CN214612782U - Charging system of nitrogen trifluoride electrolytic cell - Google Patents

Charging system of nitrogen trifluoride electrolytic cell Download PDF

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Publication number
CN214612782U
CN214612782U CN202023127779.3U CN202023127779U CN214612782U CN 214612782 U CN214612782 U CN 214612782U CN 202023127779 U CN202023127779 U CN 202023127779U CN 214612782 U CN214612782 U CN 214612782U
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ammonia
flow
electrolytic cell
main pipeline
valve
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纪振红
马朝选
王振宇
郑阳光
赵志刚
乔蓓蓓
王军岭
宋忠华
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Peric Special Gases Co Ltd
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Peric Special Gases Co Ltd
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Abstract

The utility model discloses a feeding system of a nitrogen trifluoride electrolytic cell, which is sequentially connected with a liquid ammonia storage tank, an ammonia vaporizer, an ammonia buffer tank, a molecular sieve tower, a first filter and a check valve along the flow direction of ammonia, and finally connected with an ammonia main pipeline; the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are sequentially connected along the flow direction of HF, and finally the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are connected to an HF main pipeline; a liquid level meter and a density meter are arranged in the electrolytic tank; the connecting pipeline of the electrolytic cell, the ammonia gas main pipeline and the HF main pipeline is connected with an electrolytic cell flowmeter and an electrolytic cell inlet flow valve for controlling the proportion of ammonia gas/HF in the electrolytic cell; the electrolytic cell is communicated with a flow valve and the liquid level meter to form a liquid level interlocking control loop, and the electrolytic cell and the densimeter form a component proportion control loop; the controller is connected with each sensor and the valve. The utility model can improve the safety of the feed supplement operation, improve the gas production collection rate of the electrolytic cell and reduce the cost of equipment and personnel.

