CN102661654A - Method and system for preparing high purity gas by rectification method - Google Patents
Method and system for preparing high purity gas by rectification method Download PDFInfo
- Publication number
- CN102661654A CN102661654A CN2012101353923A CN201210135392A CN102661654A CN 102661654 A CN102661654 A CN 102661654A CN 2012101353923 A CN2012101353923 A CN 2012101353923A CN 201210135392 A CN201210135392 A CN 201210135392A CN 102661654 A CN102661654 A CN 102661654A
- Authority
- CN
- China
- Prior art keywords
- gas
- removing column
- lightness
- purity
- weight
- Prior art date
- 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.)
- Granted
Links
Images
Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Landscapes
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention relates to a method and a system for preparing high purity gas by a rectification method. According to the method disclosed by the invention, a target gas raw material is firstly processed by a light component removal tower to remove light component impurities and then is processed by a heavy component removal tower to remove heavy component impurities; obtained purified gas is compressed into compressed gas; the compressed gas is at least divided into two parts which are respectively used as heat sources of a tower kettle reboiler of the light component removal tower and a tower kettle reboiler of the heavy component removal tower; the two parts of compressed gas are condensated into liquid to be converged and stored; the stored liquid is divided into three parts; two parts of the stored liquid are respectively used as a cooling medium of a tower top condenser of the light component removal tower and reflux of the heavy component removal tower after being respectively subjected to throttling expansion; and the third part of the stored liquid is recovered as a product. The system disclosed by the invention comprises the light component removal tower, the tower top condenser of the light component removal tower, the heavy component removal tower, a compressor, the tower kettle reboiler of the light component removal tower, the tower kettle reboiler of the heavy component removal tower, a liquid storage tank and a connecting pipeline. The method and the system which are disclosed by the invention have the advantages that equipment is simple; energy is saved; the method and the system are flexible to operate and have wide application; the system is easy to maintain; and the method and the system have few requirements on public works.
Description
Technical field
The present invention relates to the method and system that a kind of rectification method prepares high-purity gas.
Background technology
High-purity gas typically refers to the gas that utilizes purification technique to reach certain grade purity, and for different gas and application scenario thereof, the requirement of its purity is different.In general, the purity of high-purity gas is more than 3.0N (promptly 99.9%), and wherein the purity of used in electronic industry high-purity gas is general requires more than 5.0N level (promptly 99.999%).High-purity gas has been widely used in a plurality of industrial circles.
High-purity gas prepares through gas raw material is carried out degree of depth purifying usually.In the prior art,, need to prepare the combination of adopting usually that absorption method, reaction method, rectification method or said several method are arranged according to the different distinct methods that adopt of this gas with the physicochemical properties of impurities for different classes of gas.
Wherein, prepare the technology of high-purity gas for rectification method, patent application CN200910228635.6 discloses the apparatus and method that a kind of heat pump distillation method is produced high-purity trichlorosilane.This method is taken off the material liquid of trichlorosilane and is got into weight-removing column again after light and take off heavily through lightness-removing column, thereby obtains high-purity trichlorosilane; Wherein, Lightness-removing column and weight-removing column difference be the using heat pump rectification process independently, and promptly absorbing heat of vaporization after cooling medium in the condenser and the heat exchange of cat head end material is gas, and gas is after compression improves pressure and temperature; Get into reboiler as tower still thermal source still liquid, and itself condense into liquid; Liquid returns condenser behind expenditure and pressure, accomplish a circulation, and the heat at cat head low temperature place is delivered to tower still high temperature place through cooling medium thus.This method can effectively be removed light component impurity and the heavy ends impurity in the trichlorosilane, obtains high-purity trichlorosilane product, cuts down the consumption of energy simultaneously, increases economic efficiency.Yet still there is following problem in this technology:
(1) this technology is taken off light system and is taken off heavy system and all need overhead condenser equipment and corresponding energy, also needs independent compressed machine equipment and corresponding energy separately, thereby equipment and energy consumption are still bigger;
(2) take off light system and take off heavy system difference using heat pump distillation technology independently; After overcompression, equate fully with logistics capacity in each system through the expenditure and pressure gained at tower still reboiler and the logistics capacity of tower bottoms body heat exchange; So it is very strict to realize that system thermal and material balance require being provided with of parameter; The operating pressure of system, Flow-rate adjustment very flexible, system regulates limited;
(3) when environment temperature is higher, what this technology obtained is high-purity trichlorosilane gas, therefore still need consume other equipment and energy with its boil down to liquid, could store and use.
Therefore, need lower and rectification method flexible operation of a kind of cost to prepare the technology of high-purity gas.
Summary of the invention
The object of the present invention is to provide lower and rectification method flexible operation of a kind of cost to prepare the method and system of high-purity gas.
