CN1704335A - Process for deep dehydration and purification of high purity ammonia - Google Patents
Process for deep dehydration and purification of high purity ammonia Download PDFInfo
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- CN1704335A CN1704335A CN 200410020631 CN200410020631A CN1704335A CN 1704335 A CN1704335 A CN 1704335A CN 200410020631 CN200410020631 CN 200410020631 CN 200410020631 A CN200410020631 A CN 200410020631A CN 1704335 A CN1704335 A CN 1704335A
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- China
- Prior art keywords
- ammonia
- molecular sieve
- raw material
- deep dehydration
- silica gel
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 53
- 230000018044 dehydration Effects 0.000 title claims abstract description 23
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000000746 purification Methods 0.000 title claims abstract description 18
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002808 molecular sieve Substances 0.000 claims abstract description 35
- 238000001179 sorption measurement Methods 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000000741 silica gel Substances 0.000 claims abstract description 15
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- 229910000831 Steel Inorganic materials 0.000 claims description 11
- 239000010959 steel Substances 0.000 claims description 11
- 230000001172 regenerating effect Effects 0.000 claims description 5
- 238000004821 distillation Methods 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 5
- 230000008016 vaporization Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000007872 degassing Methods 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007420 reactivation Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- -1 this Chemical compound 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Separation Of Gases By Adsorption (AREA)
Abstract
Disclosed is a process for high purity ammonia deep dehydration and purification, which comprises passing raw material ammonia through molecular sieves for adsorption dewatering, first passing through silica gel and 13X molecular sieve to adsorb water in raw material ammonia, then passing through 3A molecular sieves for deep dewatering. If the raw material ammonia is vaporized ammonia from the liquid ammonia in the cylinders, then a stimulated single-plate rectification is employed in the evaporation process of the liquid ammonia into steamed ammonia, and ammonia gas can be obtained through a distillation process.
Description
Technical field: high-purity ammon deep dehydration purification process is the production method of the ammonia process molecular sieve adsorbing and dewatering of purifying 99.9999% (6N).
Background technology: gan GaN is the semiconductor epitaxial wafer that is adopted MOCVD (metal organic chemical vapor deposition) prepared by trimethyl-gallium TMGa and ammonia NH3, be used to prepare blue streak photodiode and blue streak laser apparatus, they all are the latest generation semiconductor materials.Employed high-purity ammon requires have very high purity, purity to reach 99.9999% (6N), and it is below the 1PPm that its gaseous impurities CO.CO2.O2.THC (total hydrocarbon) .H2O total amount requires at 1 * 10-6 (volume), wherein H
2O is controlled at below the 0.2PPm, is called " blue ammonia ".
The high-purity ammon of used in electronic industry was not to be used for the GaN preparation in the past, and also so not high to purity requirement, the purity of requirement is 99.999% (5N).Below the water content 5PPm, the adsorption dewatering method of common employing is to adopt 5A molecular sieve or 13X molecular sieve adsorption, and patent DD159259 adopts the ammonia vaporization, uses the 5A molecular sieve adsorption, and water can be reduced to 1PPm.Patent WO9731699 uses getter and 13X molecular sieve dehydration.Patent CNO1124353.8 is that to make ammonia contact a kind of aperture be that the synthetic zeolite of 4～10 dusts prepares high-purity ammon.In fact, the 5A molecular sieve be exactly the aperture be the synthetic zeolite of 4～5 dusts, the 13X molecular sieve be exactly the aperture be the synthetic zeolite of 10 dusts. in the technology of public use, the secondary absorption flow process of using 5A molecular sieve～3A molecular sieve is arranged, the secondary absorption flow process .[1 that use silica gel～5A molecular sieve is also arranged]. index all is the 5N high-purity ammon, and the dehydration degree of depth is to moisture 5～2PPm.
Summary of the invention:
The present invention will solve ammonia purge process deep dehydration difficult technologies problem exactly, and a kind of method of high-purity ammon adsorption deeply dehydration and purification is provided.
