CN207299718U - The low-temperature liquefaction purifying plant of special gas - Google Patents

The low-temperature liquefaction purifying plant of special gas Download PDF

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Publication number
CN207299718U
CN207299718U CN201721105676.2U CN201721105676U CN207299718U CN 207299718 U CN207299718 U CN 207299718U CN 201721105676 U CN201721105676 U CN 201721105676U CN 207299718 U CN207299718 U CN 207299718U
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molecular sieve
low
purifying plant
gas
gas cylinder
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CN201721105676.2U
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曹小林
徐建
朱刘
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Kunming Forerunner New Material Technology Co ltd
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Qingyuan Xiandao Materials Co Ltd
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Abstract

It the utility model is related to a kind of low-temperature liquefaction purifying plant of special gas, the purifying plant includes passing sequentially through a stock bottle, a combined column, a collection gas cylinder that gas pipeline is connected, the stock bottle, combined column, collection gas cylinder are connected with vacuum lead respectively, the combined column includes a condensation segment of condensation, the molecular sieve section for being filled with molecular sieve and connection condensation segment and a linkage section of molecular sieve section, and the stock bottle and collection gas cylinder are respectively placed in a cold-trap.The utility model, which devises, is integrated with cryogenic freezing collection, rectifying and the combined column using molecular sieve liquid purification triple functions, greatly improve the efficiency of purification, pass through low-temperature liquefaction at the same time, improve the frequency that impurity is contacted with unit volume molecular sieve, molecular sieve possesses small molecular weight impurity preferable absorption property when being contacted with liquid gas.

