CN212982464U - Dedicated H of semiconductor2Purification system - Google Patents

Dedicated H of semiconductor2Purification system Download PDF

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Publication number
CN212982464U
CN212982464U CN202021524442.3U CN202021524442U CN212982464U CN 212982464 U CN212982464 U CN 212982464U CN 202021524442 U CN202021524442 U CN 202021524442U CN 212982464 U CN212982464 U CN 212982464U
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reactor
normal
temperature adsorption
outlet
adsorption reactor
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侯鹏
李文强
杨荣博
韩江江
李文豪
李世海
田维峰
阮方
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Dalian Huabang Chemical Co ltd
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Dalian Huabang Chemical Co ltd
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Abstract

The utility model discloses a dedicated H of semiconductor2Purification system, including normal atmospheric temperature adsorption reactor, its entry links to each other with the feed gas entry, the export is through the entry linkage of second heater and high temperature reactor of breathing in, the export of high temperature reactor of breathing in links to each other with the product gas export through dehydration reactor, be equipped with first cooler between high temperature reactor of breathing in and the dehydration reactor, the export of normal atmospheric temperature adsorption reactor links to each other with the regeneration gas entry through first heater, the entry of normal atmospheric temperature adsorption reactor passes through atmospheric valve and links to each other with the drain, normal atmospheric temperature adsorption reactorA second cooler is arranged on the pipeline between the inlet and the vent. Dedicated H of semiconductor2The purification system adopts the external heater, the high-temperature air suction reactor and the dehydration reactor, so that the heated gas is uniform, the utilization rate of the catalyst is high, the water vapor in the product gas can be effectively removed, and the purity of the product gas is improved.

Description

Dedicated H of semiconductor2Purification system
Technical Field
The utility model relates to a gas purification equipment technical field, concretely relates to dedicated H of semiconductor2And (4) purifying the system.
Background
With the rapid development of industries such as integrated circuits, the requirement on the purity of used gas in the manufacturing process of finished integrated circuit products is higher and higher, and the requirement on impurities is less than 1 ppb. The prior hydrogen purification technology mostly adopts a front-end catalysis and rear-end drying adsorption technology, the front-end catalysis technology can enable impurities to react to generate carbon dioxide and water, and the rear-end deep adsorption technology can adsorb and remove the impurities such as the carbon dioxide and the water. Although the technology can remove impurity hydrocarbons, carbon monoxide, carbon dioxide and water to a certain extent, the removal depth can not meet the production and use requirements.
SUMMERY OF THE UTILITY MODEL
The utility model provides a dedicated H of semiconductor to above problem2And (4) purifying the system.
The utility model discloses a technical means as follows:
dedicated H of semiconductor2Purification system, comprising a normal temperature absorberThe system comprises an attached reactor, a second heater, a high-temperature air suction reactor and a dehydration reactor; the entry of normal atmospheric temperature adsorption reactor links to each other with the feed gas entry, the export of normal atmospheric temperature adsorption reactor with the entry linkage of the high temperature reactor of breathing in, normal atmospheric temperature adsorption reactor with be equipped with between the high temperature reactor of breathing in the second heater, the export of the high temperature reactor of breathing in with the entry linkage of dehydration reactor, the export of dehydration reactor links to each other with the product gas export, the high temperature reactor of breathing in with be equipped with first cooler between the dehydration reactor, the export of normal atmospheric temperature adsorption reactor links to each other through regeneration gas admission pipe with the regeneration gas entry, be equipped with first heater on the regeneration gas admission pipe, the entry of normal atmospheric temperature adsorption reactor links to each other with the drain through the atmospheric valve, be equipped with the second cooler on the pipeline between the entry of normal atmospheric temperature adsorption reactor and the drain.
Further, a protective gas inlet is arranged between the normal-temperature adsorption reactor and the second heater.
Further, a heat exchanger is arranged between the normal-temperature adsorption reactor and the second heater, an outlet of the normal-temperature adsorption reactor is connected with a refrigerant inlet of the heat exchanger, a refrigerant outlet of the heat exchanger is connected with the second heater, a heat medium inlet of the heat exchanger is connected with an outlet of the high-temperature air suction reactor, and a heat medium outlet of the heat exchanger is connected with the first cooler.