High-purity ammon deep dehydration purification process of the present invention, adopt raw material ammonia to it is characterized in that: earlier through the water in silica gel and the 13X molecular sieve adsorption raw material ammonia by molecular sieve adsorbing and dewatering, through 3A molecular sieve deep dehydration, raw material ammonia is passed through silica gel, 13X molecular sieve, three grades of adsorption dewaterings of 3A molecular sieve successively again.For raw material ammonia is from steel cylinder liquefied ammonia bog ammonia, is vaporized into the gaseous ammonia process in ammonia liquor and can carries out the rectifying purifying, and liquefied ammonia is vaporizated into steam ammonia process and adopts analog veneer rectifying, is vaporizated into gaseous ammonia through a rectifying.In order to guarantee to recycle the adsorption dewatering steady quality behind silica gel, 13X molecular sieve, the 3A regenerating molecular sieve, high-purity ammon deep dehydration purification process of the present invention adopts high-purity ammon self blowback cushion steam after being preferably in silica gel, 13X molecular sieve, 3A regenerating molecular sieve and finishing.The present invention adopts the adsorption dewatering of molecular sieve equally, adopt three grades of adsorption process of silica gel one 13X molecular sieve, one 3A molecular sieve, with the 3A molecular sieve as the crucial sorbent material that reaches deep dehydration, and silica gel and 13X molecular sieve are undertaken the task of removing most water content in the ammonia, guaranteed that ammonia purity reaches 6N, water drops to below the 0.4PPm in the ammonia.Table 1 is to be a collection of product detected result data of 3A molecular sieve to the dehydration of ammonia purifying by 3 grades of adsorption process of the invention described above high-purity ammon deep dehydration purification process and 3rd level sorbent material.
Table 1 3A molecular sieve is that a collection of product water content of 3rd level absorption is pursued a bottle detected result
| Sequence number | ????1# | ????2# | ????3# | ????4# | ????5# | ????6# | ????7# |
| Steel cylinder number | ????03740 | ????02321 | ????33511 | ????35367 | ????33363 | ????02379 | ????33455 |
| Filling weight kg | ????26.0 | ????22.0 | ????21.8 | ????21.6 | ????22.0 | ????20.0 | ????22.0 |
| ????H 2O ????PPm | ????0.4 | ????0.4 | ????0.09 | ????0.10 | ????1.0 | 0.1 below | ????0.22 |
The present invention and existing patented technology and public technology difference are: (1) liquefied ammonia adopts analog veneer rectifying control condition when steel cylinder is vaporizated into steam, obtain rectification effect one time; (2) employing contains three grades of absorption of the silica gel one 13X molecular sieve one 3A molecular sieve of 3A molecular sieve; (3) adopt high-purity ammon self blowback cushion steam after silica gel, regenerating molecular sieve are finished.These 3 measures guarantee that fully the 3A molecular sieve is adsorbed onto the ability of 0.2PPm to water, and can guarantee just to reach this ability from beginning.Be described in detail as follows:
1. liquefied ammonia control vaporization veneer rectifying in the steel cylinder
The raw material ammonia that is purified is to be fed to purification devices raw material interface with the form that fills at liquid ammonia steel bottle, and liquefied ammonia carries out purification process with gaseous form after vaporizing in steel cylinder.Consciously this purge process is controlled to be the veneer rectifying, vaporization back ammonia is the ammonia saturation steam, and under the resistance drop and the ambient temperature effect of supporting, there is local vapour-liquid exchange in sub-fraction ammonia in wall and the membranaceous backflow of tube wall.Liquefied ammonia vaporization institute heat requirement is provided by the outer thermal source (hot water) of steel cylinder.Like this, the higher water of boiling point is just stayed liquid phase more, and remaining liquefied ammonia is skimmed.Operation makes the water-content of ammonia in the gas phase reduce 5～10 times than raw material ammonia like this, and raw material ammonia water content 200PPm only is 30～50PPm through the vapour ammoniacal liquor content of handling like this.All do not mentioned this measure of employing in existing patent and the public technology.
2. adopt silica gel-13X molecular sieve-three grades of absorption of 3A molecular sieve
The aperture minimum of 3A molecular sieve in molecular sieve family, 3.0 dusts.Critical diameter 2.7～3.1 dusts of water vapour molecule, the critical diameter of amino molecule is 3.65～3.8 dusts, obviously, the 3A molecular sieve pore passage is to NH
3Molecule enter certain barrier effect, it is all strong than 4A, 5A, 13X molecular sieve to the selective adsorption capacity of water, back molecule sieve aperture road diameter is greater than NH
3And H
2The molecular diameter of O, NH
3, H
2O is intensive absorption at this molecular sieve analog, because NH
3Tying up of adsorption activity surface, reduced 4A, 5A, 13X molecular sieve loading capacity, adopted the flow process of 3A molecular sieve, made the 3A molecular sieve be issued to high adsorption efficiency at low dehydration load as back level absorption to water, these three grades of adsorption process are that 3rd level is done back level absorption with the 3A molecular sieve.
