CN102661654B - 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
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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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 a kind of rectification method and prepare the method and system of high-purity gas.
Background technology
High-purity gas typically refers to the gas that utilizes purification technique to reach certain grade purity, for different gas and application scenario thereof, and the requirement difference of its purity.In general, the purity of high-purity gas is at 3.0N(99.9%) more than, wherein the purity General Requirements of used in electronic industry high-purity gas is more than 5.0N level (99.999%).High-purity gas has been widely used in multiple industrial circles.
High-purity gas is prepared by gas raw material is carried out to degree of depth purifying conventionally.In prior art, for different classes of gas, need be prepared according to this gas the combination that has absorption method, reaction method, rectification method or described several method conventionally adopting from the different distinct methods that adopt of the physicochemical properties of impurities.
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.The method enters weight-removing column by the material liquid of trichlorosilane again and takes off heavily after lightness-removing column takes off gently, thereby obtains high-purity trichlorosilane; Wherein, lightness-removing column and weight-removing column difference using heat pump rectification process independently, after the cooling medium in condenser and tower top end material-heat-exchanging, absorbing heat of vaporization is gas, after the compressed raising pressure and temperature of gas, enter reboiler as tower reactor thermal source still liquid, and itself condense into liquid; Liquid returns condenser after expenditure and pressure, completes a circulation, and the heat at tower top low temperature place is delivered to tower reactor high temperature place by cooling medium thus.The method can effectively be removed light component impurity and the heavy constituent impurity in trichlorosilane, obtains high-purity trichlorosilane products, reduces energy consumption simultaneously, increases economic efficiency.But still there is following problem in this technology:
(1) the de-light system of this technology and de-heavy system all need overhead condenser equipment and corresponding energy, also need separately independently compressor apparatus and corresponding energy, thus equipment and energy consumption still larger;
(2) de-light system and de-heavy system difference using heat pump distillation technology independently, in each system after overcompression tower reactor reboiler and the logistics capacity of tower reactor liquid heat exchange with through the logistics capacity of expenditure and pressure gained, equate completely, so realize system thermal and material balance to parameter that requirement is set is very strict, 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 needs to consume other equipment and energy by its boil down to liquid, could store and use.
Therefore, need a kind of cost rectification method lower and flexible operation to prepare the technology of high-purity gas.
Summary of the invention
The object of the present invention is to provide a kind of cost rectification method lower and flexible operation to prepare the method and system of high-purity gas.
The object of the invention is to be achieved through the following technical solutions:
Rectification method is prepared a method for high-purity gas, comprises the steps:
(1) object gas raw material is passed into lightness-removing column, the gas that described lightness-removing column tower top is discharged is through overhead condenser, and the liquid of condensation is got back to described lightness-removing column as phegma from tower top, and uncooled light component contaminant stream is discharged; The material of described lightness-removing column tower reactor extraction passes into weight-removing column, and from described weight-removing column overhead extraction purifying gas, tower reactor is discharged heavy constituent contaminant stream;
(2) by boil down to Compressed Gas after the cooling medium of described lightness-removing column overhead condenser heat exchange and the merging of the purifying gas of described weight-removing column overhead extraction, described Compressed Gas is at least divided into two parts, Part I is as the thermal source of lightness-removing column tower reactor reboiler, and Part II is as the thermal source of weight-removing column tower reactor reboiler; By the fluid storage forming after described two parts compressed gas condensation;
(3) liquid step (2) being stored is divided into three parts, and Part I is the cooling medium as described lightness-removing column overhead condenser through throttling expansion; Part II is the phegma as described weight-removing column through throttling expansion; Part III is as product extraction.
Preferably, the described Compressed Gas of step (2) also separates Part III, and described Part III Compressed Gas is condensed into liquid, and the liquid forming with described first, second Partial shrinkage condensation of gas merges storage.Described Part III Compressed Gas is adjusting logistics, and owing to regulating the existence of logistics, the flow of described first, second Partial shrinkage gas can regulate according to the actual needs in each stage of System Operation, thereby has greatly improved the flexibility of system operation.