Furthermore, a refrigerant inlet of the heat exchanger is connected with the shielding gas inlet.
Further, the device comprises two normal-temperature adsorption reactors connected in parallel, namely a first normal-temperature adsorption reactor and a second normal-temperature adsorption reactor, wherein an outlet of the first normal-temperature adsorption reactor is connected to a normal-temperature adsorption reactor outlet main pipe through a first normal-temperature adsorption reactor outlet branch pipe, an outlet of the second normal-temperature adsorption reactor is connected to a normal-temperature adsorption reactor outlet main pipe through a second normal-temperature adsorption reactor outlet branch pipe, a normal-temperature adsorption reactor outlet main pipe is connected with the high-temperature air suction reactor, a regeneration gas inlet pipe comprises a regeneration gas inlet pipe main pipe, a first regeneration gas inlet pipe branch pipe and a second regeneration gas inlet pipe branch pipe, an outlet of the first normal-temperature adsorption reactor is connected with the regeneration gas inlet pipe main pipe through the first regeneration gas inlet pipe branch pipe, and an outlet of the second normal-temperature adsorption reactor is connected with the regeneration gas inlet pipe main pipe through the second regeneration gas inlet pipe branch pipe, the device comprises a first normal temperature adsorption reactor, a first heater I, a first regeneration control valve, a second heater II, a second regeneration control valve, a hydrogenation pipeline, a check valve, a pressure reducer and a flow-limiting orifice plate, wherein the first heater I and the first regeneration control valve are arranged on a first regenerated gas discharging pipe branch pipe, the first heater II and the second regeneration control valve are arranged on a second regenerated gas discharging pipe branch pipe, the hydrogenation pipeline is also arranged between a normal temperature adsorption reactor outlet main pipe and a regenerated gas discharging pipe, the check valve, the pressure reducer and the flow-limiting orifice plate are arranged on the hydrogenation pipeline, the second cooler I is arranged on a pipeline between an inlet and an exhaust port of the first normal temperature adsorption reactor, and the second cooler II.
Further, a heating jacket is arranged outside the high-temperature air suction reactor.
Furthermore, the heating jacket is an electric heating jacket, the heating jacket is divided into an upper part and a lower part, and the power of the lower part of the heating jacket is greater than that of the upper part.
Furthermore, a deoxidizer and a nickel catalyst are sequentially filled in the normal-temperature adsorption reactor from the inlet side to the outlet side, and a zirconium-vanadium-iron getter is filled in the high-temperature gas suction reactor.
Furthermore, a product analysis sampling pipeline is arranged on a pipeline between the dehydration reactor and the product gas outlet and is connected with a product analysis sampling port.
Compared with the prior art, the special H for the semiconductor2The purification system has the advantages that by arranging the normal-temperature adsorption reactor, the second heater, the high-temperature air suction reactor and the dehydration reactor, the heating gas is uniform, the utilization rate of the catalyst is high, the problem that dead gas or temperature is not required is reduced, impurities in raw materials can be deeply removed, and meanwhile, due to the arrangement of the dehydration reactor, the dehydration reactor can effectively remove a heat exchanger,The cooler and the like avoid blowing the high-temperature air suction reactor for a long time in large amount due to the fact that the tube side and the shell side contact with water molecules attached to air in the transportation process, and the index of impurity water is rapidly reduced.
Drawings
FIG. 1 shows the utility model discloses a special H for semiconductor2Structure diagram of purification system.
