CN204079491U - The device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide - Google Patents

The device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide Download PDF

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Publication number
CN204079491U
CN204079491U CN201420416513.6U CN201420416513U CN204079491U CN 204079491 U CN204079491 U CN 204079491U CN 201420416513 U CN201420416513 U CN 201420416513U CN 204079491 U CN204079491 U CN 204079491U
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adsorber
molecular sieve
nitrous oxide
water
deep removal
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高天龙
牛永进
梁肃臣
孙伟
徐永峰
保松
夏山林
孙基成
苗兴
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Zhonghao Guangming Research and Design Institute of Chemical Industry Co Ltd
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Zhonghao Guangming Research and Design Institute of Chemical Industry Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/10Capture or disposal of greenhouse gases of nitrous oxide (N2O)
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/151Reduction of greenhouse gas [GHG] emissions, e.g. CO2

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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

In deep removal Nitrous Oxide, a device for water and carbonic acid gas, belongs to chemical production technical field.This device comprises stock bottle, receiving flask and adsorber, and adsorber is the 13X molecular sieve adsorber, 5A molecular sieve adsorber, modified molecular screen adsorber and the 3A molecular sieve adsorber that connect successively.Stock bottle is heated by the well heater in outside, opens the first pressure reducer when the pressure of unstripped gas reaches 2.0-4.0MPa in bottle, and unstripped gas enters successively as molecular sieve adsorber.When the pressure of gas reaches 2.0-4.0MPa in adsorber, open the second pressure reducer, the collection and confinement of gases after adsorber removing impurity is provided with in freezing plant receiving flask to outside.The method improves adsorption deeply and the rate of adsorption of sorbent material by High Pressure Absorption, and by carrying out chemical modification to molecular sieve, make it the function simultaneously with physical adsorption and chemical reaction, improve the absorption property of sorbent material, realize the deep removal to water, carbon dioxide impurities in Nitrous Oxide, obtain high-purity Nitrous Oxide product.

