CN210595272U - Ultrapure gas purification system based on normal temperature adsorption process - Google Patents
Ultrapure gas purification system based on normal temperature adsorption process Download PDFInfo
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Abstract
The utility model relates to a purification of bulk gas that uses in the conductor chip field of making. An ultrapure gas purification system based on a normal-temperature adsorption process comprises two adsorption reactors, corresponding switching valves, corresponding pipelines, a regenerated gas heater, a regenerated gas cooler and a control system, wherein the two adsorption reactors are used for preparing the ultrapure gas; the adsorption reactor is respectively filled with two kinds of fillers, and a deoxidizer and a nickel catalyst are sequentially filled from the inflow side to the outflow side of the raw material gas. The process is simple, the one-step method is used for removing impurities, the cost of the nickel catalyst is far higher than that of the deoxidizer, the adsorption capacity of the deoxidizer on oxygen, water and carbon dioxide is larger than that of the nickel catalyst, the raw material gas is firstly purified by the deoxidizer, ppm-level impurities in the raw material are firstly removed to 10ppb, and then the raw material gas passes through the nickel catalyst, and the nickel catalyst only needs to be filled with the adsorption quantity required for removing the 10ppb impurities, so that the filling quantity of the high-cost nickel catalyst can be reduced, and the purification cost is reduced.
Description
Technical Field
The utility model relates to a purification of bulk gas that uses in the conductor chip field of making specifically is nitrogen gas, argon gas purification based on normal atmospheric temperature adsorption process and is the purification system of ultrapure gas.
Background
The requirement of bulk gases such as nitrogen, argon and the like in the semiconductor chip manufacturing process mainly comes from cryogenic air separation, wherein the content of oxygen, water, carbon dioxide, carbon monoxide, hydrogen and non-methane hydrocarbons as impurities is in the ppm level, and the content of each impurity in the chip manufacturing process is generally required to be below 1ppb, so that the bulk gases need to be further purified to meet the process requirement.
In the purification of the existing adsorption process, only oxygen, water and carbon dioxide can be removed, if carbon monoxide, hydrogen and non-methane hydrocarbons need to be further removed, a catalytic oxidation process needs to be added at the front end of the adsorption process, the catalytic oxidation process needs to heat the gas to about 300 ℃ and then pass through a noble metal catalyst bed layer, and the aim is to oxidize the carbon monoxide, the hydrogen and the non-methane hydrocarbons in the gas into water and carbon dioxide and then remove the water and the carbon dioxide in the rear end adsorption process, so that the cost of a purifier is increased, the operation cost is increased due to the fact that the gas is heated to the reaction temperature, the complexity of the purifier is increased, and the operation reliability is reduced.
In the purification of the prior adsorption process, a regenerated gas heater and a regenerated gas cooler are used for regenerating two adsorption reactors by switching high-temperature-resistant valves, so that a high-temperature corrugated pipe valve needs to be introduced into the system, the valve can meet the conditions of only one American supplier at present, the cost is high, and the shelf life needs about twenty weeks.
Disclosure of Invention
An object of the utility model is to solve the above-mentioned not enough problem, provide a ultrapure gas purification system based on normal atmospheric temperature adsorption process, reduce clarifier investment cost and purification running cost by a wide margin, can also make the clarifier miniaturization, reduce the area occupied between power, on the other hand adopts the mode of 2 regeneration gas heaters, two regeneration gas coolers to avoid using high temperature bellows valve, can reduce the valve cost by a wide margin, reduces purchase cycle and supply of material cycle.
In order to solve the above problems, the utility model adopts the following technical scheme: an ultrapure gas purification system based on a normal-temperature adsorption process comprises two adsorption reactors, corresponding switching valves, corresponding pipelines, a regenerated gas heater, a regenerated gas cooler and a control system, wherein the two adsorption reactors are used for preparing the ultrapure gas; the adsorption reactor is respectively filled with two kinds of fillers, and a deoxidizer and a nickel catalyst are sequentially filled from the inflow side to the outflow side of the raw material gas.
The gas inlet of the adsorption reactor is connected with the feed gas inlet through a feed gas input pipeline and a switching valve, and the gas outlet of the adsorption reactor is connected with the product gas outlet through a product gas output pipeline and a switching valve; the feed gas input pipeline is communicated with a regeneration gas output pipeline through a bypass, the regeneration gas output pipeline is provided with a regeneration gas cooler and a switching valve, and the regeneration gas output pipeline is communicated with a gas release port; the product gas output pipeline bypass is connected with a regenerated gas input pipeline, and a regenerated gas heater and a switching valve are installed on the regenerated gas input pipeline.