Description

Charging system of nitrogen trifluoride electrolytic cell
Technical Field
The utility model relates to a nitrogen trifluoride preparation technical field especially relates to a nitrogen trifluoride electrolysis trough's charging system.
Background
Nitrogen trifluoride is a colorless, odorless and stable gas at normal temperature, is a strong oxidant, is used as an excellent plasma etching gas in the microelectronic industry, is cracked into active fluorine ions during ion etching, has excellent etching rate and selectivity (for silicon oxide and silicon) for silicon and tungsten compounds, is a very good cleaning agent for high-purity nitrogen trifluoride, does not leave any residue on the surface of an etching object during etching, and is widely applied to chip manufacturing and high-energy lasers. With the development of nanotechnology and the large-scale development of technology in the electronics industry, the demand for it will increase.
Although nitrogen trifluoride is a low toxic substance, it can strongly irritate the eye, skin and respiratory mucosa, eroding tissues. High suctionNF3 concentration can cause headache, vomiting, and diarrhea. Long term inhalation of low concentration NF3Can damage teeth and bones, and make teeth yellow spots and bones deformed. Has strong oxidizing property. Can react with the reducing agent strongly to cause combustion explosion.
In the preparation of nitrogen trifluoride, the electrolysis bath needs to be charged for convenient preparation. If adopt artifical reinforced mode, the cost of labor is high, can not guarantee personnel's safety, and influences machining efficiency. For the automatic feeding scheme, the existing scheme firstly adopts a tank body to mix ammonia and Hydrogen Fluoride (HF) to form a mixed solution, and then the mixed solution is added into an electrolytic tank through a pipeline. The transmission of liquid has high requirements on pipelines and high cost. And the scheme of mixing firstly is the same for the proportion of the materials introduced into different electrolytic tanks, and the materials cannot be configured according to the direct electrolysis effect, so that the gas production collection rate can be reduced, and the processing efficiency can be influenced.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model provides a feed system of nitrogen trifluoride electrolysis trough can improve the security of feed supplement operation, improves the electrolysis trough and produces gas the collection rate, reduces equipment and personnel cost.
In order to solve the technical problem, the utility model discloses a so realize.
A feed system for a nitrogen trifluoride electrolyzer, comprising:
a liquid ammonia storage tank, an ammonia vaporizer, an ammonia buffer tank, a molecular sieve tower, a first filter and a check valve are sequentially connected along the flow direction of ammonia, and finally, the liquid ammonia is connected to an ammonia main pipeline; the ammonia buffer tank is provided with a first pressure gauge, and a first pressure interlocking valve for controlling the air inlet flow rate of the ammonia buffer tank is connected to a pipeline between the liquid ammonia storage tank and the ammonia vaporizer; the first pressure interlocking valve and the first pressure gauge are both connected with a controller to form an ammonia buffer tank pressure interlocking control loop; an ammonia flow valve for controlling the ammonia flow in the ammonia main pipeline and an ammonia flow meter for detecting the ammonia flow in the ammonia main pipeline are arranged on a pipeline between the check valve and the ammonia main pipeline; the ammonia flow valve and the ammonia flow meter are both connected with a controller to form an ammonia total flow interlocking control loop;
the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are sequentially connected along the flow direction of the hydrogen fluoride HF, and finally the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are connected to an HF main pipeline; the HF buffer tank is provided with a second pressure gauge, and a second pressure interlocking valve for controlling the air inlet flow rate of the HF buffer tank is connected to a pipeline between the HF storage tank and the HF vaporizer; the second pressure interlocking valve and the second pressure gauge are both connected with the controller to form an HF buffer tank pressure interlocking control loop; an HF flow valve for controlling HF flow in the HF main pipeline and an HF flow meter for detecting the HF flow in the HF main pipeline are arranged on a pipeline between the second filter and the HF main pipeline; the HF flow valve and the HF flowmeter are both connected with the controller to form an HF total flow linkage control loop;
a plurality of electrolytic tanks are connected in parallel and are respectively connected into the ammonia gas main pipeline and the HF main pipeline; a liquid level meter and a density meter are arranged in the electrolytic tank; the connecting pipeline of the electrolytic cell and the ammonia main pipeline and the connecting pipeline of the electrolytic cell and the HF main pipeline are both connected with an electrolytic cell flowmeter and an electrolytic cell lead-in flow valve for controlling the proportion of ammonia gas/HF entering the electrolytic cell; the electrolytic bath inlet flow valve and the liquid level meter are both connected with a controller to form a liquid level interlocking control loop; the densimeter is also connected with the controller and forms a component proportion control loop with the flow valve introduced into the electrolytic cell;
the liquid ammonia storage tank with the output pipeline of HF storage tank all links there is the delivery pump, and the delivery pump is connected the controller.
Preferably, the molecular sieve column comprises a 2-stage molecular sieve column.
Preferably, the molecular sieve tower comprises a main molecular sieve tower and a standby molecular sieve tower which are connected in parallel.
Preferably, the first filter and the second filter each comprise two stages of filters in series, namely a coarse filter and a fine filter.
Preferably, a valve which is used for shutting off when the device is repaired or replaced is arranged between every two devices in the system.