Description

The device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide
Technical field
The utility model relates to the device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide, and it belongs to chemical production technical field.
Background technology
Nitrous Oxide (N 2o) be commonly called as laughing gas, chemical name is nitrous oxide.In microelectronics, opto-electronic device production process, from the encapsulation growing into last device of chip, almost each step, each link be unable to do without electronic gas, and therefore, electronic gas is called as " grain " and " source " of semiconductor material.The quality of performance of semiconductor device, depends on the quality of electronic gas used to a great extent, and electronic gas purity often improves an order of magnitude, all can greatly promote semiconducter device qualitative leap.Because electronic gas quality decides the development of IC technology, and semiconducter device is widely used in civilian and military industry field, and growth momentum is powerful, and it has influence on many aspects of national economy and national defence.High-purity Nitrous Oxide (N 2o) being mainly used in the deielectric-coating technique of semiconductor photoelectric device development and production, is the irreplaceable critical electronic gas directly affecting photoelectric device quality.Using high-purity Nitrous Oxide as key gas source material, adopt pecvd process low temperature deposition SiO 2film, the formation of its masking film, passive film, device anti-reflective anti-reflection film, N 2o is absolutely necessary key raw material.Along with electronic devices and components manufacturing technology process level improves constantly, its technique requires also more and more higher to raw-material foreign matter content, especially its technique requires more and more stricter to the foreign matter content of sensitivity, as the impurity such as moisture content, carbonic acid gas, and the water impurity of Nitrous Oxide, carbon dioxide content are too high, SiO will be caused 2film hydrogen content is large, and the compactness of film does not reach requirement on devices, and therefore in deep removal Nitrous Oxide, the method for water, carbon dioxide impurities is the gordian technique technique of producing high-purity Nitrous Oxide.
Chinese patent CN1827524A " electronic-grade dental gas purification process ", this patent is by the explained hereafter such as chemical purification and molecular sieve purification electronic-grade dental gas, but this purifying technique operating pressure is 0.3-1.0MPa, belong to low pressure adsorbent, under these processing condition, the absorption property of sorbent material cannot be promoted.And the technical target of the product of this explained hereafter does not mention the index as critical impurities water in electronic-grade Nitrous Oxide, carbon dioxide content is 2PPm, also high level level is in, in product, foreign matter content all has greater difference with existing national standard " For The Electronic Gases Nitrous Oxide " (GB/T 14600-2009) and external similar Horizontal production technical indicator simultaneously, cannot meet the purity requirement of existing used in electronic industry high-purity (electron gas) Nitrous Oxide.
Summary of the invention
For solving the problems of the technologies described above, the utility model provides the device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide, utilize thermostatically heating, adopt conventional molecular sieve and modified molecular screen under elevated pressure conditions, water and carbon dioxide impurities in deep removal Nitrous Oxide.
The technical solution of the utility model is: the device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide, comprise stock bottle and receiving flask, this device also comprises adsorber, and described adsorber is the 13X molecular sieve adsorber, 5A molecular sieve adsorber, modified molecular screen adsorber and the 3A molecular sieve adsorber that are connected successively by gas piping; The outside of described stock bottle is provided with well heater, and the gas piping between stock bottle and 13X molecular sieve adsorber is provided with the first reducing valve; The outside of described receiving flask is provided with freezing plant, and the gas piping between receiving flask and 3A molecular sieve adsorber is provided with the second reducing valve, is connected a vacuum valve at the second reducing valve with in the gas piping branch between receiving flask.
The heat conducting medium of described well heater is water, and the height of well heater is 900-1100 millimeter, and the interior diameter of well heater is 400-600 millimeter.
The medium of described freezing plant is the mixture of alcohol and liquid nitrogen.
The 13X molecular sieve cooled after 4 hours through 500-600 DEG C of high-temperature activation is housed in described 13X molecular sieve adsorber, the 5A molecular sieve cooled after 4 hours through 500-600 DEG C of high-temperature activation is housed in 5A molecular sieve adsorber, the 3A molecular sieve cooled after 4 hours through 500-600 DEG C of high-temperature activation is housed in 3A molecular sieve adsorber, the modified molecular screen through high-temperature activation is housed in modified molecular screen adsorber.
The guiding theory of employing technique scheme is: general sorbent material is increase along with the increase of pressure to the adsorption deeply of purified gases and loading capacity at the same temperature, and rate of adsorption also increases along with pressure and accelerates.Nitrous Oxide purification process becomes gas by liquified gas vaporization, and gas obtains high-purity Nitrous Oxide product through purifying technique.But consume a large amount of vaporization heat during Nitrous Oxide vaporizing liquid, cooling sharply can occur raw material steel cylinder, thus the saturated vapor pressure of Nitrous Oxide in raw material steel cylinder is caused to decrease.Like this, adsorption system pressure also can reduce, affect the adsorption deeply of sorbent material, loading capacity and rate of adsorption for solving the reduction of adsorptive pressure, the utility model is by the mode of heating, increase a constant temperature water bath apparatus, guarantee temperature-stable when the sub-nitrogen steel cylinder of material oxidation is vaporized, and keep constant saturated vapor pressure, keep adsorption unit high pressure conditions absorption work, improve the absorption property of sorbent material, guarantee to realize the deep removal to water, carbon dioxide impurities in Nitrous Oxide, the high-purity Nitrous Oxide product of