The objective of the invention is to realize through following technical scheme:
A kind of rectification method prepares the method for high-purity gas, comprises the steps:
(1) the object gas raw material is fed lightness-removing column, the gas that said lightness-removing column cat head is discharged is through overhead condenser, and the liquid of condensation is got back to said lightness-removing column as phegma from cat head, and uncooled light component contaminant stream is discharged; The material of said lightness-removing column tower still extraction feeds weight-removing column, and from said weight-removing column cat head extraction purifying gas, the tower still is discharged the heavy ends contaminant stream;
(2) will pass through the cooling medium of said lightness-removing column overhead condenser heat exchange and the purifying gas of said weight-removing column cat head extraction and merge back boil down to Compressed Gas; Said Compressed Gas is divided into two parts at least; First is as the thermal source of lightness-removing column tower still reboiler, and second portion is as the thermal source of weight-removing column tower still reboiler; With the fluid storage that forms after the condensation of said two parts Compressed Gas;
(3) liquid that step (2) is stored is divided into three parts, and first is through the cooling medium of throttling expansion as said lightness-removing column overhead condenser; Second portion is through the phegma of throttling expansion as said weight-removing column; Third part is as the product extraction.
Preferably, the said Compressed Gas of step (2) is also told third part, and said third part Compressed Gas is condensed into liquid, and the liquid that forms with said first, second part Compressed Gas condensation merges storage.Said third part Compressed Gas is the adjusting logistics, owing to regulate the existence of logistics, said first, second part compressed gas flow can be regulated according to the actual needs in each stage of System Operation, thereby has improved the flexibility of system's operation greatly.
The inventive method is applicable to the gas of all suitable rectification method edulcoration purifications.In order to make the inventive method be applicable to conventional compressor and contractive condition, thus more practical in actual production, the gas that preferred said object gas can liquefy for time below pressure 10Mpa and between the temperature-50～50 ℃.
Because the purity of object gas raw material is high more, and is low more to the rectifying column equipment requirements, easy operating helps improving the rectifying purification efficiency more more, thereby the purity of preferred said object gas raw material is higher than 90%, more preferably is higher than 95%, more preferably is higher than 99%.If initial purity does not reach requirement, can adopt preliminary treatment, comprise that serial of methods such as condensation, absorption, chemical reaction, first rectifying improve its purity, use this method again.
Because rectificating method of the present invention is dark to the degree of purification of gas; Can easily obtain highly purified object gas; And effectively reduce equipment and energy consumption in the distillation process; Thereby the inventive method is particularly useful for making high-purity gas, particularly prepares the high used in electronic industry high-purity gas of purity requirement.High-purity gas according to the invention includes but not limited to used in electronic industry ammonia, chlorine, hydrogen chloride, trichlorosilane, dichloro-dihydro silicon, silicon tetrachloride, hydrogen fluoride, boron trifluoride, hydrogen phosphide, nitrous oxide, sulfur hexafluoride, boron chloride, sulfur hexafluoride, boron chloride, phosphine, silane (SiH
4) or carbon dioxide; Or the welding cutting is used carbon dioxide with combustion gas propylene, propane or welding; Or industrial gasses carbon dioxide, anhydrous hydrogen fluoride, sulfur hexafluoride, isobutene, ethene, propylene, butadiene, iso-butane (HC-600a) or 1-butylene.
For fear of using expensive corrosion resistant apparatus, preferred said object gas raw material does not have corrosivity.
Preferably, said high-purity gas is used in electronic industry hydrogen chloride, the high-purity chlorine of used in electronic industry or used in electronic industry high-purity ammon.
The present invention also provides a kind of rectification method to prepare the system of high-purity gas, comprising:
A lightness-removing column is used for removing the light component impurity of object gas raw material;
A lightness-removing column overhead condenser is used for said lightness-removing column cat head is discharged the gas cooled condensation;
A weight-removing column is used for removing the heavy ends impurity of the material of said lightness-removing column tower still extraction;
A compressor is used for the purifying gas through cooling medium after the heat exchange of said lightness-removing column overhead condenser and the extraction of said weight-removing column cat head is merged back boil down to Compressed Gas;
A lightness-removing column tower still reboiler is used for the first of said Compressed Gas and the heat exchange of lightness-removing column tower still material;
A weight-removing column tower still reboiler is used for the heat exchange of the second portion and the said weight-removing column tower still material of said Compressed Gas;
A wet tank is used to store the first of said at least Compressed Gas and the liquid that the second portion condensation forms;
The first throttle valve is used for the first of said wet tank liquid is carried out throttling expansion, as the cooling medium of said lightness-removing column overhead condenser;
Second choke valve is used for the second portion of said wet tank liquid is carried out throttling expansion, as the phegma of said weight-removing column;
Said wet tank is connected with the product pipeline, is used for third part with said wet tank liquid as the product extraction.
Preferably, said system also comprises a condenser, is used for the third part of said Compressed Gas is carried out condensation, and the gained fluid storage is in said wet tank.
Preferably, said wet tank top is provided with gas equalizing line, is used for regulating system pressure.
Some object gas has strong corrosion property after meeting water, and should select corrosion resistant apparatus this moment.
" heavy ends impurity " as herein described and " light component impurity " have the known implication of this area.In the object gas raw material, volatility is a light component impurity greater than the impurity of object gas, and volatility is a heavy ends impurity less than the impurity of object gas, and this is that those skilled in the art understand easily.