Description

The low-temperature liquefaction purifying plant of special gas
Technical field
It the utility model is related to preparation and the purification field of special gas, more particularly to a kind of low-temperature liquefaction of special gas Purifying plant.
Background technology
Field is purified in special gas, and molecular sieve purification technique comparative maturity, purifies out the special gas of 4.5N-5N It is easier, but it is also more difficult that unstrpped gas is processed into the high-purity special gases of 6N, particularly will be miscellaneous in special gas It is very difficult that matter content is reduced to 0.1ppm.
General gas purification process be make gas single flow through molecular sieve section or molecular sieve tower after collect product, due to For container in itself there are dead angle, gas flow rate and the bad control of pressure, time of contact is short, causes the product purity that occurs collecting not high With quality it is uneven the problems such as.
Thus, it is necessary to a kind of low-temperature liquefaction purifying plant of new special gas is designed to solve above-mentioned technical problem.
Utility model content
The purpose of this utility model is to provide a kind of low-temperature liquefaction of special gas easy to operate, product purity is high to carry Pure device.
To realize object defined above, the utility model adopts the following technical solution:A kind of low-temperature liquefaction purification of special gas Device, the purifying plant include passing sequentially through a stock bottle, a combined column, a collection gas cylinder that gas pipeline is connected, the original Material bottle, combined column, collection gas cylinder are connected with vacuum lead respectively, and the combined column includes a condensation segment of condensation, filling A molecular sieve section and connection condensation segment and a linkage section of molecular sieve section for molecular sieve, the stock bottle and collects gas cylinder point It is not placed in a cold-trap.
As further improvement of the utility model, the molecular sieve in the molecular sieve section is 3A, 4A, 5A, 13X molecular sieve One of them or 3A, 4A, 5A, 13X different kinds of molecules sieve the molecular sieve mixed.
As further improvement of the utility model, the collection gas cylinder and stock bottle are low temperature resistant aluminum gas cylinder.
As further improvement of the utility model, the aluminum gas cylinder passes through polishing treatment.
As further improvement of the utility model, the cold-trap is liquid nitrogen cold trap.
The utility model, which devises, to be integrated with cryogenic freezing collection, rectifying and purifies triple functions using molecular sieve liquid Combined column, greatly improves the efficiency of purification, while by low-temperature liquefaction, improves what impurity was contacted with unit volume molecular sieve Frequency, molecular sieve possess small molecular weight impurity preferable absorption property when being contacted with liquid gas.
Brief description of the drawings
Fig. 1 is the overall structure diagram of the embodiment of the low-temperature liquefaction purifying plant of the utility model special gas.
Embodiment
Technical solution is clearly and completely described below in conjunction with the utility model embodiment, it is clear that described Embodiment is only the utility model part of the embodiment, instead of all the embodiments.Based on the implementation in the utility model Example, those of ordinary skill in the art's all other embodiments obtained without making creative work, belongs to The scope of the utility model protection.
Referring to Fig. 1, a kind of low-temperature liquefaction purifying plant 100 of special gas, it includes passing sequentially through gas pipeline 160 A connected stock bottle 110, a combined column 120, one collect gas cylinder 130, and stock bottle 110, combined column 120, collect gas cylinder 130 and divide It is not connected with vacuum lead 140, stock bottle 110 and collection gas cylinder 130 are placed in cold-trap 150.Combined column 120 includes condensation and uses A condensation segment 121, be filled with molecular sieve a molecular sieve section 122 and connection condensation segment and molecular sieve section a linkage section 123。
In the present embodiment, cold-trap 150 is liquid nitrogen cold trap.
Molecular sieve in molecular sieve section 122 has uniform microcellular structure, its hole diameter is uniform, these holes Can be the Molecular Adsorption smaller than its diameter to the inside of vestibule, and there is Preferential adsorption energy to polar molecule and unsaturated molecule Power, thus can polarity degree is different, degree of saturation is different, and the molecule that molecular size is different and boiling point is different separates, i.e., Have the function that " to sieve " molecule.
In the present embodiment, the molecular sieve in molecular sieve section 122 be one of 3A, 4A, 5A, 13X molecular sieve or 3A, The molecular sieve that 4A, 5A, 13X different kinds of molecules sieve mix.
Above-mentioned low temperature purifying plant 100 is used to handle special gas, such as the gas such as arsine, phosphine, germane and hydrogen selenide, Due to use substantial amounts of liquid nitrogen, used collection gas cylinder and stock bottle are low temperature resistant aluminum gas cylinder.In the utility model Some embodiments in, used aluminum gas cylinder passes through polishing treatment, and the aluminum gas cylinder by polishing treatment is conducive to ensure The stability of product.
A kind of low-temperature purification method of special gas, using the low-temperature liquefaction purifying plant of above-mentioned special gas, purification Step is:
S1, will collect gas cylinder and stock bottle and be placed in cold-trap or refrigerating plant, after connecting low temperature purifying plant, take out true It is empty and with the air in the whole low temperature purifying plant of 6N helium replacements;
S2, add liquid nitrogen into cold-trap so that the unstripped gas in stock bottle is sublimated, and removing higher boiling is vacuumized to stock bottle Impurity composition, the unstripped gas are the special gas of impure below 5N;
S3, condensation segment into mixed column add freezing liquid, then unstripped gas are filled with combined column so that unstripped gas Condensation cured on condensation segment inner wall, until the meter in combined column shows that pressure is -0.1 MPa, during which supplements freezing liquid to condensation segment Process is set to continue to carry out;
S4, evacuate once combined column, further removes high-boiling-point impurity component;
S5, the gas for being passed through to condensation segment dry room temperature so that the raw material gas liquefaction of condensation cured, at the same time, liquefaction Unstripped gas liquid condition is maintained between boiling point and solidification point, fall into molecular sieve section so that molecular sieve directly connects with liquefied gas Touch;
Whether the temperature and pressure in S6, observation combined column is under the corresponding boiling point of unstripped gas and freezing point temperature scope Saturated vapor, by adding the gas at normal temperature of freezing liquid or drying, it is liquid to control unstripped gas, and is maintained within 1 hour;
S7, continue to be passed through dry gas at normal temperature into the condensation segment of combined column so that liquid material gas constantly gasifies, compound The meter of column shows that pressure constantly rises, until meter shows that pressure is within 0-0.5 MPa;
S8, open the valve for entering and collecting gas cylinder, and the unstripped gas of gasification, which enters in the collection gas cylinder freezed, to be collected, Until the meter of combined column shows that pressure is begun to decline;
S9, after the meter of combined column shows drop of pressure to 0 MPa, close enter collect gas cylinder valve, to condensation cured Collection gas cylinder evacuate once again remove high-boiling-point impurity component.
In the present embodiment, impurity composition includes H2、O2、H2O、N2、CH4、CO、CO2One or more of which;Freezing liquid is Liquid nitrogen.
The utility model devises a kind of combined column, and epimere is shell and tube condensation segment, and hypomere is point for being filled with molecular sieve Son sieve section, is directly contacted with molecular sieve using liquefied gas, substantially increases impurity molecule and molecular sieve making contact frequency, so that Improve adsorption effect.
Using condensation and the integrated design of molecular sieve purification, can be both precisely controlled by condensation segment combined column pressure and Temperature, while cured raw material is not plugged up during heat-absorbing liquefaction, if condensation segment and molecular sieve section split design It is difficult to allow unstripped gas to maintain liquid condition, the purpose for allowing liquefied gas directly to contact molecular sieve can not reached.
The utility model, which devises, to be integrated with cryogenic freezing collection, rectifying and purifies triple functions using molecular sieve liquid Combined column, greatly improves the efficiency of purification, while by low-temperature liquefaction, improves what impurity was contacted with unit volume molecular sieve Frequency, molecular sieve possess small molecular weight impurity preferable absorption property when being contacted with liquid gas.
Although being example purpose, the preferred embodiment of the utility model, the common skill of this area are had been disclosed for Art personnel will realize the situation of the scope of the utility model and spirit disclosed in not departing from by appended claims Under, various improvements, additions and substitutions are possible.