output.General gas flow dehydration, decarbonation can adopt alkali lye, solid alkali and 3A, 5A, 13 molecular sieves etc., but this method is N 2in O, water impurity drops to " 10 -6" order of magnitude only can not meet actual needs by traditional physical cleaning.Technique scheme, on the basis of physical adsorption, by carrying out chemical modification to traditional molecular sieve, also has the function of chemical reaction, further deep removal N while making it to have physical adsorption function 2water in O, carbon dioxide impurities.The modified molecular screen of concrete enforcement is: the high-efficiency adsorbent being activity with Lithium Oxide 98min, sodium oxide, potassium oxide, active substance is modification 3A, 5A, 13 molecular sieves, make it that there is physical adsorption function, also there is the activity of chemical reaction simultaneously, degree of depth adsorption function, the water in major depth absorption raw material and CO 2, its principle is: MO+H 2o=M (OH) x, MO+CO 2=MCO 3, wherein: M-Li, Na, K, Cs etc.
The beneficial effects of the utility model are: in this deep removal Nitrous Oxide, the device of water and carbonic acid gas comprises stock bottle, receiving flask and adsorber, and adsorber is the 13X molecular sieve adsorber, 5A molecular sieve adsorber, modified molecular screen adsorber and the 3A molecular sieve adsorber that are connected successively by gas piping.Stock bottle is heated by the well heater be arranged on outside it, opens the first pressure reducer when the pressure of unstripped gas reaches 2.0-4.0MPa in bottle, and unstripped gas enters each molecular sieve adsorber successively.When the pressure of gas reaches 2.0-4.0MPa in adsorber, open the second pressure reducer, the collection and confinement of gases after adsorber removal of impurities is provided with in freezing plant receiving flask to outside.The method improves adsorption deeply and the rate of adsorption of sorbent material by High Pressure Absorption, and by carrying out chemical modification to molecular sieve, make it the function simultaneously with physical adsorption and chemical reaction, improve the absorption property of sorbent material, realize the deep removal to water, carbon dioxide impurities in Nitrous Oxide, obtain high-purity Nitrous Oxide product.
Accompanying drawing explanation
Fig. 1 is a kind of structure iron removing the device of impurity in Nitrous Oxide.
In figure, 1, well heater, 2, stock bottle, the 3, first reducing valve, 4,13X molecular sieve adsorber, 5,5A molecular sieve adsorber, 6, modified molecular screen adsorber, 7,3A molecular sieve adsorber, the 8, second reducing valve, 9, receiving flask, 10, freezing plant, 11, gas piping, 12, vacuum valve.
Embodiment
Fig. 1 shows a kind of schematic diagram removing the device of impurity in Nitrous Oxide.In figure, in deep removal Nitrous Oxide, the device of water and carbonic acid gas comprises stock bottle 2, receiving flask 9 and adsorber, and adsorber is the 13X molecular sieve adsorber 4,5A molecular sieve adsorber 5, modified molecular screen adsorber 6 and the 3A molecular sieve adsorber 7 that are connected successively by gas piping 11.The outside of stock bottle 2 is provided with well heater 1, and the heat conducting medium of well heater 1 is water, and the height of well heater 1 is 1000 millimeters, and interior diameter is 500 millimeters.Gas piping 11 between stock bottle 2 and 13X molecular sieve adsorber 4 is provided with the first reducing valve 3.The outside of receiving flask 9 is provided with freezing plant 10, and the medium of freezing plant 10 is mixtures of alcohol and liquid nitrogen.Gas piping 11 between receiving flask 9 and 3A molecular sieve adsorber 7 is provided with the second reducing valve 8, is connected a vacuum valve 12 at the second reducing valve 8 with in the gas piping branch between receiving flask 9.
The 13X molecular sieve cooled after 4 hours through 500-600 DEG C of high-temperature activation is housed in 13X molecular sieve adsorber 4, the 5A molecular sieve cooled after 4 hours through 500-600 DEG C of high-temperature activation is housed in 5A molecular sieve adsorber 5, the 3A molecular sieve cooled after 4 hours through 500-600 DEG C of degree high-temperature activation is housed in 3A molecular sieve adsorber 7, the modified molecular screen through high-temperature activation is housed in modified molecular screen adsorber 6.
embodiment 1
The stock bottle 2 that 25Kg Nitrous Oxide is housed is placed in well heater 1, add hot heater 1 to temperature 25 DEG C, open the first reducing valve 3 when stock bottle 2 pressure reaches 2.0MPa and make unstripped gas enter 13X molecular sieve adsorber (4), 5A molecular sieve adsorber (5), modified molecular screen adsorber (6) and 3A molecular sieve adsorber (7) successively along gas piping (11) to carry out adsorption-edulcoration.Open the second reducing valve 8 when adsorber internal pressure reaches 2.0MPa, control adsorber pressure and be always 2.0MPa, collecting product bottle temperature is-100--140 DEG C, collects 5Kg product.In the Nitrous Oxide product collected, water, carbon dioxide impurities content are respectively H 2o<1PPm, CO 2<1PPm.
embodiment 2
The stock bottle 2 that 25Kg Nitrous Oxide is housed is placed in well heater 1, add hot heater 1 to temperature 25 DEG C, open the first reducing valve 3 when stock bottle 2 pressure reaches 3.0MPa and make unstripped gas enter 13X molecular sieve adsorber (4), 5A molecular sieve adsorber (5), modified molecular screen adsorber (6) and 3A molecular sieve adsorber (7) successively along gas piping (11) to carry out adsorption-edulcoration.Open the second reducing valve 8 when adsorber internal pressure reaches 3.0MPa, control adsorber pressure and be always 3.0MPa, collecting product bottle temperature is-100--140 DEG C, collects 5Kg product.In the Nitrous Oxide product collected, water, carbon dioxide impurities content are respectively H 2o<1PPm, CO 2<1PPm.
embodiment 3
The stock bottle 2 that 25Kg Nitrous Oxide is housed is placed in well heater 1, add hot heater 1 to temperature 25 DEG C, open the first reducing valve 3 when stock bottle 2 pressure reaches 4.0MPa and make unstripped gas enter 13X molecular sieve adsorber (4), 5A molecular sieve adsorber (5), modified molecular screen adsorber (6) and 3A molecular sieve adsorber (7) successively along gas piping (11) to carry out adsorption-edulcoration.Open the second reducing valve 8 when adsorber internal pressure reaches 4.0MPa, control adsorber pressure and be always 4.0MPa, collecting product bottle temperature is-100--140 DEG C, collects 5Kg product.In the Nitrous Oxide product collected, water, carbon dioxide impurities content are respectively H 2o<1PPm, CO 2<1PPm.