Prepare the technology of high-purity gas with respect to existing rectification method, beneficial effect of the present invention is embodied in:
(1) simple, the energy-efficient of equipment: compared with prior art; The present invention only lightness-removing column need dispose overhead condenser; Weight-removing column then need not overhead condenser, and the condensate liquid that adopts the throttling refrigeration gained has not only been saved equipment directly as phegma; More improve the utilization ratio of cold, saved the energy loss of indirect heat exchange; In addition,, only need a compressor can satisfy the distillation operation requirement of whole system, saved number of devices and corresponding energy loss through reasonable arrangement to the logistics pipeline; The present invention requires few, cheap to public work.
(2) flexible operation: different with existing heat pump distillation technology; The gas of the present invention after for compressor compresses; Be provided with a part especially as regulating logistics; Thereby can regulate respectively the flow of this two parts logistics the demand of heat according to the tower still reboiler of lightness-removing column and weight-removing column, improve the flexibility of system's operation; Liquid material through the heat exchange condensation gets in the same wet tank; According to lightness-removing column and weight-removing column the required concrete flow of throttling expansion is reallocated to liquid in the storage tank respectively; Such arrangement has greatly improved the flexibility of operation, is more convenient for to the adjusting of each parameter of system; In addition, product directly is stored in the storage tank for liquid condition, and pressure wherein can directly fill according to product and actual instructions for use is confirmed, conveniently stores, fills and use; The operating pressure of lightness-removing column and weight-removing column can be confirmed according to the requirement that system separates, thereby be convenient to each parameter of whole system is optimized design.
(3) be widely used: the inventive method and system are applicable to the gas of all suitable rectification method edulcoration purifications, are specially adapted to high-purity gas, particularly to the preparation of the high used in electronic industry high-purity gas of purity requirement.The present invention can easily prepare 5.0N level and more highly purified gas.
(4) for ease of maintenaince: the material that will be purified has not only been simplified production as heat carrier and refrigerating medium, and has simplified the maintenance and the maintenance of system.For example, when heat exchanger took place to leak, system can not polluted by external substance (for example, heat carrier or refrigerating medium), and after equipment was repaired, the short time just can resume production.
Description of drawings
Fig. 1 prepares the sketch map of preferred implementation of the system of high-purity gas for rectification method of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing implementation method of the present invention is further specified, but therefore the present invention does not receive any restriction.
As shown in Figure 1; Object gas raw material 1 feeds and carries out rectifying in the lightness-removing column T-101 and take off gently, and through lightness-removing column overhead condenser H-102 heat exchange condensation, condensate liquid 12 returns in the lightness-removing column T-101 from cat head from the gas of cat head discharge; As phegma, uncooled light component contaminant stream 3 is discharged; The material 2 of the tower still extraction of lightness-removing column T-101 is fed weight-removing column T-201 carry out rectifying and take off heavily, discharge heavy ends contaminant stream 5, removed the purifying gas 4 of light component impurity and heavy ends impurity from the cat head extraction from the tower still of weight-removing column T-201.After the cooling medium of purifying gas 4 and lightness-removing column overhead condenser H-102 merges; By compressor S-201 boil down to Compressed Gas; This Compressed Gas is divided into three part logistics: logistics 6 is as the thermal source of the tower still reboiler H-101 of lightness-removing column T-101; Behind liquid heat exchange in the lightness-removing column T-101 tower still, be condensed into liquid; Logistics 7 behind liquid heat exchange in the weight-removing column T-201 tower still, is condensed into liquid as the thermal source of the tower still reboiler H-201 of weight-removing column T-201; Logistics 8 is for regulating logistics, and H-202 is condensed into liquid by condenser.When logistics 6 and logistics 7 are enough to consume whole said Compressed Gas, be zero as the amount of the logistics 8 of regulating logistics.The liquid of logistics 6,7 and 8 condensations formation is fed wet tank G-201, and wet tank G-201 top is provided with gas equalizing line P-201, in order to the pressure in the regulating tank.The liquid that gets into wet tank G-201 is further divided into three part logistics: logistics 10 as the cooling medium of lightness-removing column overhead condenser H-102, merges after compressor S-201 boil down to Compressed Gas with purifying gas 4 after the heat exchange after first throttle valve J-101 throttling expansion; Logistics 11 gets into weight-removing column T-201 from cat head after the second choke valve J-201 throttling expansion, as phegma; Logistics 9 extraction are product.
The all gases that is fit to the rectification method purifying all can carry out purifying according to above flow process.As for the concrete device parameter and the logistics parameter that adopt, those skilled in the art can confirm according to the actual conditions of gas with various fully.Through specific embodiment the present invention is carried out nonrestrictive explanation below.
