CN109340578A - A kind of liquefied gas purification devices and method - Google Patents

A kind of liquefied gas purification devices and method Download PDF

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Publication number
CN109340578A
CN109340578A CN201811481825.4A CN201811481825A CN109340578A CN 109340578 A CN109340578 A CN 109340578A CN 201811481825 A CN201811481825 A CN 201811481825A CN 109340578 A CN109340578 A CN 109340578A
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China
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liquefied gas
storage device
gas
gas storage
liquefied
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CN201811481825.4A
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Chinese (zh)
Inventor
李东升
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SHANGHAI ZHENGFAN TECHNOLOGY Co Ltd
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SHANGHAI ZHENGFAN TECHNOLOGY Co Ltd
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Priority to CN201811481825.4A priority Critical patent/CN109340578A/en
Publication of CN109340578A publication Critical patent/CN109340578A/en
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17DPIPE-LINE SYSTEMS; PIPE-LINES
    • F17D3/00Arrangements for supervising or controlling working operations
    • F17D3/01Arrangements for supervising or controlling working operations for controlling, signalling, or supervising the conveyance of a product

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)

Abstract

The present invention relates to a kind of liquefied gas purification devices and methods, described device includes liquefied gas storage device, cooling device, heat riser and gas blow-off system, the heat riser is set to the lower part of liquefied gas storage device, the cooling device is set to liquefied gas storage device top, the gas blow-off system is connect with the outlet at the top of liquefied gas storage device, for discharging incoagulable gas.In purification process, liquefied gas storage device lower part is heated first, while liquefied gas storage device top is cooled down, then incoagulable gas is discharged.The content of incoagulability foreign gas in liquefied gas can be reduced to ppb grades by ppm grades by the present invention, the adverse effect that foreign gas is reduced to the highly purified of liquefied gas to subsequent manufacturing procedures is realized, and device is simple, it is easy to operate, with good economic efficiency and application prospect.

