阅读说明：本技术 一种适用于熔融盐电解质配料和转移的设备及其使用方法 (Equipment suitable for proportioning and transferring molten salt electrolyte and using method thereof ) 是由 赵纪峥 李梅 弋明涛 魏磊 王娟 酒坤 黄晓东 孙晓 高英武 王淑芳 徐朝莉 于 2019-09-24 设计创作，主要内容包括：本发明公开一种适用于熔融盐电解质配料和转移的设备及其使用方法,配料槽包括槽体(1)及配套的槽盖(2),槽盖上设计有加料口(3)、HF通料管(4)、电解质转移管(5)、温度计套管(6)、压力表(7),槽体的外部设计有加热装置(8)；HF通料管(4)和电解质转移管(5)延伸到槽体底部,电解质转移管(5)与槽盖之间设计有压力平衡阀(10),电解质转移管(5)出口端接有出料阀(9)；HF通料管入口管路通过三通分别连接HF进料阀(11)和增压阀(12)。该设备安全、高效,不开电解槽盖加料,不停车安全转移电解质入电解槽,同步精准计量转移量。(The invention discloses equipment suitable for batching and transferring molten salt electrolyte and a using method thereof, wherein a batching tank comprises a tank body (1) and a tank cover (2) matched with the tank body, a feed inlet (3), an HF (hydrogen fluoride) feed pipe (4), an electrolyte transferring pipe (5), a thermometer sleeve (6) and a pressure gauge (7) are designed on the tank cover, and a heating device (8) is designed outside the tank body; the HF material passing pipe (4) and the electrolyte transfer pipe (5) extend to the bottom of the tank body, a pressure balance valve (10) is designed between the electrolyte transfer pipe (5) and the tank cover, and the outlet end of the electrolyte transfer pipe (5) is connected with a discharge valve (9); an HF material inlet pipe is respectively connected with an HF feeding valve (11) and a pressure increasing valve (12) through a tee joint. The device is safe and efficient, the electrolytic tank cover is not opened for feeding, the electrolyte is safely transferred into the electrolytic tank without stopping, and the transfer amount is synchronously and accurately measured.)

1. A batching tank suitable for batching and transferring molten salt electrolyte comprises a tank body (1) and a tank cover (2) matched with the tank body, wherein a feed inlet (3), an HF (hydrogen fluoride) feed pipe (4), an electrolyte transferring pipe (5), a thermometer sleeve (6) and a pressure gauge (7) are designed on the tank cover, and a heating device (8) is designed outside the tank body; the HF material passing pipe (4) and the electrolyte transfer pipe (5) extend to the bottom of the tank body, a pressure balance valve (10) is designed between the electrolyte transfer pipe (5) and the tank cover, and the outlet end of the electrolyte transfer pipe (5) is connected with a discharge valve (9); an HF material inlet pipe is respectively connected with an HF feeding valve (11) and a pressure increasing valve (12) through a tee joint.

2. The dosing tank as claimed in claim 1, characterized in that there are more than one feed opening (3) in the tank cover and more than 2 HF feed lines (4).

3. the proportioning tank of claim 1 wherein lifting lugs are designed around the tank body.

4. The proportioning tank of claim 1 wherein the heating means is steam heating or electrical heating.

5. The proportioning tank of claim 1, wherein the tank body is made of one of monel steel, hastelloy or pure nickel, and the tank cover is made of one of monel steel, hastelloy, pure nickel or carbon steel.

6. The batch tank of claim 1 wherein the caliber of the electrolyte transfer tube is matched to the caliber of the level measuring port provided externally of the electrolytic tank.

7. A method of using a batch tank according to any one of claims 1 to 6, comprising the steps of:

(1) Adding the solid electrolyte into a dosing tank from a feeding port, and then sealing;

(2) Introducing HF according to the required molten salt ratio in a metering manner, and sealing;

(3) Heating to keep the electrolyte molten;

(4) Introducing nitrogen or compressed air through a pressurization valve, pressurizing the batching tank to the required pressure, and maintaining the pressure;

(5) inserting the outlet end of the electrolyte transfer pipe into a charging hand hole of the electrolytic cell or an external liquid level measuring pipe, opening a discharge valve to transfer materials, opening a pressure balance valve when the materials are transferred to the determined quantity, wherein the pressure of a gas phase area in the cell body is consistent with the pressure in the electrolyte transfer pipe, and the electrolyte transfer is stopped; nitrogen or compressed air in the gas phase area of the tank body sweeps electrolyte in a material transfer pipeline into the electrolytic tank on one hand through a pressure balance valve, and prevents the electrolyte in the batching tank from continuously flowing out to enable the electrolyte to flow back into the batching tank on the other hand; and closing the discharge valve to finish the electrolyte transfer.