The preparation of embodiment 1 high-purity ammon
Ammonia exists with the form of liquefied ammonia usually.The light component impurity that exists in the liquefied ammonia comprises hydrogen, nitrogen, oxygen, carbon monoxide, carbon dioxide etc., and heavy ends impurity generally comprises moisture, heavy hydrocarbon, greasy dirt etc.Traditional liquefied ammonia purification process is that liquefied ammonia is vaporizated into gas; At first remove heavy ends impurity such as wherein moisture and oils through acticarbon; Remove light component impurity such as hydrogen, nitrogen, oxygen, carbon monoxide, carbon dioxide then through rectifying column, after the compressor pressurizes bottling.This method operation is complicated, and the energy consumption of rectification method purifying is very high, and is difficult to reach the purity of the desired 7.0N level of used in electronic industry gaseous ammonia (99.99999%).
Through method and system of the present invention, can remove the light component and the heavy ends impurity that exist in the liquefied ammonia simultaneously, and can easily make the above used in electronic industry high-purity ammon product of purity 7.0N level.
1. device parameter:
Lightness-removing column T-101: diameter phi 0.3m, effective depth 7m;
Weight-removing column T-201: diameter phi 0.4m, effective depth 5m;
Lightness-removing column tower still reboiler H-101: heat exchange area 2.5m
2
Lightness-removing column overhead condenser H-102: heat exchange area 1m
2
Weight-removing column tower still reboiler H-201: heat exchange area 7m
2
2. logistics parameter is seen table 1.
The preparation of embodiment 2 high-purity hydrogen chloride
Generally all contain carbon dioxide impurities in the hydrogen chloride gas of conventional method preparation, and removing of carbon dioxide belongs to a difficult problem of generally acknowledging in the field in the hydrogen chloride gas, still do not have effective solution at present.The conventional absorption method that is used to remove carbon dioxide, reaction method and rectification method all are not suitable for from anhydrous hydrogen chloride, removing carbon dioxide.For absorption method, because the carbon dioxide molecule volume is bigger, be difficult for getting in the adsorbent micropore by a large amount of absorption, find effective absorbing carbon dioxide at present as yet and do not adsorb the adsorbent of hydrogen chloride; And the conventional reaction method that removes carbon dioxide, i.e. CO
2+ 3H
2=CH
4+ 2H
2O, the water that this method generates can be combined into hydrochloric acid with hydrogen chloride gas, catalyst and equipment is caused heavy corrosion, but also brought new methane impurities into.Conventional rectification method; Can carbon dioxide and hydrogen chloride be separated in theory, but the two boiling point difference is little, needs very large capacity of returns during rectifying; And then need the very big refrigerating capacity and the amount of boiling again; Huge equipment and energy consumption will cause be difficult to bear expensive, although thereby in theory rectification method can remove the carbon dioxide in the hydrogen chloride gas, in fact not the people does not adopt.
High-purity hydrogen chloride gas in the market is that the content through carbon dioxide in the raw material of strictness control synthesising hydrogen obtains; Promptly raw material chlorine and the hydrogen for synthesising hydrogen carries out the processing of deeply removing carbon dioxide, then the synthetic carbon dioxide content hydrogen chloride gas up to specification of reaction.It is numerous and diverse that this method prepares high-purity hydrogen chloride gas step, and strict to equipment requirements, cost is very high, thereby the price of the high-purity hydrogen chloride product of used in electronic industry (5.0N level) is very expensive on the market.
Use the method and system of rectification method purified gases of the present invention; Can be under the lower condition of energy and devices consume; Easily remove in the hydrogen chloride gas carbon dioxide and other impurity (for example; Oxygen, nitrogen, methane, carbon monoxide etc.), obtain the above high-purity hydrogen chloride product of used in electronic industry of 5.0N level.
It should be noted that; Because moisture hydrogen chloride has severe corrosive; If directly use the hydrogen chloride gas that contains water to feed system of the present invention as raw material; Though also can reach the purpose that cuts down the consumption of energy, obtains the high-purity hydrogen chloride of used in electronic industry, whole system need be used the equipment of acid corrosion-resistant, thereby equipment cost is still higher.Therefore, preferably at first carry out processed, the moisture removal of hydrogen chloride gas raw material to not having corrosive degree, preferably is removed to water content and is lower than 10 * 10
-6, such as adopting patent CN101774543A disclosed method or additive method.Can avoid the use of expensive corrosion resistant apparatus like this, reduce equipment cost.The hydrogen chloride gas raw material that present embodiment uses has passed through processed in advance, and equipment is not had corrosivity.
1. device parameter:
Lightness-removing column T-101: diameter phi 0.2m, effective depth 14m;
Weight-removing column T-201: diameter phi 0.2m, effective depth 5m;
Lightness-removing column tower still reboiler H-101: heat exchange area 0.5m
2
Lightness-removing column overhead condenser H-102: heat exchange area 0.7m
2
Weight-removing column tower still reboiler H-201: heat exchange area 0.9m
2
2. logistics parameter is asked for an interview table 2.
The preparation of embodiment 3 high-purity chlorine
Usually there are impurity such as hydrogen, oxygen, nitrogen, carbon monoxide, carbon dioxide in the chlorine.Traditional chlorine purification process mostly adopts absorption method, because the purifying degree of depth of product depends on the ability and the activation degree of adsorbent, so not only there is the selection difficult problem of adsorbent, and purification effect is not good, operate complicatedly, and energy consumption is high, the cost height.