Description

A kind of liquefied gas purification devices and method
Technical field
The present invention relates to liquefied gas purification arts, and in particular to a kind of liquefied gas purification devices and method.
Background technique
High-purity special gas is the important source material of semiconductor industry.Its purity requirement is usually 99.9999% or more.It is high-purity Special gas is commonly stored in steel cylinder, is divided into high pressure gas and liquefied gas.Liquefied gas is generally stored in steel cylinder, some Incoagulability foreign gas (such as nitrogen, oxygen, hydrogen, methane, carbon monoxide) can be dissolved in liquid phase.Make in high-purity special gas With in the process, these foreign gases can be parsed, and cause adverse effect to semiconductor fabrication process.
The prior art generallys use the methods of rectifying, catalytic adsorption, UF membrane and purifies to high-purity special gas.This Outside, gas to be purified is first passed through heat-exchange system cooling by the operation that portion of techniques personnel are purified by the way of heat exchange It handles, then completes the separation of foreign gas and liquefied gas in separation system.
CN207527912U provides device and the cold energy recycling system of the general pure liquefied gas high purity liquefied gas of one kind System, the device of the general pure liquefied gas high purity liquefied gas includes heat exchanger, supercharger and the first purification system, heat exchanger On be provided with general pure gasifying liquefied gas channel and high-purity gas heat releasing passage, the entrance of supercharger and general pure gasifying liquefied gas The outlet of the outlet in channel, supercharger is connected to the entrance of the first purification system, the outlet and heat exchange of the first purification system The entrance of high-purity gas heat releasing passage on device is connected to.The cooling capacity of material gasification can be recycled, pressurized general pure gas The high-purity gas that body purifies can absorb material gasification cooling capacity and be changed into liquid, be not necessarily to outer semen donors.
CN108579314A provides the purification devices and method of a kind of liquefied gas, described device include: heat-exchange system and Separation system, the heat-exchange system are connected between material inlet and the feed inlet of the separation system, the separation system Outlet for product be connected to the heat-exchange system, then access product storage tank, heat-transfer working medium is equipped in the heat-exchange system so that Heat is absorbed or discharged by the material of the heat-exchange system.
Although the mode of heat exchange can be realized the purifying of liquefied gas, structure is complex, need in purification process Will be re-liquefied after gasifying liquefied gas, whole process is complicated for operation, consumes a large amount of energy, is unfavorable for the control of cost.
Summary of the invention
In view of problems of the prior art, the purpose of the present invention is to provide a kind of liquefied gas purification devices and sides Method is realized to the highly purified of liquefied gas, and the content of incoagulability foreign gas can be reduced to by ppm grades in liquefied gas Ppb grades, with good economic efficiency and application prospect.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of liquefied gas purification devices, described device include liquefied gas storage device, Cooling device, heat riser and gas blow-off system, the heat riser is set to the lower part of liquefied gas storage device, described cold But device is set to liquefied gas storage device top, and the gas blow-off system is connect with the outlet at the top of liquefied gas storage device, For discharging incoagulable gas.
The present invention utilizes the device of above-mentioned offer, first heats liquefied gas storage device, so that in liquefied gas Foreign gas (incoagulable gas) volatilization, then cooled down on reservoir top, make volatilization liquefied gas condensation, impurity Gas is then retained in reservoir top, is then arranged the foreign gas on reservoir top using gas blow-off system (negative pressure device) Out, and then purifying to liquefied gas is realized, reduces adverse effect of the foreign gas to subsequent manufacturing procedures.
Preferably, the cooling device is set to the outside of liquefied gas storage device.
Preferably, the cooling device is located at liquefied gas storage device liquid level or more.
Preferably, the gas blow-off system is negative pressure device.
Preferably, the gas blow-off system is connected with gas collector.
Preferably, the liquefied gas storage device is steel cylinder.
Preferably, the interface of liquefied gas storage device upper and lower part is the liquid level of liquefied gas.
Second aspect, the present invention provides a kind of liquefied gas purification process, the methods are as follows: to liquefied gas storage device Lower part is heated, while being cooled down using cooling device to liquefied gas storage device top, then control and liquefied gas Incoagulable gas is discharged the exhaust apparatus of reservoir top exit connection.