8. The use according to claim 5, wherein the pressure is between 0.02MPa and 0.20 MPa.

Technical Field

The invention relates to a matched device of an electrolytic cell for preparing fluorine by an electrolytic method, in particular to a device for preparing and transferring molten salt electrolyte.

Background

In the industrial production of special gases containing fluorine such as nitrogen trifluoride, carbon tetrafluoride, sulfur hexafluoride, tungsten hexafluoride and the like, fluorine is prepared by an electrolytic method as a fluorine gas source, and ammonium fluoride, ammonium bifluoride, potassium fluoride or potassium bifluoride and the like are mixed with hydrogen fluoride in a certain proportion to prepare molten salt as an electrolyte. In the production and operation process, the electrolyte has certain loss and needs to be supplemented discontinuously.

The conventional electrolyte replenishing method comprises the following steps: stopping the operation of the electrolytic cell; nitrogen is fully blown to the cathode chamber and the anode chamber of the electrolytic cell to replace material gas; closing the electrolytic tank and all peripheral connecting valves; opening a hand hole matched with the electrolytic cell, and selecting solid electrolytes with different amounts for replenishment according to the liquid level of the electrolytic cell; HF is introduced into the electrolyte, different molar ratios of HF to ammonium fluoride or potassium fluoride are adjusted, and electrolytes of molten salts with different concentrations are prepared.

The supplementing method mainly has the following defects: 1) frequent stopping affects production; 2) the nitrogen-blowing replacement time is long, and the effective operation time of the electrolytic cell is shortened; 3) environmental pollution: the handhole cover is opened for operation, HF volatilizes into the surrounding environment, and pollution is caused; 4) the operation danger is large: if the nitrogen blowing replacement of the cathode chamber and the anode chamber of the electrolytic cell is not thorough, air is easily introduced when a handhole cover is opened for operation, so that explosion is caused and personnel are injured; 5) directly replenishing solid electrolyte, and introducing HF again to adjust the molten salt ratio before the operation of the electrolytic cell. As the HF feeding pipes are arranged at the two ends of the electrolytic cell, the mixing of the internal electrolyte and the ratio of fused salt (HF/NH) can be uneven in the process of feeding HF₃) The invention has the advantages of gradient difference and regulating effect

disclosure of Invention

The first technical problem to be solved by the invention is to provide equipment suitable for proportioning and transferring molten salt electrolyte, the equipment is safe and efficient, the electrolyte is safely transferred into an electrolytic cell without stopping and the transfer amount is synchronously and accurately measured without charging an electrolytic cell cover.

the second technical problem to be solved by the invention is to provide a using method of the equipment.

In order to solve the first technical problem, the invention provides a batching tank suitable for batching and transferring molten salt electrolyte, which comprises a tank body 1 and a matched tank cover 2, wherein the tank cover is provided with a feed inlet 3, an HF (hydrogen fluoride) material passing pipe 4, an electrolyte transferring pipe 5, a thermometer sleeve 6 and a pressure gauge 7, and the outside of the tank body is provided with a heating device 8; the HF material passing pipe 4 and the electrolyte transfer pipe 5 extend to the bottom of the tank body, a pressure balance valve 10 is designed between the electrolyte transfer pipe 5 and the tank cover, and the outlet end of the electrolyte transfer pipe 5 is connected with a discharge valve 9; the HF material inlet pipe is respectively connected with an HF feeding valve 11 and a pressure increasing valve 12 through a tee joint.

furthermore, the upper part of the tank cover is provided with more than 1 feeding port, and more than 2 HF material passing pipes are designed to improve the uniform speed of material distribution.

Furthermore, lifting lugs are arranged around the groove body and can be lifted by an electric hoist. The hanging scale and the batching groove are matched for use, and the electrolyte transferring amount can be measured.

The heating mode of the groove body can be steam heating or electric heating.

The groove body is made of one of monel alloy steel, hastelloy or pure nickel, and the groove cover is made of one of monel alloy steel, hastelloy, pure nickel or carbon steel.

To solve the second technical problem, the invention provides a batch tank suitable for the batching and transferring of molten salt electrolyte, and a using method of the batch tank, wherein the method comprises the following steps:

1) The solid electrolyte was charged into the batch tank from the charging port and then closed.

2) According to the required molten salt ratio, introducing HF according to the metering and sealing.