Use the method and system of rectification method purified gases of the present invention, can easily remove the impurity in the chlorine, obtain the above high-purity chlorine product of used in electronic industry of 5.0N level.Similar with the hydrogen chloride gas of embodiment 2, moisture chlorine also has certain corrosivity, thus present embodiment at first with the moisture removal of chlorine feed to not having corrosive degree, re-use the inventive method and system and carry out purifying.
1. device parameter:
Lightness-removing column T-101: diameter phi 0.2m, effective depth 7m;
Weight-removing column T-201: diameter phi 0.2m, effective depth 5m;
Lightness-removing column tower still reboiler H-101: heat exchange area 0.5m
2
Lightness-removing column overhead condenser H-102: heat exchange area 0.7m
2
Weight-removing column tower still reboiler H-201: heat exchange area 0.9m
2
2. logistics parameter is asked for an interview table 3.
Table 1
Table 2
Table 3
Claims (10)
1. a rectification method prepares the method for high-purity gas, comprises the steps:
(1) the object gas raw material is fed lightness-removing column, the gas that said lightness-removing column cat head is discharged is through overhead condenser, and the liquid of condensation is got back to said lightness-removing column as phegma from cat head, and uncooled light component contaminant stream is discharged; The material of said lightness-removing column tower still extraction feeds weight-removing column, and from said weight-removing column cat head extraction purifying gas, the tower still is discharged the heavy ends contaminant stream;
(2) will pass through the cooling medium of said lightness-removing column overhead condenser heat exchange and the purifying gas of said weight-removing column cat head extraction and merge back boil down to Compressed Gas; Said Compressed Gas is divided into two parts at least; First is as the thermal source of lightness-removing column tower still reboiler, and second portion is as the thermal source of weight-removing column tower still reboiler; With the fluid storage that forms after the condensation of said two parts Compressed Gas;
(3) liquid that step (2) is stored is divided into three parts, and first is through the cooling medium of throttling expansion as said lightness-removing column overhead condenser; Second portion is through the phegma of throttling expansion as said weight-removing column; Third part is as the product extraction.
2. method according to claim 1 is characterized in that, the said Compressed Gas of step (2) is also told third part, and said third part Compressed Gas is condensed into liquid, and the liquid that forms with said first, second part Compressed Gas condensation merges storage.
3. method according to claim 1 and 2 is characterized in that, the gas that said object gas can liquefy for time below pressure 10Mpa and between the temperature-50～50 ℃.
4. method according to claim 3 is characterized in that the purity of said object gas raw material is higher than 90%, is preferably to be higher than 95%, more preferably is higher than 99%.
5. method according to claim 4 is characterized in that, said high-purity gas is the used in electronic industry high-purity gas.
6. method according to claim 4; It is characterized in that said high-purity gas is used in electronic industry ammonia, chlorine, hydrogen chloride, trichlorosilane, dichloro-dihydro silicon, silicon tetrachloride, hydrogen fluoride, boron trifluoride, hydrogen phosphide, nitrous oxide, sulfur hexafluoride, boron chloride, sulfur hexafluoride, boron chloride, phosphine, silane (SiH
4) or carbon dioxide; Or the welding cutting is used carbon dioxide with combustion gas propylene, propane or welding; Or industrial gasses carbon dioxide, anhydrous hydrogen fluoride, sulfur hexafluoride, isobutene, ethene, propylene, butadiene, iso-butane (HC-600a) or 1-butylene.
7. method according to claim 6 is characterized in that, said object gas raw material does not have corrosivity.
8. method according to claim 7 is characterized in that, said high-purity gas is used in electronic industry hydrogen chloride, the high-purity chlorine of used in electronic industry or used in electronic industry high-purity ammon.
9. system that implements each said method of claim 1-8 comprises:
A lightness-removing column is used for removing the light component impurity of object gas raw material;
A lightness-removing column overhead condenser is used for said lightness-removing column cat head is discharged the gas cooled condensation;
A weight-removing column is used for removing the heavy ends impurity of the material of said lightness-removing column tower still extraction;
A compressor is used for the purifying gas through cooling medium after the heat exchange of said lightness-removing column overhead condenser and the extraction of said weight-removing column cat head is merged back boil down to Compressed Gas;
A lightness-removing column tower still reboiler is used for the first of said Compressed Gas and the heat exchange of lightness-removing column tower still material;
A weight-removing column tower still reboiler is used for the heat exchange of the second portion and the said weight-removing column tower still material of said Compressed Gas;
A wet tank is used to store the first of said at least Compressed Gas and the liquid that the second portion condensation forms;
The first throttle valve is used for the first of said wet tank liquid is carried out throttling expansion, as the cooling medium of said lightness-removing column overhead condenser;
Second choke valve is used for the second portion of said wet tank liquid is carried out throttling expansion, as the phegma of said weight-removing column;
Said wet tank is connected with the product pipeline, is used for third part with said wet tank liquid as the product extraction.