3. adopt high-purity ammon self blowback to sweep displacement and cushion steam behind the adsorbent reactivation
In existing patent and the public technology behind the adsorbent reactivation, all adopt high purity nitrogen (6N) to purge and cushion steam, " saddle-shape " occur on the purification result of high-purity ammon, during the purifying ammonia of Here it is regeneration back, in a loop cycle, early stage and later stage water-content are all higher.The present invention adopts high-purity ammon self blowback to purge, and displacement and air cushion make adsorbent of molecular sieve regeneration fully, and keep high adsorption activity.
Description of drawings: accompanying drawing has been represented a kind of process flow sheet of high-purity ammon deep dehydration purification process of the present invention.Example below in conjunction with accompanying drawing further specifies method of the present invention.
Specific embodiment: this high-purity ammon deep dehydration purification process of the present invention (technical process as shown in Figure 1), raw material ammonia is contained in liquid ammonia steel bottle 1 and inserts production line, through veneer rectifying vaporescence, gaseous ammonia is by valve 13 controls, by under meter 2, enter the purifying adsorption system, enter active carbon adsorber 3 in turn, mainly remove organic gas impurity; Silica gel adsorption device 4,13X molecular sieve adsorber 5, deoxidation adsorber 6,3A molecular sieve adsorber 7.The ammonia of finishing the adsorption and purification process contains particulate matter and non-condensable gases, again by strainer 8 enter degassing tower 9, degassing tower 9 is rectifying tower, be provided with overhead condenser 10 and tower bottom reboiler 11, through filtering and the high-purity ammon of degassing rectifying, at the bottom of tower 9 towers, becoming liquefied ammonia by valve 14 controls, be filled in the product steel cylinder 12, as high-purity ammon supplying products user.Non-condensable gas is discharged by valve 18.Adsorbers at different levels need regeneration after finishing a work period.Each adsorber is provided with electric heater, (19,20,21,22,23).System vacuumizes by valve 17 controls, and reductor regeneration needs N2+H2 gas, uses high-purity ammon behind gac, silica gel, the regenerating molecular sieve, is controlled by valve 15,16.
Table 2 is by the detected result data of the invention described above high-purity ammon deep dehydration purification process to the dehydration of ammonia purifying
Table 2
| Sequence number | ??1# | ??2# | ??3# | ??4# | ??5# | ??6# | ??7# | ??8# | ?9# |
| Steel cylinder number | ??15756 | ??18075 | ??17215 | ??17264 | ??18107 | ??161127 | ??17094 | ??15686 | ?21039 |
| Filling weight kg | ??24.2 | ??21.8 | ??22.0 | ??23.6 | ??23.6 | ??23.2 | ??25.0 | ??22.3 | ?5.0 |
| H 2O PPm | ??0.29 | ??0.22 | ??0.19 | ??0.16 | ??0.14 | ??0.44 | ??0.35 | ??0.15 | ?0.20 |
Qualification rate (H
2O≤0.5PPm) 100%
Quality product rate (H
2O≤0.4PPm) 88.9%
Special quality product rate (H
2O≤0.3PPm) 77.8%
Table 3 be with the 3A molecular sieve in the above-mentioned technology change that the 5A molecular sieve forms into to water absorption back water-content test data in the ammonia
Table 3
| Sequence number | ????1# | ????2# | ????3# |
| ????H 2O?PPm | ????12.0 | ????5.6 | ????5.6 |
Claims (3)
1, a kind of high-purity ammon deep dehydration purification process, adopt raw material ammonia to pass through molecular sieve adsorbing and dewatering, it is characterized in that: earlier through the water in silica gel and the 13X molecular sieve adsorption raw material ammonia, through 3A molecular sieve deep dehydration, raw material ammonia is passed through silica gel, 13X molecular sieve, three grades of adsorption dewaterings of 3A molecular sieve successively again.
2, as the said high-purity ammon deep dehydration of claim 1 purification process, it is characterized in that: raw material ammonia is for from steel cylinder liquefied ammonia bog ammonia the time, and liquefied ammonia is vaporizated into steam ammonia process and adopts analog veneer rectifying control, is vaporizated into gaseous ammonia through a rectifying.