The regenerated gas input pipeline is connected with a hydrogen inlet through a pipeline, and a hydrogen inlet valve is installed on the pipeline.
The switching valve adopts an electronic grade diaphragm valve or a corrugated pipe valve.
The filling volume ratio Va/Vb of the nickel catalyst and the deoxidizer is 0.1-0.6; further preferably, Va/Vb is 0.2 to 0.4.
The adsorption reactor is characterized in that a temperature measuring point is arranged on a bed layer of the adsorption reactor, the control system comprises a CPU central control unit, and the CPU central control unit is respectively connected with a flow switch, a pressure sensor, a temperature sensor, a relay, a contactor and a display panel.
Compared with the similar products in the field, the utility model, have outstanding substantive characteristics:
1. the system has simple structure, one of the two adsorption reactors is provided with an adsorption reactor, and the adsorption reactor is required to be automatically regenerated on line after adsorption saturation so as to recover the adsorption activity of the adsorption reactor, and the two adsorption reactors are respectively in the stages of normal-temperature adsorption purification and regeneration standby so as to achieve the purpose of continuous on-line work of the purifier;
2. the regenerated gas heater is separated from the adsorption reactor, so that the problems of nonuniform flow velocity of gas at each position in the container, difficult formation of stable turbulence and overlarge wall effect caused by a heater built-in mode of the reactor are solved;
3. the regenerated gas cooler cools the regenerated gas of the adsorption reactor, and the regenerated gas is discharged from the vent after passing through the valve, so that the temperature of the gas is reduced, and the regenerated gas can be controlled by adopting a universal valve in the electronic industry, thereby greatly reducing the system cost;
4. the process is simple, the one-step method is used for removing impurities, the cost of the nickel catalyst is far higher than that of the deoxidizer, the adsorption capacity of the deoxidizer on oxygen, water and carbon dioxide is larger than that of the nickel catalyst, the raw material gas is firstly purified by the deoxidizer, ppm-level impurities in the raw material are firstly removed to 10ppb, and then the raw material gas passes through the nickel catalyst, and the nickel catalyst only needs to be filled with the adsorption quantity required for removing the 10ppb impurities, so that the filling quantity of the high-cost nickel catalyst can be reduced, and the purification cost is reduced.
Drawings
Fig. 1 is a schematic view of the patent structure of the present invention.
In the figure: 1. the device comprises a raw material gas inlet, a raw material gas outlet, a product gas outlet, a vent port, a nickel catalyst layer, a deoxidizing agent layer, a hydrogen inlet valve, a raw material gas input pipeline, a regeneration gas output pipeline, a product gas output pipeline and a regeneration gas input pipeline, wherein the raw material gas inlet is 2, the product gas outlet is 3, the vent port is 4, the nickel catalyst layer is 5;
A. adsorption reactors A, B, adsorption reactors B, A1, switching valves A1, A2, switching valves A2, A3, switching valves A3, A4, switching valves A4, B1, switching valves B1, B2, switching valves B2, B3, switching valves B3, B4 and switching valves B4;
HA. The regeneration gas heaters HA and HB and the regeneration gas heater HB;
TA1, a regeneration gas heater HA temperature control point, TB1, a regeneration gas heater HB temperature control point, TA2, an adsorption reactor A bed temperature measurement point, TB2 and an adsorption reactor B bed temperature measurement point;
EA. Regeneration gas coolers EA, EB, regeneration gas cooler EB.
Detailed Description
The present invention will be further explained with reference to fig. 1:
the purification system of the utility model consists of two automatically switched adsorption reactors A and B, corresponding switching valves A1-A4, B1-B4, corresponding pipelines, corresponding regenerated gas heaters HA and HB and corresponding control systems; the adsorption reactors A and B are respectively filled with two kinds of fillers, and a deoxidizer and a nickel catalyst are sequentially filled from the inflow side to the outflow side of the raw material gas; when the filling amount of the nickel catalyst in the adsorption reactor is Va and the filling amount of the deoxidizer is Vb, the filling ratio Va/Vb of the nickel catalyst and the deoxidizer is 0.1 to 0.6, and more preferably 0.2 to 0.4.