10. system according to claim 9 is characterized in that, said system also comprises a condenser, is used for the third part of said Compressed Gas is carried out condensation, and the gained fluid storage is in said wet tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210135392.3A CN102661654B (en) | 2012-05-02 | 2012-05-02 | Method and system for preparing high purity gas by rectification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210135392.3A CN102661654B (en) | 2012-05-02 | 2012-05-02 | Method and system for preparing high purity gas by rectification method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102661654A true CN102661654A (en) | 2012-09-12 |
| CN102661654B CN102661654B (en) | 2014-04-30 |
Family
ID=46771189
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210135392.3A Active CN102661654B (en) | 2012-05-02 | 2012-05-02 | Method and system for preparing high purity gas by rectification method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102661654B (en) |
Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043612A (en) * | 2013-02-02 | 2013-04-17 | 瓮福（集团）有限责任公司 | Method for rectifying high-purity anhydrous hydrogen fluoride |
| 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 |
| CN105502295A (en) * | 2015-12-31 | 2016-04-20 | 上海正帆科技股份有限公司 | Electronic grade hydrogen chloride purification method |
| CN104926581B (en) * | 2014-03-21 | 2017-02-15 | 青岛科技大学 | Process flow for dry separation of propylene and hydrogen chloride |
| CN106904617A (en) * | 2017-04-06 | 2017-06-30 | 洛阳中硅高科技有限公司 | A kind of device for preparing dichlororosilane eiectronic grade |
| CN107715491A (en) * | 2017-11-21 | 2018-02-23 | 滨化集团股份有限公司 | A kind of chlorine refines process units |
| CN107746040A (en) * | 2017-10-17 | 2018-03-02 | 山东新龙科技股份有限公司 | A kind of Processes and apparatus that hydrogen chloride is refined using the by-product gas for producing trichloro ethylene |
| CN108313983A (en) * | 2018-05-03 | 2018-07-24 | 繁昌县凯艺电子商务有限公司 | The hydrofluoric acid purifying prepared for high purity lithium fluoride and preparation method |
| CN109019631A (en) * | 2018-08-24 | 2018-12-18 | 苏州金宏气体股份有限公司 | A kind of production system and production method of ultra-pure ammonia |
| CN109084527A (en) * | 2018-09-20 | 2018-12-25 | 中科瑞奥能源科技股份有限公司 | Laughing gas rectification and purification device and laughing gas rectificating method |
| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
| CN110065951A (en) * | 2019-03-20 | 2019-07-30 | 河南心连心深冷能源股份有限公司 | A kind of device producing high-purity boron chloride and its production method |
| CN110508105A (en) * | 2019-08-28 | 2019-11-29 | 山东康宝生化科技有限公司 | A kind of apparatus and method separating carbon dioxide and hydrogen chloride in Sucralose tail gas |
| CN110562924A (en) * | 2019-09-12 | 2019-12-13 | 天津中科拓新科技有限公司 | Preparation method of electronic grade hydrogen bromide |
| CN110668456A (en) * | 2019-11-19 | 2020-01-10 | 安徽艾佩科电子材料有限公司 | Purification method and device of high-purity boron tribromide |
| CN110902655A (en) * | 2018-09-18 | 2020-03-24 | 中昊晨光化工研究院有限公司 | Method and device for treating waste catalyst in difluoroethane production |
| CN111056540A (en) * | 2019-12-25 | 2020-04-24 | 中船重工（邯郸）派瑞特种气体有限公司 | Electrolytic NF3Continuous pre-purification device and continuous pre-purification method |
| CN111675220A (en) * | 2020-05-08 | 2020-09-18 | 江西江氨科技有限公司 | CO is contained in tail gas generated in carbonate production2Extraction and refining system |
| CN113072419A (en) * | 2021-03-27 | 2021-07-06 | 上海化工研究院有限公司 | Hexafluorobutadiene purification method with high recovery rate |
| CN113247862A (en) * | 2021-06-18 | 2021-08-13 | 湖北和远气体股份有限公司 | High-purity electronic-grade hydrogen chloride production device and process |
| CN114275743A (en) * | 2021-12-10 | 2022-04-05 | 湖北兴福电子材料有限公司 | Method for producing high-purity liquid sulfur trioxide for electronic-grade sulfuric acid |
| CN114506859A (en) * | 2022-02-18 | 2022-05-17 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation method of high-purity deuterated ammonia |
| CN114602201A (en) * | 2022-01-17 | 2022-06-10 | 福建久策气体股份有限公司 | Carbonyl sulfide purification device and purification method thereof |
| CN114712877A (en) * | 2022-04-15 | 2022-07-08 | 南京佳华工程技术有限公司 | Method and equipment for preparing electronic grade gas by adopting thermal coupling technology |
| CN115490236A (en) * | 2022-09-20 | 2022-12-20 | 云南通威高纯晶硅有限公司 | Preparation method and system of trichlorosilane for electronic grade polycrystalline silicon production |