The inventive method is applicable to the gas of all applicable 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, preferred described object gas be below pressure 10Mpa and temperature-50～50 ℃ between time the gas that can liquefy.
Because the purity of object gas raw material is higher, lower to rectifying column equipment requirement, more easy operating, be more conducive to improve rectifying purification efficiency, thereby the purity of preferred described object gas raw material is higher than 90%, more preferably higher than 95%, more preferably higher than 99%.If initial purity does not reach requirement, can adopt pretreatment, comprise that the serial of methods such as condensation, absorption, chemical reaction, first rectifying improve its purity, then apply this method.
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 distillation process, thereby the inventive method is particularly useful for making high-purity gas, particularly prepare the high used in electronic industry high-purity gas of purity requirement.High-purity gas of the present 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 welding Cutting Gases propylene, propane or welding carbon dioxide; 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 described object gas raw material does not have corrosivity.
Preferably, described 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, for removing the light component impurity of object gas raw material;
A lightness-removing column overhead condenser, for by described lightness-removing column tower top Exhaust Gas cooling condensation;
A weight-removing column, for removing the heavy constituent impurity of material of described lightness-removing column tower reactor extraction;
A compressor, for boil down to Compressed Gas after the purifying gas of the cooling medium after the heat exchange of described lightness-removing column overhead condenser and described weight-removing column overhead extraction is merged;
A lightness-removing column tower reactor reboiler, for the heat exchange of Part I and the lightness-removing column tower reactor material of described Compressed Gas;
A weight-removing column tower reactor reboiler, for the heat exchange of Part II and the described weight-removing column tower reactor material of described Compressed Gas;
A wet tank, for storing the Part I of at least described Compressed Gas and the liquid that Part II condensation forms;
First throttle valve, for carrying out throttling expansion by the Part I of described wet tank liquid, as the cooling medium of described lightness-removing column overhead condenser;
The second choke valve, for carrying out throttling expansion by the Part II of described wet tank liquid, as the phegma of described weight-removing column;
Described wet tank is connected with product pipeline, for using the Part III of described wet tank liquid as product extraction.
Preferably, described system also comprises a condenser, and for the Part III of described Compressed Gas is carried out to condensation, gained fluid storage is in described wet tank.
Preferably, described wet tank top is provided with gas equalizing line, for regulating system pressure.
Some object gas has strong corrosion after meeting water, now should select corrosion resistant apparatus.
" heavy constituent impurity " as herein described and " light component impurity " have the known implication of this area.In object gas raw material, the impurity that volatility is greater than object gas is light component impurity, the impurity that volatility the is less than object gas composition impurity of attaching most importance to, and it is intelligible that this is that those skilled in the art hold.
With respect to existing rectification method, prepare the technology of high-purity gas, beneficial effect of the present invention is embodied in:
(1) simple, the energy of equipment is saved: compared with prior art, the present invention only lightness-removing column need to configure overhead condenser, weight-removing column is without overhead condenser, and adopt the condensate liquid of throttling refrigeration gained directly as phegma, not only saved equipment, more improve the utilization ratio of cold, saved the energy loss of indirect heat exchange; In addition, by the reasonable arrangement to logistics pipeline, only need a compressor can meet the distillation operation requirement of whole system, saved number of devices and corresponding energy loss; The present invention requires few, cheap to public work.
