CN106335884A - Method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide - Google Patents
Method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide Download PDFInfo
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- CN106335884A CN106335884A CN201610153568.6A CN201610153568A CN106335884A CN 106335884 A CN106335884 A CN 106335884A CN 201610153568 A CN201610153568 A CN 201610153568A CN 106335884 A CN106335884 A CN 106335884A
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- laughing gas
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/22—Nitrous oxide (N2O)
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
- Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)
- Gas Separation By Absorption (AREA)
Abstract
A method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide is characterized in that an ionic liquid is introduced to the preparation process of the electronic grade nitrous oxide, and the alkaline ionic liquid is adopted as an absorbent to trap acidic gases in the medical grade nitrous oxide. The method has the advantages of large absorption capacity, high selectivity, no solvent volatilization and no solvent loss.
Description
Technical field
The invention belongs to gas separation technique field is and in particular to a kind of separate, from medical grade laughing gas, the method preparing electronic-grade dental gas.
Background technology
Laughing gas, chemical name is nitrous oxide, is a kind of colourless pleasantly sweet gaseous oxidant, and boiling point is -88.49 DEG C, stable at room temperature, has light anaesthesia effect, and people can be caused to laugh.The main production process of laughing gas has ammonium nitrate thermal decomposition method and the contact oxidation method of ammonia at present, all being easier to prepare purity by above two method is 99%(2n, medical grade) laughing gas, the laughing gas of this purity can be used for human body anesthesia, meet medical requirement, domestic many producers can produce.
High-purity laughing gas refers to that purity reaches 99.999%(5n, electron level) more than laughing gas, the laughing gas of this purity is mainly used in the medium membrane process of semiconductor photoelectric device development and production, is the irreplaceable critical electronic gas directly affecting photoelectric device quality.How the laughing gas of medical grade to be further purified the laughing gas of electron level, be the emphasis that people competitively study.The major impurity of medical grade laughing gas is co2、h2o、n2、o2、no、no2Deng, main removal methods adopting both at home and abroad at present be by adsorb and cryogenic rectification combine by the way of deep removal objectionable impurities (high Gekko Swinhonis, " development of high-purity nitrous oxide ", master thesis, Dalian University of Technology, 2014).Absorption is main to remove co2、h2O, no and no2Impurity, cryogenic rectification mainly removes n2And o2Impurity.Absorption includes physical absorption and two kinds of means of chemisorbed, and physical absorption adopts silica gel and molecular sieve as adsorbing material, and chemisorbed adopts alkali metal oxide, alkaline earth oxide as adsorbing material.Above-mentioned adsorbing material is solid, have the advantages that operation is simple, the rate of departure is fast, rotten to equipment little and energy consumption needed for regeneration little, but the gas absorption capacity of solid adsorption material and selectivity are not ideal enough.
The salt that ionic liquid refers under the room temperature being made up of organic cation and inorganic/organic anion or near room temperature is in a liquid state.Ionic liquid vapour pressure is extremely low, almost do not have volatility, can be reclaimed by way of reducing pressure or heating up, and when being applied to GAS ABSORPTION, can avoid that the solvent loss amount that conventional solvent causes because of volatilization is big, recycle the problems such as difficulty and environmental pollution.Ionic liquid is applied to the separation preparation of high-purity laughing gas by the present invention as absorbent, develops a kind of technique that medical grade laughing gas is purified to electronic-grade dental gas.
Content of the invention
For solving deficiency and the defect that traditional method exists, ionic liquid is incorporated in the preparation process of electronic-grade dental gas the present invention, it is used for trapping sour gas in medical grade laughing gas using alkali ionic liquid as absorbent, have the advantages that absorptive capacity is big, selectivity is high, solvent-free volatilization and losing.