| WO2023138089A1 (en) * | 2022-01-24 | 2023-07-27 | 广州市华达石化有限公司 | Liquid ammonia double-working-condition refrigerating system and liquid carbon dioxide production equipment |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0060357A1 (en) * | 1981-03-18 | 1982-09-22 | Conoco Phillips Company | Heat pump fractionation process |
| JPS57176919A (en) * | 1981-04-24 | 1982-10-30 | Takara Shuzo Co Ltd | Preparation of anhydrous ethanol |
| CN1417182A (en) * | 2002-12-10 | 2003-05-14 | 西安交通大学 | Heat pump azeotropic rectification process and equipment for fuel ethanol |
| CN101357890A (en) * | 2008-09-17 | 2009-02-04 | 西安交通大学 | Methyl carbonate synthesis and refining technique using heat pump technique and apparatus thereof |
| CN101704524A (en) * | 2009-11-20 | 2010-05-12 | 天津大学 | Production device and method of high purity trichlorosilane by using heat pump distillation |
| CN101712592A (en) * | 2009-11-25 | 2010-05-26 | 南京大学 | Process for producing absolute ethanol through low-grade heat source |
-
2012
- 2012-05-02 CN CN201210135392.3A patent/CN102661654B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0060357A1 (en) * | 1981-03-18 | 1982-09-22 | Conoco Phillips Company | Heat pump fractionation process |
| JPS57176919A (en) * | 1981-04-24 | 1982-10-30 | Takara Shuzo Co Ltd | Preparation of anhydrous ethanol |
| CN1417182A (en) * | 2002-12-10 | 2003-05-14 | 西安交通大学 | Heat pump azeotropic rectification process and equipment for fuel ethanol |
| CN101357890A (en) * | 2008-09-17 | 2009-02-04 | 西安交通大学 | Methyl carbonate synthesis and refining technique using heat pump technique and apparatus thereof |
| CN101704524A (en) * | 2009-11-20 | 2010-05-12 | 天津大学 | Production device and method of high purity trichlorosilane by using heat pump distillation |
| CN101712592A (en) * | 2009-11-25 | 2010-05-26 | 南京大学 | Process for producing absolute ethanol through low-grade heat source |
Cited By (34)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043612A (en) * | 2013-02-02 | 2013-04-17 | 瓮福（集团）有限责任公司 | Method for rectifying high-purity anhydrous hydrogen fluoride |
| CN104926581B (en) * | 2014-03-21 | 2017-02-15 | 青岛科技大学 | Process flow for dry separation of propylene and hydrogen chloride |
| 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 |
| CN105502295A (en) * | 2015-12-31 | 2016-04-20 | 上海正帆科技股份有限公司 | Electronic grade hydrogen chloride purification method |
| CN106904617A (en) * | 2017-04-06 | 2017-06-30 | 洛阳中硅高科技有限公司 | A kind of device for preparing dichlororosilane eiectronic grade |
| CN106904617B (en) * | 2017-04-06 | 2020-07-21 | 洛阳中硅高科技有限公司 | Device for preparing electronic-grade dichlorosilane |
| CN107746040A (en) * | 2017-10-17 | 2018-03-02 | 山东新龙科技股份有限公司 | A kind of Processes and apparatus that hydrogen chloride is refined using the by-product gas for producing trichloro ethylene |
| CN107746040B (en) * | 2017-10-17 | 2021-04-13 | 山东新龙科技股份有限公司 | Process and equipment for refining hydrogen chloride by using byproduct gas from production of trichloroethylene |
| CN107715491A (en) * | 2017-11-21 | 2018-02-23 | 滨化集团股份有限公司 | A kind of chlorine refines process units |
| CN108313983A (en) * | 2018-05-03 | 2018-07-24 | 繁昌县凯艺电子商务有限公司 | The hydrofluoric acid purifying prepared for high purity lithium fluoride and preparation method |
| CN109019631A (en) * | 2018-08-24 | 2018-12-18 | 苏州金宏气体股份有限公司 | A kind of production system and production method of ultra-pure ammonia |
| CN110902655A (en) * | 2018-09-18 | 2020-03-24 | 中昊晨光化工研究院有限公司 | Method and device for treating waste catalyst in difluoroethane production |
| CN109084527B (en) * | 2018-09-20 | 2024-06-11 | 中科瑞奥能源科技股份有限公司 | Laughing gas rectifying and purifying device and laughing gas rectifying method |
| CN109084527A (en) * | 2018-09-20 | 2018-12-25 | 中科瑞奥能源科技股份有限公司 | Laughing gas rectification and purification device and laughing gas rectificating method |
| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
| CN110065951A (en) * | 2019-03-20 | 2019-07-30 | 河南心连心深冷能源股份有限公司 | A kind of device producing high-purity boron chloride and its production method |
| CN110065951B (en) * | 2019-03-20 | 2023-05-12 | 河南心连心深冷能源股份有限公司 | Device and method for producing high-purity boron trichloride |
| CN110508105A (en) * | 2019-08-28 | 2019-11-29 | 山东康宝生化科技有限公司 | A kind of apparatus and method separating carbon dioxide and hydrogen chloride in Sucralose tail gas |
| CN110508105B (en) * | 2019-08-28 | 2021-08-10 | 山东康宝生化科技有限公司 | Device and method for separating carbon dioxide and hydrogen chloride from sucralose tail gas |
| CN110562924A (en) * | 2019-09-12 | 2019-12-13 | 天津中科拓新科技有限公司 | Preparation method of electronic grade hydrogen bromide |
| CN110668456A (en) * | 2019-11-19 | 2020-01-10 | 安徽艾佩科电子材料有限公司 | Purification method and device of high-purity boron tribromide |