Preferably, the interface of the reservoir upper and lower part is the liquid level of liquefied gas, to liquefied gas storage device It lower part should be as close as possible to liquefied gas storage device bottom when heating.
Preferably, the temperature of the heating is 30-50 DEG C, such as can be 30 DEG C, 33 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 43 DEG C, 45 DEG C, 48 DEG C or the specific point value between 50 DEG C and above-mentioned numerical value, as space is limited and for concise consideration, the present invention No longer exclusive list.
Preferably, the time of the heating be 1-3h, such as can be 1h, 1.3h, 1.5h, 1.8h, 2h, 2.3h, 2.5h, Specific point value between 2.8h or 3h and above-mentioned numerical value, as space is limited and for concise consideration, the no longer exhaustive column of the present invention It lifts.
Preferably, the liquefied gas is any one in arsine, phosphine or ammonia.
Preferably, the incoagulable gas is at least one of nitrogen, oxygen, hydrogen, methane or carbon monoxide, such as It can be any one in nitrogen, oxygen, hydrogen, methane or carbon monoxide, typical but non-limiting combination are as follows: nitrogen and oxygen Gas, hydrogen and methane, nitrogen and carbon monoxide, oxygen and hydrogen, methane and carbon monoxide, nitrogen, oxygen and hydrogen etc., are limited to Length and for concise consideration, the present invention no longer exclusive list.
Preferably, the incoagulable gas after the discharge is collected.
The present invention purifies liquefied gas using device described in first aspect as a preferred technical solution, institute State method are as follows: heated using heat riser in liquefied gas storage device lower part, while to liquefied gas storage device top into Row cooling, then controls gas blow-off system, incoagulable gas is discharged.
Compared with prior art, the present invention is at least had the advantages that
(1) present invention is in liquefied gas before use, the content of incoagulability foreign gas in liquefied gas is reduced by ppm grades To ppb grades, the highly purified of liquefied gas is realized, thereby reduces adverse effect of the foreign gas to subsequent manufacturing procedures.
(2) apparatus of the present invention are simple, easy to operate, have apparent cost advantage for more existing purification process, fit For large-scale promotion.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the liquefied gas purification devices that the embodiment of the present invention 1 provides;
In figure: 1- liquefied gas steel cylinder, 2- cylinder valve, 3- pressure regulator valve, 4- intake valve, 5- vacuum valve, 6- flowmeter, 7- Drain valve, 8- cooler, 9- dry ice, 10- heater, 11- operation panel.
The present invention is described in more detail below.But following examples is only simple example of the invention, not generation Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.
The present invention provides a kind of liquefied gas purification devices in specific embodiment part, and described device includes liquefied gas Body reservoir, cooling device, heat riser and gas blow-off system, the heat riser are set under liquefied gas storage device Portion, the cooling device is at the top of liquefied gas storage device top, the gas blow-off system and liquefied gas storage device Outlet connection, for discharging incoagulable gas.
For the present invention, the liquefied gas storage device can be any liquefied gas storage dress well known in the art It sets, such as steel cylinder etc.;Equally, the heating device may be well known in the art is suitable for above-mentioned liquefied gas storage dress It sets any heating device heated, such as can directly be heated using the heater with temperature control device, it can also be with Indirect heating is carried out using modes such as water-baths, should be specifically chosen according to the material and actual conditions of storage device.
Similar, the cooling device is equally carried out using any cooling device well known in the art, as long as can reach this Invent desired cooling effect, such as can be cooled down using cooling gas, can also using liquid or solid etc. its He cools down mode, and the present invention does not do particular determination to its specific methods for cooling.
Above-mentioned gas exhaust system of the present invention is preferably negative pressure device, so that the incoagulable gas can be smoothly discharged Without bringing new foreign gas into liquefied gas storage device.
In device provided by the invention, the cooling device is set to the outside of liquefied gas storage device, due to foreign gas It is located at the top (higher than the space of liquid level) in reservoir after volatilization, in order to realize more preferably cooling effect, while avoids wasting Energy, the cooling device should be higher than that liquefied gas storage device liquid level.
In device provided by the invention, the heat riser is set to the lower part of liquefied gas storage device, and lower part refers to storing up Liquid level position below in storage, is specifically as follows the surrounding of reservoir, or the bottom of reservoir, for raising energy The considerations of utilization efficiency, preferably will heat up device be located at reservoir bottom or surrounding close to bottom position.