An air inlet of the adsorption reactor is connected with a raw material gas inlet 1 through a raw material gas input pipeline 8 and a switching valve, and an air outlet of the adsorption reactor is connected with a product gas outlet 2 through a product gas output pipeline 10 and a switching valve; a raw gas input pipeline is communicated with a regeneration gas output pipeline 9 by a bypass, a regeneration gas cooler and a switching valve are arranged on the regeneration gas output pipeline, and the regeneration gas output pipeline is communicated with a gas release port; the product gas output pipeline bypass is connected with a regeneration gas input pipeline 11, and a regeneration gas heater and a switching valve are installed on the regeneration gas input pipeline.
Taking the example that the a adsorption reactor is in the purification stage, the raw material gas enters the purifier from the raw material gas inlet 1, the switching valve a1 and the switching valve a4 are in the open state, and the switching valve a2 and the switching valve A3 are in the closed state. The raw material gas enters an adsorption reactor A and then contacts with a stripperOxygen, water and carbon dioxide in the gas are absorbed to be below 10ppb by the oxygen agent bed layer 5, wherein the water and the carbon dioxide are physically absorbed, the oxygen is chemically absorbed, and the absorption principle is as follows: AO + O2-- →AO2Wherein AO represents a metal oxide as a deoxidizing effective component in the deoxidizing agent;
the gas oxygen, water and carbon dioxide passing through the deoxidizer bed layer are removed to be below 10ppb and then continuously flow into the nickel catalyst bed layer 4, and the nickel catalyst bed layer 4 can further remove the oxygen, water, carbon dioxide, carbon monoxide, hydrogen and non-methane hydrocarbons in the gas to be below 1 ppb.
Wherein the nickel catalyst bed layer 4 is filled with a regenerated nickel catalyst which has the capability of removing trace oxygen, water, carbon dioxide, carbon monoxide, hydrogen and non-methane hydrocarbons in the gas. Specifically, the nickel catalyst can be prepared by loading 20-80 wt% of metallic nickel on a carrier such as activated alumina, a zeolite molecular sieve, activated carbon or silica gel. Further preferably, a nickel catalyst having 30 to 50 wt% of a carrier is used.
The regeneration process is performed by a central control unit in a time sequence control manner, and the regeneration process of the adsorption reactor is described by taking the adsorption reactor B as an example with reference to fig. 1.
1) Pressure relief:
initial state: the valves B1-B4 are in a closed state, the pressure in the adsorption reactor B is the use pressure of the last purification stage, and is generally 0.6-0.8 Mpa; 5 seconds after the pressure relief operation starts, the central control unit gives a valve B2 opening signal, and the valve B2 is opened; and (3) finally flowing the gas in the adsorption reactor B to a high-level emptying position installed outdoors through a valve B2 and an emptying port 3 for emptying until the pressure in the adsorption reactor B is reduced to atmospheric pressure, wherein the process duration is 5-8 minutes.
2) Heating and purging 1:
the initial state is a pressure relief finished state, a valve B3 is opened, a part of product gas from the front end of a product gas outlet 2 passes through a valve B3 as regeneration gas, flows into an adsorption reactor B through a regeneration gas heater HB, passes through a regeneration gas cooler EB, a valve B2 and a vent 3, and finally flows to a high-level vent arranged outdoors, and meanwhile, the regeneration gas heater HB is started to heat the regeneration gas to 300 ℃ required by the regeneration process; the duration of the process is 6-8 hours.
Further, in the process, the high-temperature regeneration gas brings the water vapor adsorbed by the adsorption reactor B in the purification stage out of the bed layer and is discharged at a high position through a vent 3;
furthermore, the regeneration gas cooler EB is used for cooling the high-temperature regeneration gas to near normal temperature by air cooling and then emptying the cooled regeneration gas. This protects the valve B2 used at ambient temperature and reduces the risk of high temperature scalding of the pipeline between the vent line and the outdoor high-level vent.
Further, the flow rate of the regeneration gas is 5% of the treatment gas flow rate of the purifier; the process pressure was atmospheric.
3) Hydrogenation regeneration:
the initial state is the heating purge 1 state. And a hydrogen inlet valve 7 is opened, a certain amount of high-purity hydrogen is added into the regenerated gas, and the hydrogen is used as the reducing gas of the nickel catalyst bed layer and the deoxidizer bed layer to regenerate the adsorption reactor B. The duration of the process is 2-4 hours.
Further, the amount of hydrogen added is 3% of the amount of the regenerated gas, and the process pressure is normal pressure.