| CN111056540A (en) * | 2019-12-25 | 2020-04-24 | 中船重工（邯郸）派瑞特种气体有限公司 | Electrolytic NF3Continuous pre-purification device and continuous pre-purification method |
| CN111056540B (en) * | 2019-12-25 | 2023-09-15 | 中船(邯郸)派瑞特种气体股份有限公司 | Electrolytic NF 3 Continuous prepurification device and continuous prepurification method |
| CN111675220A (en) * | 2020-05-08 | 2020-09-18 | 江西江氨科技有限公司 | CO is contained in tail gas generated in carbonate production2Extraction and refining system |
| CN113072419B (en) * | 2021-03-27 | 2022-12-09 | 上海化工研究院有限公司 | Hexafluorobutadiene purification method with high recovery rate |
| CN113072419A (en) * | 2021-03-27 | 2021-07-06 | 上海化工研究院有限公司 | Hexafluorobutadiene purification method with high recovery rate |
| CN113247862A (en) * | 2021-06-18 | 2021-08-13 | 湖北和远气体股份有限公司 | High-purity electronic-grade hydrogen chloride production device and process |
| CN114275743A (en) * | 2021-12-10 | 2022-04-05 | 湖北兴福电子材料有限公司 | Method for producing high-purity liquid sulfur trioxide for electronic-grade sulfuric acid |
| CN114602201A (en) * | 2022-01-17 | 2022-06-10 | 福建久策气体股份有限公司 | Carbonyl sulfide purification device and purification method thereof |
| WO2023138089A1 (en) * | 2022-01-24 | 2023-07-27 | 广州市华达石化有限公司 | Liquid ammonia double-working-condition refrigerating system and liquid carbon dioxide production equipment |
| CN114506859A (en) * | 2022-02-18 | 2022-05-17 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation method of high-purity deuterated ammonia |
| CN114712877A (en) * | 2022-04-15 | 2022-07-08 | 南京佳华工程技术有限公司 | Method and equipment for preparing electronic grade gas by adopting thermal coupling technology |
| CN115490236A (en) * | 2022-09-20 | 2022-12-20 | 云南通威高纯晶硅有限公司 | Preparation method and system of trichlorosilane for electronic grade polycrystalline silicon production |
| CN115490236B (en) * | 2022-09-20 | 2024-03-29 | 云南通威高纯晶硅有限公司 | Preparation method of trichlorosilane for producing electronic grade polysilicon |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102661654B (en) | 2014-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102661654A (en) | Method and system for preparing high purity gas by rectification method | |
| US5335504A (en) | Carbon dioxide recovery process | |
| CN101922850B (en) | Method for utilizing coalbed methane containing oxygen to prepare liquefied natural gas | |
| CN104406364B (en) | The argon of a kind of double tower coupling reclaims purifier apparatus and argon reclaims purification process | |
| JP4624343B2 (en) | Removal of liquid natural gas from gaseous natural gas streams | |
| CN101929788B (en) | Device for preparing liquefied natural gas by oxygen-bearing coal mine methane | |
| KR20000005637A (en) | Method and apparatus for producing carbon dioxide | |
| CN109833638A (en) | A kind of rectification method prepares the method and system of high-purity gas | |
| CN104263443A (en) | Method and system for separating nitrogen from liquefied natural gas | |
| US9513050B2 (en) | Apparatus and method for the distillation separation of a mixture containing carbon dioxide | |
| CN105731379A (en) | Purifying method of electronic grade chlorine | |
| CN202522015U (en) | Neon and helium separation and purification device with refrigeration equipment | |
| CN107648976B (en) | Method for preparing ultra-high-purity gas through low-temperature separation and low-temperature separation system | |
| US6321566B1 (en) | Method for producing oxygen gas | |
| CN103773529B (en) | Pry-mounted associated gas liquefaction system | |
| CN107352510B (en) | Polycrystalline silicon reduction exhaust recovery method and recovery system | |
| CN101634515B (en) | Method for extracting high-yield pure krypton and pure xenon by full distillation | |
| CN204373313U (en) | A kind of argon gas of double tower coupling reclaims purifier apparatus | |
| CN204111708U (en) | A kind of system of separation of nitrogen from natural gas liquids | |
| JP4814587B2 (en) | Method for separating C2 + fraction from light gas containing NOx | |
| CN110255501A (en) | A kind of electronic grade high-purity hydrogen chloride preparation method | |
| CN106978226B (en) | Process and system for separating heavy hydrocarbon in natural gas by cryogenic method | |
| JP4814588B2 (en) | Method for separating C2 + fraction from light gas containing NOx | |
| CN208166954U (en) | A kind of process unit of nitrogenous natural gas double tower deep cooling denitrogenation | |
| CN102589250A (en) | Process of separating and preparing nitrogen by using air |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |