communication with DCS or PLC. The electrode connection wires are made of polytetrafluoro material. The material of the acidity measurement electrodes is pure copper or Monel.

[0009] Preferably, the signal converter is used to convert the electrolyte resistance value signal into 4 - 20mA or 485 communication.

[0010] Preferably, the fastener includes a feeding flange for the fluorine production electrolytic cell, and the electrolytic protection sleeve, the potential protection sleeve and the two acidity measuring electrodes are fastened at the position of the feeding flange of the fluorine production electrolytic cell by bolts.

[0011] Preferably, the potential protection sleeve has openings above the liquid level.

[0012] A method for measuring the acidity of the electrolyte in a fluorine production electrolytic cell includes the following steps: checking whether the seal of the fluorine production electrolytic cell cover is intact, applying a 1V voltage to the acidity measuring electrode by a signal converter, sampling and titrating the acidity of the electrolyte to adjust the output signal of the signal converter, running the fluorine production electrolytic cell at 2000A for 24 hours without supplementing HF, then sampling and titrating the acidity and comparing it with the displayed acidity, and if there is a difference, continue to calibrate; supplementing the electrolyte in the fluorine production electrolytic cell to a HF mass fraction of 42% and continuing to calibrate the acidity of the signal converter, and then stably operating the fluorine production electrolytic cell.

[0013] Preferably, the electrolyte is in a molten state, the mass fraction of HF in the electrolyte is 38%-42%, and the balance is potassium fluoride.

[0014] Preferably, the fluorine production electrolytic cell is calibrated once every 3-6 months.

[0015] The main equipment for measuring the acidity of the fluorine production electrolytic cell is installed at the electrolytic feed inlet, which is convenient for equipment maintenance and does not change the structure of the existing fluorine production electrolytic cell.

[0016] Use the electrode to measure the resistance value of the electrolyte and then convert it into the HF mass fraction through equipment calculation, convert it into 4-20mA or 485 communication through the signal converter, and transmit it to the DCS or PLC for display.

[0017] The potential protection sleeve is to shield the influence of the potential generated during the operation of the fluorine production electrolytic cell on the measurement;

[0018] The signal converter is mainly to convert the measured electrolyte resistance value signal into other signals for convenient transmission and calculation;

[0019] The electrolytic protection sleeve uses polytetrafluoro material to isolate the connection part from the electrolyte, avoiding inaccurate measurement caused by the change of the liquid level.

[0020] The utility model is directly installed at the feeding port of the fluorine production electrolytic cell. This port is only used when the fluorine production electrolytic cell is refilled for the first time and when the material is pressed after the operation stops. It does not cause conflicts in time for the structure measurement of the fluorine production electrolytic cell and does not damage the structure of the fluorine production electrolytic cell.

[0021] The prior art is mainly a method of measuring the liquid level of the electrolyte and then converting it into the acidity of the electrolyte through calculation. Compared with the prior art, the beneficial effects of the utility model are:

[0022] 1. In the present utility model, a potential protection sleeve is provided in a device for measuring the acidity of the electrolyte in a fluorine - producing electrolytic cell to isolate the influence of the potential during the operation of the fluorine - producing electrolytic cell on the measurement result. Moreover, openings are provided above the liquid level of the potential protection sleeve for the pressure balance inside and outside the sleeve.

[0023] 2. In the present utility model, an acidity measurement electrode is provided in a device for measuring the acidity of the electrolyte in a fluorine - producing electrolytic cell. The acidity measurement electrode is made of pure copper or Monel material and is used to measure the resistance value between the electrodes of the electrolyte in the fluorine - producing electrolytic cell. The signal converter converts the electrolyte resistance value into the acidity of the electrolyte and then transmits it to the DCS or PLC through an electrical signal.

[0024] 3. In the present utility model, a signal converter is provided in a device for measuring the acidity of the electrolyte in a fluorine - producing electrolytic cell. It is used to convert the measured resistance value data into electrolyte acidity data and convert it into an electrical signal for transmission to the PLC or DCS for further automatic control. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the overall structure of the present utility model;

[0026] In the figure, 1. Fluorine - producing electrolytic cell; 2. Fluorine - producing electrolytic cell cover; 3. Electrode protection sleeve; 4. Signal converter; 5. Fastener; 6. Potential protection sleeve; 7. Acidity measurement electrode. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0027] The following further describes the present utility model in detail with reference to the Figure 1 accompanying drawings and embodiments.

[0028] First, as Figure 1 shown, a device for measuring the acidity of the electrolyte in a fluorine - producing electrolytic cell includes a fluorine - producing electrolytic cell 1, a fluorine - producing electrolytic cell cover 2, an electrode protection sleeve 3, a signal converter 4, a fastener 5, a potential protection sleeve 6, and an acidity measurement electrode 7. Among them, the electrode protection sleeve 3 is for protecting the measurement electrode, the acidity measurement electrode 7 is for measuring the electrolyte resistance value, and the signal converter 4 is used to convert the electrolyte resistance value measured by the acidity measurement electrode 7 into an HF mass fraction signal and then into an electrical signal.