4) Heating and purging 2:
the initial state is a hydrogenation regeneration state. The hydrogen inlet valve 7 is closed and the high temperature regeneration gas carries the water produced in the adsorption reactor B during the hydrogenation regeneration phase out of the bed in gaseous form and vents it at a high level through vent 3.
The duration of the process is 2-4 hours.
Further, taking oxygen as an example, the principle of hydrogenation reduction is as follows: AO2+H2--→AO+H2O。
5) And (3) cooling:
the initial state is the heating purge 2 state. The regeneration gas heater HB stops heating, and the regeneration gas at normal temperature brings out the heat of the adsorption reactor until the reactor is cooled to normal temperature. The duration of the process is 8-10 hours.
6) Pressurizing for standby:
the initial state is a cooling state, the valve B2 is closed, the regenerated gas starts to pressurize the adsorption reactor B through the valve B3, when the pressure of the adsorption reactor B reaches the normal working pressure of the purifier, the valve B3 is closed, the adsorption reactor B enters a standby stage, and after the purification period of the adsorption reactor A is finished, the adsorption reactor A automatically enters a purification state, and the adsorption reactor A simultaneously enters an automatic regeneration process.
Claims (7)
1. An ultrapure gas purification system based on normal temperature adsorption technology which is characterized in that: comprises two adsorption reactors, corresponding switching valves, corresponding pipelines, a regenerated gas heater, a regenerated gas cooler and a control system; the adsorption reactor is respectively filled with two kinds of fillers, and a deoxidizer and a nickel catalyst are sequentially filled from the inflow side to the outflow side of the raw material gas.
2. The system for purifying ultrapure gas based on the ambient temperature adsorption process of claim 1, wherein: the gas inlet of the adsorption reactor is connected with the feed gas inlet through a feed gas input pipeline and a switching valve, and the gas outlet of the adsorption reactor is connected with the product gas outlet through a product gas output pipeline and a switching valve; the feed gas input pipeline is communicated with a regeneration gas output pipeline through a bypass, the regeneration gas output pipeline is provided with a regeneration gas cooler and a switching valve, and the regeneration gas output pipeline is communicated with a gas release port; the product gas output pipeline bypass is connected with a regenerated gas input pipeline, and a regenerated gas heater and a switching valve are installed on the regenerated gas input pipeline.
3. The system for purifying ultrapure gas based on the ambient temperature adsorption process of claim 2, wherein: the regenerated gas input pipeline is connected with a hydrogen inlet through a pipeline, and a hydrogen inlet valve is installed on the pipeline.
4. The system for purifying ultrapure gas based on the ambient temperature adsorption process of claim 1, wherein: the switching valve adopts an electronic grade diaphragm valve or a corrugated pipe valve.
5. The system for purifying ultrapure gas based on the ambient temperature adsorption process of claim 1, wherein: the filling volume ratio Va/Vb of the nickel catalyst and the deoxidizer is 0.1-0.6.
6. The system for purifying ultrapure gas based on the ambient temperature adsorption process of claim 1, wherein: the filling volume ratio Va/Vb of the nickel catalyst and the deoxidizer is 0.2-0.4.
7. The system for purifying ultrapure gas based on the ambient temperature adsorption process of claim 1, wherein: the adsorption reactor is characterized in that a temperature measuring point is arranged on a bed layer of the adsorption reactor, the control system comprises a CPU central control unit, and the CPU central control unit is respectively connected with a flow switch, a pressure sensor, a temperature sensor, a relay, a contactor and a display panel.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775671A (en) * | 2019-03-18 | 2019-05-21 | 大连华邦化学有限公司 | A kind of hyperpure gas purification system and technique based on room temperature absorbing process |
| CN113998678A (en) * | 2021-10-13 | 2022-02-01 | 安徽华中半导体材料有限公司 | Argon recovery and purification device and purification method thereof |
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2019
- 2019-03-18 CN CN201920337938.0U patent/CN210595272U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775671A (en) * | 2019-03-18 | 2019-05-21 | 大连华邦化学有限公司 | A kind of hyperpure gas purification system and technique based on room temperature absorbing process |
| CN109775671B (en) * | 2019-03-18 | 2023-08-15 | 大连华邦化学有限公司 | Ultra-pure gas purification system and process based on normal temperature adsorption process |
| CN113998678A (en) * | 2021-10-13 | 2022-02-01 | 安徽华中半导体材料有限公司 | Argon recovery and purification device and purification method thereof |
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