Claims (4)

1. the device of water and carbonic acid gas in a deep removal Nitrous Oxide, comprise stock bottle (2) and receiving flask (9), it is characterized in that, this device also comprises adsorber, and described adsorber is the 13X molecular sieve adsorber (4), 5A molecular sieve adsorber (5), modified molecular screen adsorber (6) and the 3A molecular sieve adsorber (7) that are connected successively by gas piping (11); The outside of described stock bottle (2) is provided with well heater (1), and the gas piping (11) between stock bottle (2) and 13X molecular sieve adsorber (4) is provided with the first reducing valve (3); The outside of described receiving flask (9) is provided with freezing plant (10), gas piping (11) between receiving flask (9) and 3A molecular sieve adsorber (7) is provided with the second reducing valve (8), the gas piping branch between the second reducing valve (8) with receiving flask (9) is connected a vacuum valve (12).
2. the device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide according to claim 1, it is characterized in that: the heat conducting medium of described well heater (1) is water, the height of well heater (1) is 900-1100 millimeter, and the interior diameter of well heater (1) is 400-600 millimeter.
3. the device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide according to claim 1, is characterized in that: the medium of described freezing plant (10) is the mixture of alcohol and liquid nitrogen.
4. the device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide according to claim 1, it is characterized in that, in described 13X molecular sieve adsorber (4), the 13X molecular sieve cooled after 4 hours through 500-600 DEG C of high-temperature activation is housed, the 5A molecular sieve cooled after 4 hours through 500-600 DEG C of high-temperature activation is housed in 5A molecular sieve adsorber (5), the 3A molecular sieve cooled after 4 hours through 500-600 DEG C of degree high-temperature activation is housed in 3A molecular sieve adsorber (7), the modified molecular screen through high-temperature activation is housed in modified molecular screen adsorber (6).
CN201420416513.6U 2014-07-28 2014-07-28 The device of water and carbonic acid gas in a kind of deep removal Nitrous Oxide Expired - Lifetime CN204079491U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104140085A (en) * 2014-07-28 2014-11-12 中昊光明化工研究设计院有限公司 Device and method for deep removing water and carbon dioxide in nitrous oxide

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104140085A (en) * 2014-07-28 2014-11-12 中昊光明化工研究设计院有限公司 Device and method for deep removing water and carbon dioxide in nitrous oxide
CN104140085B (en) * 2014-07-28 2016-06-22 中昊光明化工研究设计院有限公司 The apparatus and method of water and carbon dioxide in a kind of deep removal nitrous oxide

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