[0029] A device for measuring the acidity of the electrolyte in a fluorine - producing electrolytic cell includes a fluorine - producing electrolytic cell 1, an electrolytic protection sleeve 3, a potential protection sleeve 6, two acidity measurement electrodes 7, a signal converter 4, and a fastener 5;

[0030] The fluorine production electrolytic cell 1 is installed at the electrolytic material adding port. A fluorine production electrolytic cell cover 2 is provided on the fluorine production electrolytic cell 1. The upper ends of the electrolytic protection sleeve 3, the potential protection sleeve 6 and the two acidity measurement electrodes 7 are fixed above the fluorine production electrolytic cell 1 through a fastener 5. The fastener 5 includes a fluorine production electrolytic cell feeding flange. The electrolytic protection sleeve 3, the potential protection sleeve 6 and the two acidity measurement electrodes 7 are fastened at the position of the fluorine production electrolytic cell feeding flange using bolts. The fluorine production electrolytic cell 1 is filled with electrolyte. The lower ends of the acidity measurement electrodes 7 and the potential protection sleeve 6 are both immersed below the electrolytic liquid level. The potential protection sleeve 6 is arranged inside the acidity measurement electrodes 7. The potential protection sleeve 6 has openings above the liquid level. The upper ends of the acidity measurement electrodes 7 are protected by the electrolytic protection sleeve 3. The two acidity measurement electrodes 7 are connected to a signal converter 4 through an electrode connecting wire. The signal converter 4 is in signal communication with a DCS or a PLC. The signal converter 4 is used to convert the electrolyte resistance value signal into 4 - 20 mA or 485 communication. The electrode connecting wire is made of polytetrafluoro material. The signal converter 4 is located above the fluorine production electrolytic cell 1. The material of the acidity measurement electrodes 7 is pure copper or Monel.

[0031] A method for measuring the acidity of the electrolyte in a fluorine production electrolytic cell includes the following steps: Check whether the seal of the fluorine production electrolytic cell cover is intact. The signal converter applies a 1V voltage to the acidity measurement electrode. Take about 1g of the electrolyte and titrate the HF mass fraction using a 0.5mor / L sodium hydroxide solution. Titrate in parallel 3 times, and take the average value of the HF mass fraction as 41.3%. Calibrate the acidity of the electrolyte to adjust the output signal of the signal converter to 41.3%. Without replenishing HF, the fluorine production electrolytic cell operates at 2000A for 24 hours, and then perform acid-base titration on 3 parallel samples using the above method. Take the average value of the HF mass fraction as 40.5%, and compare it with the displayed acidity. If there is a difference, continue to calibrate; replenish the electrolyte in the fluorine production electrolytic cell to an HF mass fraction of 42% and continue to calibrate the acidity of the signal converter, and then stably operate the fluorine production electrolytic cell.

[0032] After the fluorine production electrolytic cell operates for 3 months, take 3 parallel samples of the electrolyte again for acid-base titration. The average value of the titration result of the HF mass fraction is 40.4%, and the acidity value displayed by the signal converter is 40.3%. After the fluorine production electrolytic cell stably operates for 4 months, take 3 parallel samples of the electrolyte again for acid-base titration. The average value of the titration result of the HF mass fraction is 39.6%, and the acidity value displayed by the signal converter is 39.7%. After the fluorine production electrolytic cell operates for 3 months, take 3 parallel samples of the electrolyte again for acid-base titration. The average value of the titration result of the HF mass fraction is 41.2%, and the acidity value displayed by the signal converter is 40.6%, with an error of 0.6%. Calibrate the converter again, and then calibrate the signal converter every 3 - 6 months.

[0033] Next, in combination with the embodiments of the present utility model, the technical solutions in the embodiments of the present utility model will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all the embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present utility model.

[0034] Although the embodiments of the present utility model have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present utility model. The scope of the present utility model is defined by the appended claims and their equivalents.

Claims

1. An apparatus for measuring the acidity of the electrolyte in a fluorine electrolytic cell, characterized in that, It includes a fluorine production electrolytic cell (1), an electrolysis protective sleeve (3), a potential protective sleeve (6), two acidity measurement electrodes (7), a signal converter (4), and fasteners (5); The fluorine production electrolytic cell (1) is installed at the electrolytic material addition port. The upper ends of the electrolysis protective sleeve (3), the potential protective sleeve (6), and the two acidity measurement electrodes (7) are fixed above the fluorine production electrolytic cell (1) through fasteners (5). The fluorine production electrolytic cell (1) is filled with electrolyte. The lower ends of the acidity measurement electrodes (7) and the potential protective sleeve (6) are both immersed below the electrolytic liquid level. The potential protective sleeve (6) is arranged inside the acidity measurement electrodes (7). The upper ends of the acidity measurement electrodes (7) are protected by the electrolysis protective sleeve (3). The two acidity measurement electrodes (7) are connected to the signal converter (4) through electrode connection wires. The signal converter (4) is located above the fluorine production electrolytic cell (1).

2. The device for measuring the acidity of the electrolyte in a fluorine electrolysis cell according to claim 1, characterized in that, A fluorine production electrolytic cell cover (2) is provided on the fluorine production electrolytic cell (1).

3. The device for measuring the acidity of the electrolyte in a fluorine electrolysis cell according to claim 1, wherein, The signal converter (4) is in signal communication with DCS or PLC. The electrode connection wires are made of polytetrafluoro material. The material of the acidity measurement electrodes (7) is pure copper or Monel.

4. The device for measuring the acidity of the electrolyte in a fluorine electrolysis cell according to claim 1, characterized in that, The signal converter (4) is used to convert the electrolyte resistance value signal into 4 - 20 mA or 485 communication.

5. The device for measuring the acidity of the electrolyte in a fluorine production electrolytic cell according to claim 1, wherein The fasteners (5) include a fluorine production electrolytic cell feeding flange. The electrolysis protective sleeve (3), the potential protective sleeve (6), and the two acidity measurement electrodes (7) are fastened at the position of the fluorine production electrolytic cell feeding flange using bolts.

6. The device for measuring the acidity of the electrolyte in a fluorine electrolysis cell according to claim 1, characterized in that, The potential protective sleeve (6) has openings above the liquid level.