The present invention solves the technical scheme that adopted of above-mentioned technical problem: a kind of separate, from medical grade laughing gas, the method preparing electronic-grade dental gas, first gas compressor that the system that the method is adopted includes setting gradually, spray absorber, drying tower, adsorption tower, second gas compressor, rectifying column；The wherein previous outlet of equipment is connected by pipeline with the import of latter apparatus；The tower top of rectifying column is condenser, and bottom of towe is reboiler；It is characterized in that: described method includes the following step carrying out in order:
1) by first gas compressor, medical grade laughing gas is compressed to the pressure of 0.3 ~ 0.5 mpa, then passes through the import that Pipeline transport is located at bottom sides to spray absorber；
2) in spray absorber, the medical grade laughing gas flowing from bottom to top will be contacted with the ionic liquid in tower, thus getting rid of most co in medical grade laughing gas2、h2o、no、no2, then drying tower is entered by the road by upper outlet；
3) in drying tower, the medical grade laughing gas flowing from bottom to top will be contacted with the silica gel in tower, thus getting rid of the h of residual2O, enters adsorption tower by the road by upper outlet afterwards；
4) in adsorption tower, medical grade laughing gas is when by modified 3a molecular sieve by wherein remaining co2、no、no2Remove, afterwards second gas compressor is entered by the road by upper outlet；
5) second gas compressor enters the import in the middle part of rectifying column after medical grade laughing gas is compressed to the pressure of 1.0 ~ 2.0 mpa, by lower boiling n in this device2、o2, alkane discharge from the outlet of tower top, what bottom of towe outlet was discharged is electronic-grade dental gas；In rectifying column, overhead condenser temperature is -65 ~ -85 DEG C, and tower bottom reboiler temperature is -35 ~ -55 DEG C.
As improvement, the n being 99% containing volume fraction in described medical grade laughing gas2O, remaining volume fraction is that 1% foreign gas includes co2、h2o、no、no2、n2、o2And alkane.
As improvement, described ionic liquid is three hexyl myristyl scute methyllanthionines or three hexyl myristyl squama proline.
As improvement, the tower top temperature of described spray absorber controls at 40 ~ 70 DEG C.
As improvement, described modified 3a molecular sieve is that 3a molecular sieve is invaded in the sodium hydroxide solution or 1 ~ 1.5 mol/l sodium carbonate liquor of 0.3 ~ 0.5 mol/l the molecular sieve that 12 hours post-dryings of bubble obtain.
Compared with prior art, it is an advantage of the current invention that: be used for trapping sour gas in medical grade laughing gas using alkali ionic liquid as absorbent, have that absorptive capacity is big, selectivity is high, a solvent-free volatilization and losing.
Brief description
Fig. 1 is a kind of schematic flow sheet separating the method preparing electronic-grade dental gas from medical grade laughing gas of the present invention.
Wherein: 1- first gas compressor, 2- spray absorber, 3- drying tower, 4- adsorption tower, 5- second gas compressor, 6- rectifying column.
Specific embodiment
Embodiment is described in further detail to the present invention below in conjunction with the accompanying drawings.
Embodiment 1
In conjunction with accompanying drawing 1, a kind of separation from medical grade laughing gas of the inventive method is prepared the method for electronic-grade dental gas and is: will contain n by first gas compressor (1)2O accounts for the pressure that the medical grade laughing gas that volume fraction is 99% is compressed to 0.3 mpa, then passes through the import that Pipeline transport is located at bottom sides to spray absorber (2)；The tower top temperature of spray absorber (2) is arranged on 40 DEG C, and the medical grade laughing gas flowing from bottom to top will be contacted with three hexyl myristyl scute methyllanthionine ionic liquids in tower, thus getting rid of most co in medical grade laughing gas2、h2o、no、no2, then drying tower (3) is entered by the road by upper outlet；In drying tower (3), the medical grade laughing gas flowing from bottom to top will be contacted with the silica gel in tower, thus getting rid of the h of residual2O, enters adsorption tower (4) by the road by upper outlet afterwards；It is filled with modified 3a molecular sieve in adsorption tower (4), this molecular sieve is that the molecular sieve that 12 hours post-dryings of bubble obtain invaded in the sodium hydroxide solution of 0.3 mol/l by 3a molecular sieve, and medical grade laughing gas is when by modified 3a molecular sieve by wherein remaining co2、no、no2Remove, afterwards second gas compressor (5) is entered by the road by upper outlet；Second gas compressor (5) enters the import in the middle part of rectifying column (6) after medical grade laughing gas is compressed to the pressure of 1.0 mpa, in rectifying column (6), overhead condenser temperature is -85 DEG C, tower bottom reboiler temperature is -55 DEG C, by lower boiling n in this device2、o2, alkane discharge from the outlet of tower top, what bottom of towe outlet was discharged is n2O accounts for the electronic-grade dental gas that volume fraction is 99.999%.
Embodiment 2
In conjunction with accompanying drawing 1, a kind of separation from medical grade laughing gas of the inventive method is prepared the method for electronic-grade dental gas and is: will contain n by first gas compressor (1)2O accounts for the pressure that the medical grade laughing gas that volume fraction is 99% is compressed to 0.5 mpa, then passes through the import that Pipeline transport is located at bottom sides to spray absorber (2)；The tower top temperature of spray absorber (2) is arranged on 70 DEG C, and the medical grade laughing gas flowing from bottom to top will be contacted with three hexyl myristyl squama proline ionic liquids in tower, thus getting rid of most co in medical grade laughing gas2、h2o、no、no2, then drying tower (3) is entered by the road by upper outlet；In drying tower (3), the medical grade laughing gas flowing from bottom to top will be contacted with the silica gel in tower, thus getting rid of the h of residual2O, enters adsorption tower (4) by the road by upper outlet afterwards；It is filled with modified 3a molecular sieve in adsorption tower (4), this molecular sieve is that the molecular sieve that 12 hours post-dryings of bubble obtain invaded in the sodium hydroxide solution of 0.5 mol/l by 3a molecular sieve, and medical grade laughing gas is when by modified 3a molecular sieve by wherein remaining co2、no、no2Remove, afterwards second gas compressor (5) is entered by the road by upper outlet；Second gas compressor (5) enters the import in the middle part of rectifying column (6) after medical grade laughing gas is compressed to the pressure of 2.0 mpa, in rectifying column (6), overhead condenser temperature is -65 DEG C, tower bottom reboiler temperature is -35 DEG C, by lower boiling n in this device2、o2, alkane discharge from the outlet of tower top, what bottom of towe outlet was discharged is n2O accounts for the electronic-grade dental gas that volume fraction is 99.999%.
Embodiment 3
In conjunction with accompanying drawing 1, a kind of separation from medical grade laughing gas of the inventive method is prepared the method for electronic-grade dental gas and is: will contain n by first gas compressor (1)2O accounts for the pressure that the medical grade laughing gas that volume fraction is 99% is compressed to 0.4 mpa, then passes through the import that Pipeline transport is located at bottom sides to spray absorber (2)；The tower top temperature of spray absorber (2) is arranged on 60 DEG C, and the medical grade laughing gas flowing from bottom to top will be contacted with three hexyl myristyl scute methyllanthionine ionic liquids in tower, thus getting rid of most co in medical grade laughing gas2、h2o、no、no2, then drying tower (3) is entered by the road by upper outlet；In drying tower (3), the medical grade laughing gas flowing from bottom to top will be contacted with the silica gel in tower, thus getting rid of the h of residual2O, enters adsorption tower (4) by the road by upper outlet afterwards；It is filled with modified 3a molecular sieve in adsorption tower (4), this molecular sieve is that the molecular sieve that 12 hours post-dryings of bubble obtain invaded in 1 mol/l sodium carbonate liquor by 3a molecular sieve, and medical grade laughing gas is when by modified 3a molecular sieve by wherein remaining co2、no、no2Remove, afterwards second gas compressor (5) is entered by the road by upper outlet；Second gas compressor (5) enters the import in the middle part of rectifying column (6) after medical grade laughing gas is compressed to the pressure of 1.5 mpa, in rectifying column (6), overhead condenser temperature is -75 DEG C, tower bottom reboiler temperature is -45 DEG C, by lower boiling n in this device2、o2, alkane discharge from the outlet of tower top, what bottom of towe outlet was discharged is n2O accounts for the electronic-grade dental gas that volume fraction is 99.999%.
Embodiment 4
In conjunction with accompanying drawing 1, a kind of separation from medical grade laughing gas of the inventive method is prepared the method for electronic-grade dental gas and is: will contain n by first gas compressor (1)2O accounts for the pressure that the medical grade laughing gas that volume fraction is 99% is compressed to 0.4 mpa, then passes through the import that Pipeline transport is located at bottom sides to spray absorber (2)；The tower top temperature of spray absorber (2) is arranged on 50 DEG C, and the medical grade laughing gas flowing from bottom to top will be contacted with three hexyl myristyl squama proline ionic liquids in tower, thus getting rid of most co in medical grade laughing gas2、h2o、no、no2, then drying tower (3) is entered by the road by upper outlet；In drying tower (3), the medical grade laughing gas flowing from bottom to top will be contacted with the silica gel in tower, thus getting rid of the h of residual2O, enters adsorption tower (4) by the road by upper outlet afterwards；It is filled with modified 3a molecular sieve in adsorption tower (4), this molecular sieve is that the molecular sieve that 12 hours post-dryings of bubble obtain invaded in 1.5 mol/l sodium carbonate liquors by 3a molecular sieve, and medical grade laughing gas is when by modified 3a molecular sieve by wherein remaining co2、no、no2Remove, afterwards second gas compressor (5) is entered by the road by upper outlet；Second gas compressor (5) enters the import in the middle part of rectifying column (6) after medical grade laughing gas is compressed to the pressure of 1.5 mpa, in rectifying column (6), overhead condenser temperature is -70 DEG C, tower bottom reboiler temperature is -40 DEG C, by lower boiling n in this device2、o2, alkane discharge from the outlet of tower top, what bottom of towe outlet was discharged is n2O accounts for the electronic-grade dental gas that volume fraction is 99.999%.
Claims (5)
1. a kind of separate, from medical grade laughing gas, the method preparing electronic-grade dental gas, first gas compressor that the system that the method is adopted includes setting gradually, spray absorber, drying tower, adsorption tower, second gas compressor, rectifying column；The wherein previous outlet of equipment is connected by pipeline with the import of latter apparatus；The tower top of rectifying column is condenser, and bottom of towe is reboiler；It is characterized in that: described method includes the following step carrying out in order:
1) by first gas compressor, medical grade laughing gas is compressed to the pressure of 0.3 ~ 0.5 mpa, then passes through the import that Pipeline transport is located at bottom sides to spray absorber；
2) in spray absorber, the medical grade laughing gas flowing from bottom to top will be contacted with the ionic liquid in tower, thus getting rid of most co in medical grade laughing gas2、h2o、no、no2, then drying tower is entered by the road by upper outlet；
3) in drying tower, the medical grade laughing gas flowing from bottom to top will be contacted with the silica gel in tower, thus getting rid of the h of residual2O, enters adsorption tower by the road by upper outlet afterwards；
4) in adsorption tower, medical grade laughing gas is when by modified 3a molecular sieve by wherein remaining co2、no、no2Remove, afterwards second gas compressor is entered by the road by upper outlet；
5) second gas compressor enters the import in the middle part of rectifying column after medical grade laughing gas is compressed to the pressure of 1.0 ~ 2.0 mpa, by lower boiling n in this device2、o2, alkane discharge from the outlet of tower top, what bottom of towe outlet was discharged is electronic-grade dental gas；In rectifying column, overhead condenser temperature is -65 ~ -85 DEG C, and tower bottom reboiler temperature is -35 ~ -55 DEG C.