Preferably, the electrolytic cell comprises a temperature sensor and a heating device which are connected with a controller to work, and the temperature of the electrolytic cell is controlled to be 80-130 ℃.
Preferably, the cell pressure is atmospheric.
Has the advantages that:
(1) the utility model discloses vaporize liquid ammonia and liquid HF into ammonia and HF gas, transmit respectively to each electrolysis trough through the pipeline. The gas transmission has relatively lower pipeline requirements than liquid and higher safety, thereby reducing the equipment cost and the requirements on personnel. Meanwhile, the two substances are respectively transmitted to the electrolytic tanks through pipelines, so that the flow of the two substances can be respectively controlled, the proportion can be adjusted according to the density of the electrolyte, and the gas production collection rate is improved.
(2) The electrolysis trough is under the condition of producing nitrogen trifluoride in succession, the utility model discloses utilize the delivery pump to pass through the pipeline with hydrogen fluoride and ammonia and add the electrolysis trough in, realize continuous feed supplement and the proportion adjustment to the electrolysis trough.
(3) The electrolytic cell utilizes the pipeline to continuously feed, can improve the safety of feeding operation, improve the yield of the produced gas of the electrolytic cell, reduce the personnel cost, can prepare NF3 gas safely on a large scale, and has strong practicability.
Drawings
FIG. 1 is a schematic diagram showing the composition of a feed system of a nitrogen trifluoride electrolyzer.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings by way of examples.
Referring to fig. 1, the utility model provides a nitrogen trifluoride electrolysis cell's feeding scheme, this scheme gasifies liquid ammonia and liquid HF into ammonia and HF gas, transmits respectively to each electrolysis cell through the pipeline. The gas transmission has relatively lower pipeline requirements than liquid and higher safety, thereby reducing the equipment cost and the requirements on personnel. Meanwhile, the two substances are respectively transmitted to the electrolytic tanks through pipelines, so that the flow of the two substances can be respectively controlled, the proportion can be adjusted according to the density of the electrolyte, and the gas production collection rate is improved.
FIG. 1 shows a feeding system of a nitrogen trifluoride electrolyzer, as shown in FIG. 1:
for the ammonia feed line: connect gradually liquid ammonia storage tank, ammonia vaporizer, ammonia buffer tank, molecular sieve tower, first filter, check valve along the flow direction of ammonia, insert the ammonia main line at last.
The output pipeline of the liquid ammonia storage tank is connected with a delivery pump for controlling the outlet flow of the liquid ammonia and ensuring the continuous feeding of the electrolytic tank. The delivery pump is connected with the controller.
The ammonia buffer tank is provided with a first pressure gauge, and a first pressure interlocking valve for controlling the air inlet flow rate of the ammonia buffer tank is connected to a pipeline between the liquid ammonia storage tank and the ammonia vaporizer; the first pressure interlocking valve and the first pressure gauge are both connected with the controller to form an ammonia buffer tank pressure interlocking control loop. A pressure value, for example, 0.3MP, may be preset, and the controller may control the flow rate of the ammonia buffer tank inlet air by adjusting the opening degree of the first pressure interlock valve according to the collected value of the first pressure gauge, so as to keep the pressure of the ammonia buffer tank at about 0.3 MP. By using the better pressure, the continuous feeding of the electrolytic cell is ensured.
The molecular sieve tower is used for filtering heavy oil in liquid ammonia, and comprises a 2-stage molecular sieve tower in a preferred embodiment; meanwhile, two sets of main and standby molecular sieve towers which are connected in parallel can be arranged, and the two sets of molecular sieve towers are switched by a valve. When the molecular sieve tower of the main part needs to be overhauled or maintained, the molecular sieve tower is switched to the backup molecular sieve tower, and vice versa.
The first filter is used for filtering particulate impurities and residual oil. In the preferred embodiment, the first filter comprises two stages of filters connected in series, and is divided into a coarse filter and a fine filter, wherein the coarse filter is performed first, and the fine filter is performed first.
And an ammonia flow valve for controlling the ammonia flow in the ammonia main pipeline and an ammonia flow meter for detecting the ammonia flow in the ammonia main pipeline are arranged on a pipeline between the check valve and the ammonia main pipeline. The ammonia flow valve and the ammonia flow meter are both connected with the controller to form an ammonia total flow interlocking control loop. The controller can adjust the opening of the ammonia flow valve according to the acquisition value of the ammonia flowmeter so as to control the ammonia gas supply flow.
For the feed line for HF: the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are sequentially connected along the flow direction of the hydrogen fluoride HF, and finally the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are connected to an HF main pipeline.
The output pipeline of the HF storage tank is connected with a delivery pump for controlling the outlet flow of HF and ensuring the continuous feeding of the electrolytic bath. The delivery pump is connected with the controller.
The HF buffer tank is provided with a second pressure gauge, and a second pressure interlocking valve for controlling the air inlet flow rate of the HF buffer tank is connected to a pipeline between the HF storage tank and the HF vaporizer; the second pressure interlocking valve and the second pressure gauge are both connected with the controller to form an HF buffer tank pressure interlocking control loop. A pressure value can be preset, and the controller can control the air inlet flow rate of the HF buffer tank by adjusting the opening degree of the second pressure linkage valve according to the acquisition value of the second pressure gauge, so that the pressure of the HF buffer tank is kept at about a set value.