Claims (5)

  1. A kind of 1. low-temperature liquefaction purifying plant of special gas, it is characterised in that:The purifying plant includes passing sequentially through flue A stock bottle that road is connected, a combined column, one collect gas cylinder, the stock bottle, combined column, collect gas cylinder respectively with vacuum-pumping tube Road is connected, and the combined column includes a condensation segment of condensation, the molecular sieve section for being filled with molecular sieve and connection condensation segment With a linkage section of molecular sieve section, the stock bottle and collection gas cylinder are respectively placed in a cold-trap.
  2. 2. the low-temperature liquefaction purifying plant of special gas according to claim 1, it is characterised in that:
    Molecular sieve in the molecular sieve section is one of 3A, 4A, 5A, 13X molecular sieve or 3A, 4A, 5A, 13X different kinds of molecules Sieve the molecular sieve mixed.
  3. 3. the low-temperature liquefaction purifying plant of special gas according to claim 1, it is characterised in that:
    The collection gas cylinder and stock bottle are low temperature resistant aluminum gas cylinder.
  4. 4. the low-temperature liquefaction purifying plant of special gas according to claim 3, it is characterised in that:
    The aluminum gas cylinder passes through polishing treatment.
  5. 5. the low-temperature liquefaction purifying plant of special gas according to claim 1, it is characterised in that:
    The cold-trap is liquid nitrogen cold trap.
CN201721105676.2U 2017-08-31 2017-08-31 The low-temperature liquefaction purifying plant of special gas Active CN207299718U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112142015A (en) * 2020-09-30 2020-12-29 苏州金宏气体股份有限公司 High-purity hydrogen selenide purification process using carbon nano tube
CN113041641A (en) * 2021-03-07 2021-06-29 无锡恒大电子科技有限公司 Liquefied gas grading and purifying device
CN114593560A (en) * 2022-03-11 2022-06-07 苏州金宏气体股份有限公司 Removal of NO from NO2、N2O purification device and purification method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112142015A (en) * 2020-09-30 2020-12-29 苏州金宏气体股份有限公司 High-purity hydrogen selenide purification process using carbon nano tube
CN113041641A (en) * 2021-03-07 2021-06-29 无锡恒大电子科技有限公司 Liquefied gas grading and purifying device
CN113041641B (en) * 2021-03-07 2022-02-22 无锡恒大电子科技有限公司 Liquefied gas grading and purifying device
CN114593560A (en) * 2022-03-11 2022-06-07 苏州金宏气体股份有限公司 Removal of NO from NO2、N2O purification device and purification method

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Effective date of registration: 20210907

Address after: 511500 Heyun Town Industrial Zone, Qingxin District, Qingyuan City, Guangdong Province (beside Yuba highway)

Patentee after: FIRST RARE MATERIALS Co.,Ltd.

Address before: 511517 27-9B, Guangdong Qingyuan hi tech Industrial Park

Patentee before: FIRST RARE MATERIALS Co.,Ltd.

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Effective date of registration: 20220531

Address after: No. 1116-1, building 1, Dianzhong Business Plaza, Dianzhong new area, Kunming, Yunnan 650212

Patentee after: Kunming forerunner New Material Technology Co.,Ltd.

Address before: 511500 Heyun Town Industrial Zone, Qingxin District, Qingyuan City, Guangdong Province (beside Yuba highway)

Patentee before: FIRST RARE MATERIALS Co.,Ltd.

TR01 Transfer of patent right