In the figure: 1. a raw material gas inlet, 2, a regeneration gas inlet, 3, an emptying port, 4, a protective gas inlet, 5, a product analysis sampling port, 6, a product gas outlet, 7, a first normal-temperature adsorption reactor, 8, a second normal-temperature adsorption reactor, 9, a heat exchanger, 10, a high-temperature air suction reactor, 11, a second cooler I, 12, a second cooler II, 13, a first cooler, 14, a hydrogenation valve, 15, a first regeneration air control valve, 16, a second regeneration air control valve, 18, a first adsorber outlet valve, a first emptying valve 19, 20, a second emptying valve, 21, a second adsorber outlet valve, 22, a regeneration gas main control valve, 23, a protective air control valve, 24, an air suction process control valve, 25, a first heater I, 26, a first heater II, 27, a second heater, 28, a one-way valve, 29, a pressure reducer, 30, a flow limiting orifice plate, 31, a heating sleeve, 33. the system comprises a hydrogenation pipeline, 34 a product analysis sampling pipeline, 35 a dehydration reactor, 36 a first normal temperature adsorption reactor outlet branch pipe, 37 a second normal temperature adsorption reactor outlet branch pipe, 38 a normal temperature adsorption reactor outlet main pipe, 39 a regeneration gas discharging main pipe, 40 a first regeneration gas discharging pipe branch pipe, and 41 a second regeneration gas discharging pipe branch pipe.
Detailed Description
As shown in fig. 1, the utility model discloses a special purpose of semiconductor H2A purification system comprising a normal temperature adsorption reactor, a second heater 27, a high temperature air suction reactor 10 and a dehydration reactor 35; the entry of normal atmospheric temperature adsorption reactor links to each other with feed gas inlet 1, the export of normal atmospheric temperature adsorption reactor with the entry linkage of high temperature reactor 10 of breathing in, normal atmospheric temperature adsorption reactor with be equipped with between the high temperature reactor 10 of breathing in second heater 27, the export of high temperature reactor 10 of breathing in with dehydration reactor 35's entry linkage, the anti-entry linkage of dehydrationThe export of reactor 35 links to each other with product gas outlet 6, high temperature breathe in reactor 10 with be equipped with first cooler 13 between dehydration reactor 35, the export of normal atmospheric temperature adsorption reactor links to each other with regeneration gas entry 2 through regeneration gas discharge pipe 32, be equipped with first heater on the regeneration gas discharge pipe, the entry of normal atmospheric temperature adsorption reactor passes through the atmospheric valve and links to each other with drain 3, be equipped with the second cooler on the pipeline between the entry of normal atmospheric temperature adsorption reactor and the drain 3. The molecular sieve in the dehydration reactor 35 is a synthetic water with molecular screening function and aluminosilicate (zeolite) or natural zeolite, and is white powder with particle size of 0.5-10 μm, and can be extruded into strip, sheet or sphere by adding binder. The molecular sieve is non-toxic, tasteless, non-corrosive, insoluble in water and organic solvent, and soluble in strong acid and strong alkali. The molecular sieve loses crystal water after being heated, a plurality of holes are formed in the crystal, and the pore size is similar to the diameter of a plurality of gas molecules and is very uniform. It can suck gas molecules smaller than the pore diameter into the pores and exclude molecules larger than the pore diameter. Can get rid of the adnexed hydrone of tube side and shell side contact air in heat exchanger, the cooler fast at normal atmospheric temperature, avoid long-time atmospheric quantity to sweep the high temperature reactor rear end of breathing in, reduce impurity water index fast, because there is the filter at the rear end, the hydrone does not blow into the filter of polytetrafluoroethylene material through dehydration reactor, can remain the hydrone on the filter core and hardly get rid of, leads to the product gas unqualified always, and the process may be as long as about half a year. The two ends of the dehydration reactor are in threaded connection, so that the dehydration reactor is convenient to disassemble, can be replaced and regenerated after adsorption saturation, and achieves the purpose of recycling. Compared with the prior device, the device can reduce the water content in the product gas more quickly and meet the rear-end use requirement.