Gas blow-off system of the present invention is preferably connected with gas collector, for the incoagulable gas to discharge into Row is collected.
The present invention additionally provides a kind of liquefied gas purification process, the method are as follows: to liquid in specific embodiment part Change gas reservoir lower part to be heated, while liquefied gas storage device top is cooled down using cooling device, then controls It makes the exhaust apparatus connecting with liquefied gas storage device top exit incoagulable gas is discharged.
Currently preferred heating temperature is 30-50 DEG C, and at the temperature disclosed above, most incoagulability foreign gases obtain Volatilization;Heating temperature, which is crossed, then to cause liquefied gas volatile quantity excessive, increase cooling energy consumption, and pressure is excessive in reservoir, Risk increases;Temperature is too low, and incoagulability foreign gas is difficult to effectively volatilize, and causes purification effect bad.
Currently preferred heating time is 1-3h, and in above-mentioned time range, most incoagulability foreign gases are obtained To volatilization;Heating time is too long to have will increase energy consumption, while reducing working efficiency, is unfavorable for controlling cost;Heating time mistake It is short, still there are a large amount of incoagulability foreign gas dissolutions in a liquid, it is difficult to realize to the highly purified of liquefied gas.
The present invention for the liquefied gas type and without particular determination, as long as liquefied gas commonly used in the art Body is suitable for the present invention, such as the liquefied gas can be arsine, phosphine, ammonia etc., and above-mentioned is to enumerate to it, But it is non-to be only limitted to this.
Similar, the present invention does not do particular determination to the type of the incoagulable gas, can be known in this field Incoagulability foreign gas, such as nitrogen, oxygen, hydrogen, methane or carbon monoxide etc., but non-be only limitted to this.
For the present invention before incoagulable gas is discharged, should first ensure that in discharge pipe does not have other impurities gas, avoids Foreign gas, which enters, causes secondary pollution in liquefied gas.
The present invention should be collected it using collection device after the incoagulable gas is discharged, in case some of them have Poisonous gas spills into air and damages to human body.
Present invention preferably employs above-mentioned liquefied gas purification devices to purify to liquefied gas.
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, of the invention is typical but non-limiting Embodiment is as follows:
Embodiment 1
A kind of liquefied gas purification devices are present embodiments provided, as shown in Figure 1, described device includes liquefied gas storage Device, cooling device, heat riser and gas blow-off system, the heat riser are set to the lower part of liquefied gas storage device, institute Outlet of the cooling device at the top of liquefied gas storage device top, the gas blow-off system and liquefied gas storage device is stated to connect It connects, for discharging incoagulable gas;
Further, the liquefied gas storage device is liquefied gas steel cylinder 1, and cylinder valve 2 is equipped at the top of it;It is described cold But device includes cooler 8 and deposits in dry ice 9 in cooler 8;The heat riser is the heating with temperature control device Device 10;The gas blow-off system includes operation panel 11 and the discharge tube that connect with cylinder valve 2, the operation panel 11 include pressure regulator valve 3, intake valve 4, vacuum valve 5, flowmeter 6 and drain valve 7.
The heater 10 is located at 1 surrounding of liquefied gas steel cylinder close to the position of bottom, and the cooler 8 is located at liquefied gas Position more than 1 liquid level of body steel cylinder, the gas blow-off system are connected with gas collector.
Embodiment 2
The present embodiment provides a kind of liquefied gas purification devices, described device include liquefied gas storage device, cooling device, Heat riser and gas blow-off system, the heat riser are set to the lower part of liquefied gas storage device, and the cooling device is set In liquefied gas storage device top, the gas blow-off system is connect with the outlet at the top of liquefied gas storage device, for discharging Incoagulable gas;
Further, the liquefied gas storage device is liquefied gas steel cylinder, and cylinder valve is equipped at the top of it;The cooling Device includes the recirculated water in cooling line and cooling line, and region of the cooling line more than steel cylinder liquid level is set It sets;The heat riser is water bath device, and the liquefied gas storage device lower submerged is in water (under water bath device liquid level);Institute State the discharge tube that gas blow-off system includes a vacuum pump and connect with cylinder valve.
Embodiment 3
The present embodiment provides a kind of liquefied gas purification process, are carried out using the device in embodiment 1 to liquefied gas pure Change, the described method comprises the following steps:
(1) it opens intake valve 4 and purges helium, to gas blow-off system pressurising, be then shut off and check seal for pipe joints;It opens Pressure regulator valve 3, setting pressure are closed after being less than 3bar (g);Then vacuum valve 5 is opened, is closed after system is taken out negative pressure;