2. method according to claim 1 it is characterised in that: the n being 99% containing volume fraction in described medical grade laughing gas2O, remaining volume fraction is that 1% foreign gas includes co2、h2o、no、no2、n2、o2And alkane.
3. method according to claim 1 it is characterised in that: described ionic liquid be three hexyl myristyl scute methyllanthionines or three hexyl myristyl squama proline.
4. method according to claim 1 it is characterised in that: the tower top temperature of described spray absorber controls at 40 ~ 70 DEG C.
5. method according to claim 1 it is characterised in that: described modified 3a molecular sieve is that 3a molecular sieve is invaded in the sodium hydroxide solution or 1 ~ 1.5 mol/l sodium carbonate liquor of 0.3 ~ 0.5 mol/l the molecular sieve that 12 hours post-dryings of bubble obtain.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610153568.6A CN106335884A (en) | 2016-03-17 | 2016-03-17 | Method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610153568.6A CN106335884A (en) | 2016-03-17 | 2016-03-17 | Method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide |
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| CN106335884A true CN106335884A (en) | 2017-01-18 |
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| CN201610153568.6A Pending CN106335884A (en) | 2016-03-17 | 2016-03-17 | Method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980670A (en) * | 2019-10-28 | 2020-04-10 | 宿州伊维特新材料有限公司 | Rectification method of high-purity nitrous oxide |
Citations (6)
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|---|---|---|---|---|
| JPH06122506A (en) * | 1992-10-14 | 1994-05-06 | Mitsui Toatsu Chem Inc | Method for producing nitrous oxide |
| CN102126968A (en) * | 2011-01-11 | 2011-07-20 | 中国科学院过程工程研究所 | Alkaline ionic liquid as well as preparation and application thereof |
| CN103221377A (en) * | 2010-11-19 | 2013-07-24 | 因温斯特技术公司 | Nitrous oxide-containing ionic liquids as chemical reagents |
| CN104229760A (en) * | 2013-06-18 | 2014-12-24 | 气体产品与化学公司 | Recovery and purification of nitrous oxide |
| CN105110304A (en) * | 2015-09-01 | 2015-12-02 | 上海交通大学 | Device and method for preparing high-purity nitrogen monoxide from adipic acid production tail gases |
| CN105271144A (en) * | 2015-10-10 | 2016-01-27 | 山东金博环保科技有限公司 | Device and method for extraction and refinement of N2O from petrochemical industrial tail gas |
-
2016
- 2016-03-17 CN CN201610153568.6A patent/CN106335884A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06122506A (en) * | 1992-10-14 | 1994-05-06 | Mitsui Toatsu Chem Inc | Method for producing nitrous oxide |
| CN103221377A (en) * | 2010-11-19 | 2013-07-24 | 因温斯特技术公司 | Nitrous oxide-containing ionic liquids as chemical reagents |
| CN102126968A (en) * | 2011-01-11 | 2011-07-20 | 中国科学院过程工程研究所 | Alkaline ionic liquid as well as preparation and application thereof |
| CN104229760A (en) * | 2013-06-18 | 2014-12-24 | 气体产品与化学公司 | Recovery and purification of nitrous oxide |
| CN105110304A (en) * | 2015-09-01 | 2015-12-02 | 上海交通大学 | Device and method for preparing high-purity nitrogen monoxide from adipic acid production tail gases |
| CN105271144A (en) * | 2015-10-10 | 2016-01-27 | 山东金博环保科技有限公司 | Device and method for extraction and refinement of N2O from petrochemical industrial tail gas |
Non-Patent Citations (1)
| Title |
|---|
| 汪志平: "氨基酸离子液体吸收CO2的机理及CO2辅助的反萃取过程", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980670A (en) * | 2019-10-28 | 2020-04-10 | 宿州伊维特新材料有限公司 | Rectification method of high-purity nitrous oxide |
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