Preferably, the utility model discloses a dedicated H of semiconductor2The purification system comprises two normal-temperature adsorption reactors connected in parallel, namely a first normal-temperature adsorption reactor 7 and a second normal-temperature adsorption reactor 8, wherein the outlet of the first normal-temperature adsorption reactor 7 is connected to the outlet main pipe 38 of the normal-temperature adsorption reactor through an outlet branch pipe 36 of the first normal-temperature adsorption reactor, and the outlet of the second normal-temperature adsorption reactor 8 is connected to the outlet main pipe 38 of the normal-temperature adsorption reactor through an outlet branch pipe 36 of the second normal-temperature adsorption reactorThe outlet branch pipe 37 of the second normal temperature adsorption reactor is connected to the outlet main pipe 38 of the normal temperature adsorption reactor, the outlet main pipe 38 of the normal temperature adsorption reactor is provided with a gas suction process control valve 24, the outlet branch pipe 36 of the first normal temperature adsorption reactor is provided with a first adsorber outlet valve 18, the outlet branch pipe 37 of the second normal temperature adsorption reactor is provided with a second adsorber outlet valve 21, the outlet main pipe 38 of the normal temperature adsorption reactor is connected with the high temperature gas suction reactor 10, the regeneration gas inlet pipe comprises a regeneration gas inlet pipe main pipe 39, a first regeneration gas inlet pipe branch pipe 40 and a second regeneration gas inlet pipe branch pipe 41, the outlet of the first normal temperature adsorption reactor 7 is connected with the regeneration gas inlet pipe main pipe 39 through the first regeneration gas inlet pipe branch pipe 40, the outlet of the second normal temperature adsorption reactor 8 is connected with the regeneration gas inlet pipe main pipe 39 through the second regeneration gas inlet pipe branch pipe 41, the main pipe of the regeneration gas discharging pipe is connected with the regeneration gas inlet 2, the first regeneration gas discharging pipe branch pipe 40 is provided with a first heater I25 and a first regeneration control valve 15, the second regeneration gas discharge pipe branch pipe 41 is provided with a first heater II 26 and a second regeneration gas control valve 16, a hydrogenation pipeline 33 is also arranged between the outlet main pipe 38 of the normal temperature adsorption reactor and the regenerated gas discharge pipe, the hydrogenation pipeline 33 is provided with a one-way valve 28, a pressure reducer 29 and a flow-limiting orifice plate 30, a second cooler I11 is arranged on a pipeline between the inlet of the first normal-temperature adsorption reactor 7 and the vent 3, and a first vent valve 19 is arranged between the first cooler I11 and the vent 3, a second cooler II 12 is arranged on a pipeline between the inlet of the second normal-temperature adsorption reactor 8 and the vent 3, and a second vent valve 20 is arranged between the second cooler II 12 and the vent 3. The hydrogenation pipeline adopts a mode of combining a check valve 28, a pressure reducer 29 and a flow-limiting pore plate 30, the interface is a VCR interface, the tightness of the hydrogen pipeline is improved, and the flow-limiting device is more stable compared with the traditional flow meter, the flow-limiting pore plate is a single-pore single plate, the flow-limiting pore plate is used for limiting the flow of fluid, the pressure drop is generated when the fluid passes through the pore plate, the flow passing through the pore plate is increased along with the increase of the pressure drop, the pressure at the front section of the pore plate is ensured by adjusting the pressure reducer, so the hydrogen flow is ensured, the service life is,and is safer.
Still be equipped with heat exchanger 9 between normal atmospheric temperature adsorption reactor with the second heater 27, normal atmospheric temperature adsorption reactor export person in charge 38 with the refrigerant inlet connection of heat exchanger 9, the refrigerant export of heat exchanger 9 with the second heater 27 is connected, the heat medium entry of heat exchanger 9 with the exit linkage of high temperature reactor 10 of breathing in, the heat medium export of heat exchanger 9 with first cooler 13 is connected, the export of first cooler 13 and the entry linkage of dehydration reactor 35, the exit linkage product gas export 6 of dehydration reactor 35. Through setting up heat exchanger 9 for carry out the heat exchange by the gas of export in the normal atmospheric temperature adsorption reactor with the gas of export in the high temperature reactor of breathing in the heat exchanger, promptly through the gas of export in the high temperature reactor of breathing in to the gas that flows into the second heater has preheated, the temperature of the gas of input second heater of improvement has reduced the temperature of the gas of input to first cooler simultaneously, reduces the power of second heater and first cooler, has saved the consumption of energy.
A protective gas inlet 4 is also arranged between the normal temperature adsorption reactor and the second heater 27. Specifically, the shielding gas inlet 4 is connected with a refrigerant inlet of the heat exchanger 9 through a pipeline, and a shielding gas control valve 23 is arranged on the pipeline between the shielding gas inlet and the heat exchanger.