3, as claim 1 or 2 said high-purity ammon deep dehydration purification process, it is characterized in that: adopt high-purity ammon self blowback cushion steam after silica gel, 13X molecular sieve, 3A regenerating molecular sieve are finished.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020631 CN1704335A (en) | 2004-05-28 | 2004-05-28 | Process for deep dehydration and purification of high purity ammonia |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020631 CN1704335A (en) | 2004-05-28 | 2004-05-28 | Process for deep dehydration and purification of high purity ammonia |
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| Publication Number | Publication Date |
|---|---|
| CN1704335A true CN1704335A (en) | 2005-12-07 |
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|---|---|---|---|
| CN 200410020631 Pending CN1704335A (en) | 2004-05-28 | 2004-05-28 | Process for deep dehydration and purification of high purity ammonia |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102109092A (en) * | 2010-12-20 | 2011-06-29 | 上海正帆科技有限公司 | Electric heating conveying device and conveying method for high-purity liquefied gas |
| CN102109091A (en) * | 2010-12-20 | 2011-06-29 | 上海正帆科技有限公司 | Conveying device and conveying method for high-purity liquefied gas |
| JP2012153545A (en) * | 2011-01-21 | 2012-08-16 | Sumitomo Seika Chem Co Ltd | Ammonia purification system and ammonia purification method |
| CN103153861A (en) * | 2011-01-25 | 2013-06-12 | 住友精化株式会社 | Ammonia purification system and method for purifying ammonia |
| TWI500580B (en) * | 2011-03-31 | 2015-09-21 | Sumitomo Seika Chemicals | Ammonia purification system and ammonia purification method |
| CN106310870A (en) * | 2016-11-15 | 2017-01-11 | 苏州金宏气体股份有限公司 | Device for gradually adsorbing and purifying ammonia gas and method for utilizing device to purify ammonia gas |
| CN113028285A (en) * | 2021-03-23 | 2021-06-25 | 兖矿鲁南化工有限公司 | Process and system for blowing off air pipe in filling station |
| CN115430408A (en) * | 2022-09-23 | 2022-12-06 | 全椒科利德电子材料有限公司 | Preparation method and preparation system of high-purity ammonia |
| CN115448325A (en) * | 2022-09-15 | 2022-12-09 | 四川绵竹川润化工有限公司 | Liquid ammonia purification process and system |
| CN119161237A (en) * | 2024-11-04 | 2024-12-20 | 北京鹏同科技有限公司 | A continuous deep dehydration method for anisole for boron isotope separation |
-
2004
- 2004-05-28 CN CN 200410020631 patent/CN1704335A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102109092A (en) * | 2010-12-20 | 2011-06-29 | 上海正帆科技有限公司 | Electric heating conveying device and conveying method for high-purity liquefied gas |
| CN102109091A (en) * | 2010-12-20 | 2011-06-29 | 上海正帆科技有限公司 | Conveying device and conveying method for high-purity liquefied gas |
| JP2012153545A (en) * | 2011-01-21 | 2012-08-16 | Sumitomo Seika Chem Co Ltd | Ammonia purification system and ammonia purification method |
| CN103153861A (en) * | 2011-01-25 | 2013-06-12 | 住友精化株式会社 | Ammonia purification system and method for purifying ammonia |
| CN103153861B (en) * | 2011-01-25 | 2015-04-22 | 住友精化株式会社 | Ammonia purification system and method for purifying ammonia |
| TWI491558B (en) * | 2011-01-25 | 2015-07-11 | Sumitomo Seika Chemicals | Ammonia purification system and ammonia purification method |
| TWI500580B (en) * | 2011-03-31 | 2015-09-21 | Sumitomo Seika Chemicals | Ammonia purification system and ammonia purification method |
| CN106310870A (en) * | 2016-11-15 | 2017-01-11 | 苏州金宏气体股份有限公司 | Device for gradually adsorbing and purifying ammonia gas and method for utilizing device to purify ammonia gas |
| CN113028285A (en) * | 2021-03-23 | 2021-06-25 | 兖矿鲁南化工有限公司 | Process and system for blowing off air pipe in filling station |
| CN113028285B (en) * | 2021-03-23 | 2022-12-16 | 兖矿鲁南化工有限公司 | Process and system for blowing off air pipe in filling station |
| CN115448325A (en) * | 2022-09-15 | 2022-12-09 | 四川绵竹川润化工有限公司 | Liquid ammonia purification process and system |
| CN115430408A (en) * | 2022-09-23 | 2022-12-06 | 全椒科利德电子材料有限公司 | Preparation method and preparation system of high-purity ammonia |
| CN119161237A (en) * | 2024-11-04 | 2024-12-20 | 北京鹏同科技有限公司 | A continuous deep dehydration method for anisole for boron isotope separation |
| CN119161237B (en) * | 2024-11-04 | 2025-08-08 | 北京鹏同科技有限公司 | A continuous deep dehydration method for anisole for boron isotope separation |
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