3) The heating keeps the electrolyte molten.

4) Nitrogen or compressed air is introduced through a pressure increasing valve, and the batching tank is pressurized to the required pressure for pressure maintaining. The pressure is preferably 0.02MPa to 0.20 MPa.

5) Inserting the outlet end of the electrolyte transfer pipe into a charging hand hole of the electrolytic cell or a peripheral liquid level measuring pipe, opening a discharge valve 9 to transfer materials, opening a pressure balance valve 10 when the materials are transferred to a given quantity, wherein the pressure of a gas phase area in the cell body is consistent with the pressure in the electrolyte transfer pipe, and the electrolyte transfer is stopped; nitrogen or compressed air in the gas phase area of the tank body blows electrolyte in the material transfer pipeline through one side of the pressure balance valve 10 to the electrolytic tank, and on the other hand, the electrolyte in the batching tank is prevented from continuously flowing out, so that the electrolyte flows back into the batching tank; the discharge valve 9 is closed and the electrolyte transfer is finished.

The caliber of the electrolyte transfer pipe can be matched and formulated according to the caliber of a liquid level measuring port arranged outside the electrolytic cell, and the electrolyte transfer pipe is directly inserted into the liquid level measuring port to transfer materials. The electrolytic cell receiving the electrolyte can be kept in normal operation without stopping the cell.

The invention has the advantages that:

1) Solid electrolyte is added through a feed inlet of the batching tank, so that the working strength of the operation of opening the cover of the electrolytic tank every time is reduced.

2) Utilize HF to lead to the material pipe and let in nitrogen gas or compressed air as the booster pipe, impress HF in the pipe into the batching groove, avoided HF to lead to the risk that the material pipe blockked up, provided the guarantee for batching next time.

3) At the interval design balanced pressure's of discharging pipe and batching groove gaseous phase pipeline, when opening balanced valve 10, during nitrogen gas or the compressed air entering discharging pipe 5 of batching groove gaseous phase district, to impressing the batching groove to the electrolyte downwards, outwards to impressing the electrolyte and receiving the electrolysis trough, guaranteed that discharging pipeline 5 does not persist the electrolyte to bleeder valve 9 epitaxial position above the batching groove liquid level. The discharge valve 9 is closed, and a certain pressure can be kept in the batching tank; opening bleeder valve 9, the internal pressure of batching groove can be discharged to receiving the electrolysis trough through ejection of compact pipeline pressure release to discharge through the cathode system of receiving the groove, reduced the acid gas and discharged, avoided environmental pollution.

4) Before transferring the electrolyte, keep certain malleation in the batching groove, need not the pressure boost once more when the batching groove is given different electrolysis trough feed supplements in succession, can the direct operation.

5) And in the electrolyte transfer process, the gas is not required to be discharged to the outside, so that the pollution of acid gas to the environment is avoided.

Drawings

FIG. 1 is a schematic view of the construction of the feed chute of the present invention.

Wherein: 1. the electrolytic bath comprises a bath body, 2 parts of a bath cover, 3 parts of a charging port, 4 parts of an HF material feeding pipe, 5 parts of an electrolyte transfer pipe, 6 parts of a thermometer sleeve, 7 parts of a pressure gauge, 8 parts of a heating device, 9 parts of an electrolyte discharging valve, 10 parts of a pressure balancing valve, 11 parts of an HF feeding valve and 12 parts of a pressure increasing valve

Detailed Description

The invention is further described below with reference to the figures and examples.

As shown in fig. 1, a batching tank suitable for batching and transferring molten salt electrolyte comprises a tank body 1 and a tank cover 2 matched with the tank body, wherein a feed inlet 3, an HF (hydrogen fluoride) feed pipe 4, an electrolyte transfer pipe 5, a thermometer sleeve 6 and a pressure gauge 7 are designed on the tank cover, and a heating device 8 is designed outside the tank body; the HF material passing pipe 4 and the electrolyte transfer pipe 5 extend to the bottom of the tank body, a pressure balance valve 10 is designed between the electrolyte transfer pipe 5 and the tank cover, and the outlet end of the electrolyte transfer pipe 5 is connected with a discharge valve 9; the HF material inlet pipe is respectively connected with an HF feeding valve 11 and a pressure increasing valve 12 through a tee joint. The upper part of the tank cover is provided with 2 HF material passing pipes. Lifting lugs are arranged around the groove body.

The groove body is made of one of monel alloy steel, hastelloy or pure nickel, and the groove cover is made of one of monel alloy steel, hastelloy, pure nickel or carbon steel.