The high temperature reactor 10 of breathing in is equipped with heating jacket 31 in the outside, cooperates with external second heater, heats for the gas that gets into high temperature reactor 10 of breathing in jointly. In the case of a small flow rate of the conventional device, the upper temperature is far higher than the lower temperature, so that the lower temperature does not reach the use temperature requirement, while the heating jacket 31 of the present embodiment is an electric heating jacket, the heating jacket 31 is divided into an upper part and a lower part, the power of the lower part of the heating jacket 31 is greater than that of the upper part, when the small flow rate of gas enters the upper temperature to reach the use temperature, because the lower heating power is greater than the upper heating power and the lower set temperature is greater than the upper set temperature, the lower temperature cannot reach the use temperature under the small flow rate condition, and if the lower heating power is too small, the heating temperature cannot reach the set requirement.
And the normal-temperature adsorption reactor is sequentially filled with a deoxidizing agent and a nickel catalyst from the inlet side to the outlet side, and the high-temperature air suction reactor is filled with a zirconium-vanadium-iron getter. In this embodiment, the first normal temperature adsorption reactor 7 and the second normal temperature adsorption reactor 8 adopt a lower end air intake mode, and the high temperature air intake reactor 10 is filled with a zirconium vanadium iron getter.
A product analysis sampling pipeline 34 is arranged on a pipeline between the dehydration reactor 35 and the product gas outlet 6, and the product analysis sampling pipeline 34 is connected with the product analysis sampling port 5.
The cooler adopts air cooling when the flow rate of the raw material gas is less than 100 cubic meters per hour. The air cooling is that air is used as a medium to cool an object to be cooled, a cooling device is added with radiating fins or a surface cooling device through a coil pipe to increase the contact area, and fans are arranged to enhance the ventilation and enhance the cooling effect, the air cooling is composed of two groups or four groups, each group of air cooling is provided with two fans, when part of the fans need to be replaced, the air cooling does not need to stop producing gas, the replacement can be carried out on line, the air cooling is lower in cost than cooling water in the service life, and the maintenance is convenient and can realize the maintenance of producing gas without stopping.
At normal temperature, raw material hydrogen enters a normal temperature adsorption reactor from a raw material gas inlet 1 through an inlet valve to remove impurities such as oxygen, carbon monoxide, carbon dioxide, water, hydrocarbon and the like in the raw material hydrogen, a first normal temperature adsorption reactor 7 and a second normal temperature adsorption reactor 8 are used for standby, a deoxidizing agent in the normal temperature adsorption reactors removes the oxygen, the water and the carbon dioxide in the raw material hydrogen to be below 10ppb, a nickel catalyst continuously removes the rest oxygen, the water and the carbon dioxide to be below 1ppb, simultaneously removes the carbon monoxide and the non-methane hydrocarbon to be below 1ppb, one normal temperature adsorption reactor is switched to regenerate after being adsorbed and saturated, and the regeneration temperature is 200-250 ℃. The cost of the nickel catalyst is far higher than that of the deoxidizer, the adsorption capacity of the deoxidizer for oxygen, water and carbon dioxide is larger than that of the nickel catalyst, the raw gas in the embodiment is firstly purified by the deoxidizer to remove ppm-level impurities in the raw gas to 10ppb, and then passes through the nickel catalyst, and the nickel catalyst only needs to be filled with the adsorption quantity required for removing 10ppb impurities, so that the filling quantity of the high-cost nickel catalyst can be reduced, the purification cost is reduced, the regeneration times are reduced, the valve action is reduced, and the service life of equipment is prolonged.
The hydrogen gas after the low temperature adsorption process enters a heat exchanger 9 through a valve and then enters a high temperature gas suction reactor 10, impurities such as methane, nitrogen and the like in the hydrogen gas are removed, and the purified hydrogen gas is sent to a dehydration reactor 35 through a cooler to be dehydrated and then sent to a product gas outlet 6. The working temperature of the high-temperature gas suction reactor is 350-400 ℃, and the zirconium-vanadium-iron getter in the high-temperature gas suction reactor 10 is a Fischer-Tropsch type getter and an alloy type intermetallic compound getter, and has different adsorption capacities on various gases. The getter generates violent phase change after being activated at the high temperature of 300 ℃ and 400 ℃, so that the getter has higher gas suction rate. The getter can react with trace impurities such as nitrogen, oxygen, methane, carbon monoxide, carbon dioxide, water and the like mixed in the hydrogen within the temperature range of 350-450 ℃, and can irreversibly adsorb other gases except the hydrogen. The getter is activated before use by heating to 350-450 deg.C in vacuum or inert atmosphere to generate a highly active surface.