(2) operation 10 times or more of step (1) pressurising/pumping negative pressure are repeated;
(3) heater 10 heat liquefied gas steel cylinder 1 controlled at 40 DEG C, heating time 2h, together Dry ice in Shi Liyong cooler 8 cools down to steel cylinder top;
(4) cylinder valve 2 is opened, while slowly opening vent valves 7, adjusting flowmeter 6 is 2L/min, by incoagulability gas Body drains into collector;
(5) after continued emissions 1min, valve 7 is closed, after waiting 4min, valve 7 is reopened and is discharged, is repeated 5 times More than;
(6) after incoagulable gas discharge to the greatest extent, cylinder valve 2 is closed, heater 10 is simultaneously closed off;
(7) it opens vacuum valve 5 and system is evacuated to vacuum, be then shut off;It opens intake valve 4 and purges helium, be then shut off;
(8) operation 10 times or more of step (7) are repeated;
(9) discharge tube, heater 10 and cooler 8 that gas blow-off system is connect with cylinder valve 2 are removed.
Liquefied gas described in the present embodiment is arsine, and initial purity 99.999%, wherein incoagulable gas impurity contains Amount is 5ppm.After the completion of purifying, the liquefied gas in steel cylinder is subjected to analysis detection, purity 99.9999%, wherein not coagulating Property gaseous impurity content be lower than 50ppb.
Embodiment 4
The present embodiment provides a kind of liquefied gas purification process, are carried out using the device in embodiment 1 to liquefied gas pure Change, the described method comprises the following steps:
(1) it opens the purging helium of intake valve 4 to be then shut off gas blow-off system pressurising, checks seal for pipe joints;It beats Pressure regulator valve 3 is opened, setting pressure is closed after being less than 3bar (g);Then vacuum valve 5 is opened, is closed after system is taken out negative pressure;
(2) step (1) pressurising/pumping negative pressure movement 10 times or more is repeated;
(3) heater 10 heat liquefied gas steel cylinder 1 controlled at 50 DEG C, heating time 1.5h, Cooled down simultaneously using the dry ice in cooler 8 to steel cylinder top;
(4) cylinder valve 2 is opened, while slowly opening vent valves 7, adjusting flowmeter 6 is 3L/min, by incoagulability gas Body drains into collector;
(5) after continued emissions 1min, valve 7 is closed, after waiting 3-5min, valve 7 is reopened and is discharged, repeats 10 More than secondary;
(6) after incoagulable gas discharge to the greatest extent, cylinder valve 2 is closed, heater 10 is simultaneously closed off.
Liquefied gas described in the present embodiment is phosphine, and initial purity 99.995%, wherein incoagulable gas impurity contains Amount is 10ppm.After the completion of purifying, the liquefied gas in steel cylinder is subjected to analysis detection, purity 99.9999%, wherein not Solidifying property gaseous impurity content is lower than 100ppb.
Embodiment 5
The present embodiment provides a kind of liquefied gas purification process, are carried out using the device in embodiment 1 to liquefied gas pure Change, the described method comprises the following steps:
(1) it opens the purging helium of intake valve 4 to be then shut off gas blow-off system pressurising, checks seal for pipe joints;It beats Pressure regulator valve 3 is opened, setting pressure is closed after being less than 3bar (g);Then vacuum valve 5 is opened, is closed after system is taken out negative pressure;
(2) step (1) pressurising/pumping negative pressure movement 10 times or more is repeated;
(3) heater 10 heat liquefied gas steel cylinder 1 controlled at 30 DEG C, heating time 3h, together Dry ice in Shi Liyong cooler 8 cools down to steel cylinder top;
(4) cylinder valve 2 is opened, while slowly opening vent valves 7, adjusting flowmeter 6 is 1L/min, by incoagulability gas Body drains into collector;
(5) after continued emissions 1min, valve 7 is closed, after waiting 3-5min, valve 7 is reopened and is discharged, repeats 8 More than secondary;
(6) after incoagulable gas discharge to the greatest extent, cylinder valve 2 is closed, heater 10 is simultaneously closed off.
Liquefied gas described in the present embodiment is ammonia, and initial purity 99.9995%, wherein incoagulable gas impurity contains Amount is 2ppm.After the completion of purifying, the liquefied gas in steel cylinder is subjected to analysis detection, purity 99.99995%, wherein not Solidifying property gaseous impurity content is lower than 30ppb.
The Applicant declares that the present invention is explained by the above embodiments detailed construction feature of the invention, but the present invention is simultaneously It is not limited to above-mentioned detailed construction feature, that is, does not mean that the present invention must rely on above-mentioned detailed construction feature and could implement.Institute Belong to those skilled in the art it will be clearly understood that any improvement in the present invention, to the equivalence replacement of component selected by the present invention And increase, selection of concrete mode of accessory etc., all of which fall within the scope of protection and disclosure of the present invention.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (10)