In the preferred embodiment, the second filter comprises two stages of filters connected in series, and is divided into a coarse filter and a fine filter, wherein the coarse filter is performed first, and the fine filter is performed later.
An HF flow valve for controlling HF flow in the HF main pipeline and an HF flow meter for detecting the HF flow in the HF main pipeline are arranged on a pipeline between the second filter and the HF main pipeline; the HF flow valve and the HF flowmeter are both connected with the controller to form an HF total flow interlocking control loop. The controller can adjust the opening of the HF flow valve according to the acquisition value of the HF flowmeter so as to control the HF gas supply flow.
The system comprises a plurality of electrolytic cells which are connected in parallel and are respectively connected into an ammonia main pipeline and an HF main pipeline. A liquid level meter and a density meter are arranged in each electrolytic cell. The connecting pipeline of the electrolytic cell and the ammonia main pipeline and the connecting pipeline of the HF main pipeline are both connected with an electrolytic cell flowmeter and an electrolytic cell lead-in flow valve. The cell inlet flow valve is used to control the flow of ammonia/HF into the cell and thus the ammonia/HF ratio into the cell.
The electrolytic cell is connected with the controller through the flow valve and the liquid level meter to form a liquid level interlocking control loop. And the controller controls the flow valve to be introduced into the electrolytic cell according to the acquired value of the liquid level meter to realize liquid supplement of the electrolytic cell, automatically closes the flow valve to be introduced into the electrolytic cell when the liquid level is supplemented to a required value, and automatically opens and supplements electrolyte when the liquid level is lower than the required value.
The electrolytic cell inlet flow valve and the densimeter are both connected with the controller to form a component proportion control loop. The controller obtains the ratio of HF to ammonia in the electrolyte according to the acquisition value of the densimeter, compares the ratio with the required ratio to determine the introduction amount of ammonia and HF, and realizes the ratio adjustment of the ammonia and the HF by controlling the opening of the inlet flow valve of the electrolytic cell.
The electrolytic bath can also be provided with a temperature sensor and a heating device which are connected with the controller to work, and the temperature of the electrolytic bath is controlled to be 80-130 ℃. The pressure of the electrolytic cell is normal pressure. The liquid level height of the electrolytic cell can be controlled to be 550 mm.
Valves which are used for shutting off when the devices are maintained and replaced can be arranged between every two devices in the system. The valves can be manually controlled or can be automatically controlled by connecting with a controller. When a certain device needs to be maintained, the valves at the two ends of the device are closed, and after the device is maintained or replaced, the valves at the two ends of the device are opened.
The controller can also be connected with a display to output the acquisition values of the ammonia gas flowmeter, the HF flowmeter, the ammonia gas pipeline and the electrolytic bath flowmeter and the liquid level meter of the HF pipeline to the display for displaying.
The utility model discloses nitrogen trifluoride electrolysis trough charging system working process does:
respectively starting the delivery pumps of the HF storage tank and the liquid ammonia storage tank, and controlling the outlet flow of the delivery pumps; after being converted into ammonia gas by an ammonia vaporizer, the ammonia gas passes through an ammonia gas buffer tank, a molecular sieve tower, a first filter and a check valve and then enters an ammonia gas main pipeline under the flow control of an ammonia gas flow valve; HF is converted into HF gas by an HF vaporizer, and then enters an HF main pipeline under the flow control of an HF flow valve after passing through an HF buffer tank and a second filter; the controller controls the air inlet flow rates of the hydrogen fluoride and the ammonia gas entering the buffer tank through the pressure interlocking of the buffer tanks according to the acquisition values of the first pressure gauge and the second pressure gauge;
the controller controls the total flow of ammonia and HF by controlling HF of the ammonia flow valve and the HF flow valve according to the acquisition values of the ammonia flow meter and the HF flow meter;
the controller realizes the liquid supplement of the electrolytic cell by controlling the flow valve door to be introduced into the electrolytic cell according to the acquisition value of the liquid level meter, automatically closes the flow valve door to be introduced into the electrolytic cell when the liquid level is supplemented to a required value, and controls the flow valve door to be introduced into the electrolytic cell to open and supplement the electrolyte when the liquid level is lower than the required value;
the controller can also obtain the ratio of HF to ammonia in the electrolyte according to the acquisition value of the densimeter in the electrolytic cell, compares the ratio with the required ratio, and adjusts the ratio of the ammonia to the HF by controlling the opening of the flow valve which is communicated into the electrolytic cell so as to enable the ratio to meet the set requirement.
The controller can also output the collected values of the ammonia gas flowmeter, the HF flowmeter, the electrolytic cell flowmeter of the ammonia gas pipeline, the electrolytic cell flowmeter of the HF pipeline and the liquid level meter to a display for displaying.
The above embodiments only describe the design principle of the present invention, and the shapes and names of the components in the description may be different without limitation. Therefore, a person skilled in the art of the present invention can modify or substitute the technical solutions described in the foregoing embodiments; the modifications and substitutions do not depart from the spirit and technical scope of the present invention, and shall all fall within the scope of the present invention.