The first normal temperature adsorption reactor 7 and the second normal temperature adsorption reactor 8 are used for one purpose, and the working process will be described below by taking the first normal temperature adsorption reactor 7 as an example and the second normal temperature adsorption reactor 8 as an example.
(1) Pressure relief before regeneration
Initial state: the valve at the inlet of the second normal temperature adsorption reactor 8 is in a closed state, the outlet valve 21 of the second adsorber is closed, and the pressure in the second normal temperature adsorption reactor 8 is the use pressure of the last purification stage, generally 0.6-0.8 MPa. 5 seconds after the pressure relief operation starts, the PLC control unit gives a valve opening signal to the second emptying valve 20, the second emptying valve 20 is opened, the gas in the second normal-temperature adsorption reactor 8 flows to a high-position emptying position installed outdoors through the second emptying valve 20 and the emptying port 3 to be emptied until the pressure in the second normal-temperature adsorption reactor 8 is reduced to the atmospheric pressure, and the process duration is 5-8 minutes.
(2) Heating and purging
The initial state is a pressure relief finished state, the regeneration gas main control valve 22 is opened, argon from an external gas source is used as regeneration gas, enters the second normal-temperature adsorption reactor 8 through the second regeneration control valve 16, and flows to a high-position emptying part arranged outdoors through the second cooler II 12, the second emptying valve 20 and the emptying port 3. Meanwhile, the first heater II starts heating, and the purpose is to heat the regeneration gas to the temperature required by the regeneration process, wherein the regeneration temperature is 200-250 ℃. The heating purge process lasts 6-8 hours. In the process, the high-temperature regeneration gas takes the water vapor adsorbed in the second normal-temperature adsorption reactor 8 in the purification stage out of the bed layer and is discharged at high position through the vent 3. The second cooler II 12 is used for cooling the high-temperature regeneration gas to be close to normal temperature in an air cooling mode and then emptying the regeneration gas, so that the second emptying valve 20 used at normal temperature can be protected, and the risk of high-temperature scalding of the pipeline between the emptying pipeline and the outdoor high-position emptying position is reduced. The regeneration pressure is normal pressure.
(3) Hydrogenation regeneration
The initial state is a heating purge state. The hydrogenation valve 14 is opened, hydrogen enters a hydrogenation pipeline from the outlet main pipe of the normal temperature adsorption reactor, and enters a regeneration gas discharge pipe through a check valve 28, a pressure reducer 29 and a flow-limiting orifice plate 30 on the hydrogenation pipeline, a certain amount of high-purity hydrogen is added into the regeneration gas, the hydrogen is used as reducing gas of a nickel catalyst bed layer and a deoxidizer bed layer to regenerate the second normal temperature adsorption reactor 8, and the duration of the process is 2-4 hours. The adding amount of hydrogen is 1-10% of the regeneration gas amount, and the pressure in the regeneration process is normal pressure.
(4) Heating and purging
The initial state is a hydrogenation regeneration state. The hydrogenation valve 14 is closed, and the high-temperature regeneration gas carries the water generated in the hydrogenation regeneration stage of the second normal-temperature adsorption reactor 8 out of the bed layer in a gaseous state and is discharged in an elevated mode through a vent 3 for 2-4 hours. Taking oxygen as an example, the principle of hydrogenation reduction is as follows: AO2+H2→AO+H2O。
(5) Cooling down
The initial state is a heating purge state. And stopping heating by the first heater II, taking the heat of the second normal-temperature adsorption reactor 8 out by the regeneration gas at the normal temperature until the reactor is cooled to the normal temperature, and continuing the process for 8-10 hours.