1. a kind of liquefied gas purification devices, which is characterized in that described device includes liquefied gas storage device, cooling device, liter Warm device and gas blow-off system, the heat riser are set to the lower part of liquefied gas storage device, and the cooling device is set to Liquefied gas storage device top, the gas blow-off system are connect with the outlet at the top of liquefied gas storage device, for discharging not Solidifying property gas.
2. device as described in claim 1, which is characterized in that the cooling device is set to the outside of liquefied gas storage device.
3. device as claimed in claim 1 or 2, which is characterized in that the cooling device is located at liquefied gas storage device liquid level More than.
4. device as described in any one of claims 1-3, which is characterized in that the gas blow-off system is negative pressure device.
5. device according to any one of claims 1-4, which is characterized in that the gas blow-off system is connected with gas collection Device.
6. device as described in any one in claim 1-5, which is characterized in that the liquefied gas storage device is steel cylinder.
7. a kind of liquefied gas purification process, which is characterized in that the method are as follows: add to liquefied gas storage device lower part Heat, while liquefied gas storage device top is cooled down, then control the row connecting with liquefied gas storage device top exit Incoagulable gas is discharged device of air.
8. the method for claim 7, which is characterized in that the temperature of the heating is 30-50 DEG C;
Preferably, the time of the heating is 1-3h.
9. method as claimed in claim 7 or 8, which is characterized in that the liquefied gas is appointing in arsine, phosphine or ammonia It anticipates one kind;
Preferably, the incoagulable gas is at least one of nitrogen, oxygen, hydrogen, methane or carbon monoxide;
Preferably, the incoagulable gas after the discharge is collected.
10. the method for claim 7, which is characterized in that using device described in any one of claims 1-6 to liquefaction Gas is purified, the method are as follows: is heated using heat riser in liquefied gas storage device lower part, while utilizing cooling Device cools down liquefied gas storage device top, then controls gas blow-off system and incoagulable gas is discharged.
CN201811481825.4A 2018-12-05 2018-12-05 A kind of liquefied gas purification devices and method Pending CN109340578A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113057156A (en) * 2021-03-31 2021-07-02 上海正帆科技股份有限公司 Phosphine gas generating device and method

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CN108579314A (en) * 2018-06-14 2018-09-28 北京万机汇机电工程技术有限公司 A kind of purification devices and method of liquid gas
CN209484283U (en) * 2018-12-05 2019-10-11 上海正帆科技股份有限公司 A kind of liquefied gas purification devices

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Publication number Priority date Publication date Assignee Title
JP2005162546A (en) * 2003-12-03 2005-06-23 Taiyo Nippon Sanso Corp Method and apparatus for refining ammonia
TWI372728B (en) * 2006-02-09 2012-09-21 Mitsubishi Chem Eng Corp
US20130206582A1 (en) * 2012-02-15 2013-08-15 PLAZMATRONIKA NT Sp. zo.o. Method and device for distilling or thickening fluids
CN203678021U (en) * 2013-12-07 2014-07-02 重庆市合川区邓健萍摩托车配件加工厂 Two-stage oil online vacuum purifying equipment
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113057156A (en) * 2021-03-31 2021-07-02 上海正帆科技股份有限公司 Phosphine gas generating device and method

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