Claims (7)

1. A feed system for a nitrogen trifluoride electrolyzer, characterized by comprising:
a liquid ammonia storage tank, an ammonia vaporizer, an ammonia buffer tank, a molecular sieve tower, a first filter and a check valve are sequentially connected along the flow direction of ammonia, and finally, the liquid ammonia is connected to an ammonia main pipeline; the ammonia buffer tank is provided with a first pressure gauge, and a first pressure interlocking valve for controlling the air inlet flow rate of the ammonia buffer tank is connected to a pipeline between the liquid ammonia storage tank and the ammonia vaporizer; the first pressure interlocking valve and the first pressure gauge are both connected with a controller to form an ammonia buffer tank pressure interlocking control loop; an ammonia flow valve for controlling the ammonia flow in the ammonia main pipeline and an ammonia flow meter for detecting the ammonia flow in the ammonia main pipeline are arranged on a pipeline between the check valve and the ammonia main pipeline; the ammonia flow valve and the ammonia flow meter are both connected with a controller to form an ammonia total flow interlocking control loop;
the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are sequentially connected along the flow direction of the hydrogen fluoride HF, and finally the HF storage tank, the HF vaporizer, the HF buffer tank and the second filter are connected to an HF main pipeline; the HF buffer tank is provided with a second pressure gauge, and a second pressure interlocking valve for controlling the air inlet flow rate of the HF buffer tank is connected to a pipeline between the HF storage tank and the HF vaporizer; the second pressure interlocking valve and the second pressure gauge are both connected with the controller to form an HF buffer tank pressure interlocking control loop; an HF flow valve for controlling HF flow in the HF main pipeline and an HF flow meter for detecting the HF flow in the HF main pipeline are arranged on a pipeline between the second filter and the HF main pipeline; the HF flow valve and the HF flowmeter are both connected with the controller to form an HF total flow linkage control loop;
a plurality of electrolytic tanks are connected in parallel and are respectively connected into the ammonia gas main pipeline and the HF main pipeline; a liquid level meter and a density meter are arranged in the electrolytic tank; the connecting pipeline of the electrolytic cell and the ammonia main pipeline and the connecting pipeline of the electrolytic cell and the HF main pipeline are both connected with an electrolytic cell flowmeter and an electrolytic cell lead-in flow valve for controlling the proportion of ammonia gas/HF entering the electrolytic cell; the electrolytic bath inlet flow valve and the liquid level meter are both connected with a controller to form a liquid level interlocking control loop; the densimeter is also connected with the controller and forms a component proportion control loop with the flow valve introduced into the electrolytic cell;
the liquid ammonia storage tank with the output pipeline of HF storage tank all links there is the delivery pump, and the delivery pump is connected the controller.
2. The system of claim 1, wherein the molecular sieve column comprises a 2-stage molecular sieve column.
3. The system of claim 1, wherein the molecular sieve column comprises two primary and secondary sets of molecular sieve columns in parallel.
4. The system of claim 1, wherein the first filter and the second filter each comprise two stages of filters in series, a coarse filter and a fine filter.
5. The system of claim 1, wherein a valve is provided between each two devices for shutting down when repairing or replacing the devices.
6. The system of claim 1, wherein the cell includes a temperature sensor and a heating device, each operatively connected to the controller, to control the cell temperature to between 80 ℃ and 130 ℃.
7. The system of claim 1, wherein the cell pressure is atmospheric.
CN202023127779.3U 2020-12-22 2020-12-22 Charging system of nitrogen trifluoride electrolytic cell Active CN214612782U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112626548A (en) * 2020-12-22 2021-04-09 中船重工(邯郸)派瑞特种气体有限公司 Charging system and method for nitrogen trifluoride electrolytic cell

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112626548A (en) * 2020-12-22 2021-04-09 中船重工(邯郸)派瑞特种气体有限公司 Charging system and method for nitrogen trifluoride electrolytic cell

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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1

Patentee after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd.

Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province

Patentee before: PERIC SPECIAL GASES Co.,Ltd.