(6) Pressurizing for standby
The initial state is a cooling state, the second emptying valve 20 is closed, the regeneration gas starts to pressurize the second normal-temperature adsorption reactor 8 through the second regeneration control valve 16, when the pressure of the second normal-temperature adsorption reactor 8 reaches the normal working pressure of the purifier, the second regeneration control valve 16 is closed, and the second normal-temperature adsorption reactor 8 enters a standby stage. After the purification period of the first normal temperature adsorption reactor 7 is finished, the purification state is automatically entered, and the first normal temperature adsorption reactor 7 simultaneously enters the regeneration process.
(7) Activation of gettering process
The initial state is the normal gas production state of the adsorption process. The raw gas enters the high-temperature air suction reactor through the heat exchanger 9 after passing through the adsorption process, the air suction process control valve 24 is closed before the heat exchanger is opened for the first time, the high-temperature air suction reactor 10 is heated by the heating sleeve to rise the temperature, meanwhile, the protective control valve 23 is opened, and argon of an external gas source enters the high-temperature air suction reactor 10 from the protective gas inlet 4 through the heat exchanger 9 and the second heater to rise the temperature of the reactor. When the temperature reaches 250-350 ℃, the control valve 24 of the air suction procedure is operated, when the temperature reaches 350-400 ℃, and the temperature is not obviously increased by introducing hydrogen, the protective air control valve 23 is closed, the argon in the high-temperature air suction reactor 10 is replaced, and air supply can be carried out after the replacement is finished. The opening of the gas suction process control valve 24 is operated by observing the temperature of the high temperature gas suction reactor 10 by operating the gas suction process control valve 24. The replacement operation is to open the gas suction process control valve 24 and close the protective gas control valve 23, and when the high temperature gas suction reactor 10 is at a certain pre-system pressure, close the gas suction process control valve 24, open the product gas outlet 6, relieve the pressure of the high temperature gas suction reactor 10 to the normal pressure, close the product gas outlet 6, and open the gas suction process control valve 24, and this operation is replacement, and the number of times of replacement is related to the volume of the reactor and the pre-system pressure. The gettering process needs to be activated once for use, but the content of gaseous impurities in the feed gas may affect the lifetime of the high temperature gettering reactor 10.
The system can realize full-automatic unmanned operation, the whole system adopts a SMART200 programmable controller of Siemens company, SMARTLINE700IE touch display monitors the whole equipment in real time, and the system has the functions of automatic regeneration, manual operation, operation monitoring and the like. The system can access a customer central control system, and has two connection modes of RS485 and Ethernet. The temperature system of the system comprises a PLC, a solid-state relay, thermocouples, heating rods and the like, wherein the temperature of each reactor is transmitted to the PLC by the thermocouples, and the PLC records all alarm information in a report form according to a historical data table. The control system can judge according to the temperature, pressure and other data of the reactor, and can give an alarm or interlock when the detected data is higher than a set value. In order to ensure the reliability of temperature control of equipment, the temperature of the reactor adopts a plurality of control points, the alarm point in the middle of the reactor, the alarm point at the lower part of the reactor packing and the ultrahigh temperature can cut off the main power supply. When the feedback signal obtained by the PLC is abnormal and the time continuously exceeds the set alarm value and exceeds the wave-resisting time delay (false alarm caused by wave motion is avoided), the device sends out an alarm signal, and the device still keeps a purification gas production state during alarm. Part of alarm signals are not processed within the set time, or the signals exceed the standard and reach the set interlocking value, and the device automatically adopts corresponding interlocking counter-sense according to the situation so as to avoid the occurrence of dangerous accidents. After the interlock is released, the state before the interlock is recovered to continue the operation.
The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.

Claims (8)

1. Dedicated H of semiconductor2A purification system, characterized by: comprises a normal temperature adsorption reactor, a second heater, a high temperature air suction reactor and a dehydration reactor; the inlet of the normal temperature adsorption reactor is connected with the feed gas inlet, and the outlet of the normal temperature adsorption reactorThe mouth with the high temperature inhales the entry linkage of reactor, normal atmospheric temperature adsorption reactor with the high temperature is inhaled and is equipped with between the reactor the second heater, the high temperature inhale the export of reactor with the entry linkage of dehydration reactor, the export of dehydration reactor links to each other with the product gas export, the high temperature inhale the reactor with be equipped with first cooler between the dehydration reactor, the export of normal atmospheric temperature adsorption reactor links to each other through the regeneration gas admission pipe with the regeneration gas entry, be equipped with first heater on the regeneration gas admission pipe, the entry of normal atmospheric temperature adsorption reactor passes through the atmospheric valve and links to each other with the drain, be equipped with the second cooler on the pipeline between the entry of normal atmospheric temperature adsorption reactor and the drain.
2. H specific to semiconductor according to claim 12A purification system, characterized by: and a protective gas inlet is also arranged between the normal-temperature adsorption reactor and the second heater.
3. H specific to semiconductor according to claim 22A purification system, characterized by: the heat exchanger is further arranged between the normal-temperature adsorption reactor and the second heater, an outlet of the normal-temperature adsorption reactor is connected with a refrigerant inlet of the heat exchanger, a refrigerant outlet of the heat exchanger is connected with the second heater, a heat medium inlet of the heat exchanger is connected with an outlet of the high-temperature air suction reactor, and a heat medium outlet of the heat exchanger is connected with the first cooler.
4. H specific to semiconductor according to claim 32A purification system, characterized by: and a refrigerant inlet of the heat exchanger is connected with the protective gas inlet.
5. H dedicated to semiconductors according to any of claims 1 to 42A purification system, characterized by: comprises two parallel normal temperature adsorption reactors, namely a first normal temperature adsorption reactor and a second normal temperature adsorption reactor, wherein the first normal temperature adsorption reactorThe outlet of the reactor is connected to a normal temperature adsorption reactor outlet main pipe through a first normal temperature adsorption reactor outlet branch pipe, the outlet of a second normal temperature adsorption reactor is connected to a normal temperature adsorption reactor outlet main pipe through a second normal temperature adsorption reactor outlet branch pipe, the normal temperature adsorption reactor outlet main pipe is connected with the high temperature air suction reactor, the regeneration gas inlet pipe comprises a regeneration gas inlet pipe main pipe, a first regeneration gas inlet pipe branch pipe and a second regeneration gas inlet pipe branch pipe, the outlet of the first normal temperature adsorption reactor is connected with the regeneration gas inlet pipe main pipe through the first regeneration gas inlet pipe branch pipe, the outlet of the second normal temperature adsorption reactor is connected with the regeneration gas inlet pipe main pipe through the second regeneration gas inlet pipe branch pipe, and the first regeneration gas inlet pipe branch pipe is provided with a first heater I and a first regeneration control valve, the second regeneration gas is gone into to be equipped with first heater II and second regeneration air control valve on the pipe branch, the normal atmospheric temperature adsorption reactor export be responsible for with still be equipped with the hydrogenation pipeline between the regeneration gas admission pipe, be equipped with check valve, pressure reducer and current-limiting orifice plate on the hydrogenation pipeline, be equipped with second cooler I on the pipeline between the entry of first normal atmospheric temperature adsorption reactor and the drain, be equipped with second cooler II on the pipeline between the entry of second normal atmospheric temperature adsorption reactor and the drain.
6. H specific to semiconductor according to claim 12A purification system, characterized by: and a heating sleeve is arranged outside the high-temperature air suction reactor.
7. H specific to semiconductor according to claim 62A purification system, characterized by: the heating jacket is an electric heating jacket, the heating jacket is divided into an upper part and a lower part, and the power of the lower part of the heating jacket is greater than that of the upper part.
8. H specific to semiconductor according to claim 12A purification system, characterized by: a product branch is arranged on a pipeline between the dehydration reactor and the product gas outletAnd the product analysis sampling pipeline is connected with the product analysis sampling port.
CN202021524442.3U 2020-07-28 2020-07-28 Dedicated H of semiconductor2Purification system Active CN212982464U (en)

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CN113501497A (en) * 2021-07-06 2021-10-15 湖北力拓能源化工装备有限公司 Method for purifying hydrogen

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113501497A (en) * 2021-07-06 2021-10-15 湖北力拓能源化工装备有限公司 Method for purifying hydrogen

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