(2) flexible operation: different from existing heat pump distillation technology, the gas of the present invention after for compressor compresses, be provided with especially a part as regulating logistics, thereby can to the demand of heat, to the flow of this two parts logistics, regulate respectively according to the tower reactor reboiler of lightness-removing column and weight-removing column, improve the flexibility of system operation; Liquid material through heat exchange condensation enters in same wet tank, according to lightness-removing column and weight-removing column, the required concrete flow of throttling expansion is reallocated to storage pot liquid respectively, such arrangement has greatly improved the flexibility of operation, the adjusting of being more convenient for to system parameters; In addition, product is directly stored in storage tank for liquid condition, and pressure wherein can directly fill according to product and actual operation requirements is determined, conveniently stores, fills and use; The operating pressure of lightness-removing column and weight-removing column can be determined according to the Fen Li requirement of system, thereby be convenient to whole system parameters to be optimized design.
(3) be widely used: the inventive method and system are applicable to the gas of all applicable rectification method edulcoration purifications, are specially adapted to high-purity gas, particularly the preparation to 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: using the material being purified as heat carrier and refrigerating medium not only simplified production, and simplified maintenance and the maintenance of system.For example, when heat exchanger occurs to leak, system can for example, not polluted by external substance (, heat carrier or refrigerating medium), and after equipment is repaired, the short time just can resume production.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that rectification method of the present invention is prepared the preferred embodiment of the system of high-purity gas.
The specific embodiment
Below in conjunction with accompanying drawing, implementation method of the present invention is described further, but therefore the present invention is not subject to any restriction.
As shown in Figure 1, object gas raw material 1 passes into that in lightness-removing column T-101, to carry out rectifying de-light, and the gas of discharging from tower top is through lightness-removing column overhead condenser H-102 heat exchange condensation, and condensate liquid 12 returns in lightness-removing column T-101 from tower top, as phegma, uncooled light component contaminant stream 3 is discharged; The material 2 of the tower reactor extraction of lightness-removing column T-101 is passed into weight-removing column T-201 and carry out the de-weight of rectifying, from the tower reactor of weight-removing column T-201, discharge heavy constituent contaminant stream 5, from overhead extraction, removed the purifying gas 4 of light component impurity and heavy constituent impurity.After purifying gas 4 merges with the cooling medium of lightness-removing column overhead condenser H-102, 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 reactor reboiler H-101 of lightness-removing column T-101, after liquid heat exchange in lightness-removing column T-101 tower reactor, be condensed into liquid; Logistics 7, as the thermal source of the tower reactor reboiler H-201 of weight-removing column T-201, after liquid heat exchange in weight-removing column T-201 tower reactor, is condensed into liquid; Logistics 8 is for regulating logistics, and by condenser, H-202 is condensed into liquid.When logistics 6 and logistics 7 are enough to consume whole described Compressed Gas, as the amount of the logistics 8 that regulates logistics, be zero.The liquid that logistics 6,7 and 8 condensations are formed passes into wet tank G-201, and wet tank G-201 top is provided with gas equalizing line P-201, in order to the pressure in regulating tank.The liquid that enters wet tank G-201 is further divided into three part logistics: logistics 10 after first throttle valve J-101 throttling expansion as the cooling medium of lightness-removing column overhead condenser H-102, after merging with purifying gas 4 after heat exchange through compressor S-201 boil down to Compressed Gas; Logistics 11 enters weight-removing column T-201 from tower top after the second choke valve J-201 throttling expansion, as phegma; Logistics 9 extraction, are product.
The various gases that are applicable to 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 determine according to the actual conditions of gas with various completely.Below by specific embodiment, the present invention is carried out to nonrestrictive explanation.
The preparation of embodiment 1 high-purity ammon
Ammonia exists with the form of liquefied ammonia conventionally.The light component impurity existing in liquefied ammonia comprises hydrogen, nitrogen, oxygen, carbon monoxide, carbon dioxide etc., and heavy constituent impurity generally comprises moisture, heavy hydrocarbon, greasy dirt etc.Traditional liquefied ammonia purification process is to be gas by liquid ammonia vaporization, first by acticarbon, remove the heavy constituent impurity such as moisture wherein and oils, then through rectifying column, remove the light component impurity such as hydrogen, nitrogen, oxygen, carbon monoxide, carbon dioxide, finally by compressor pressurizes, bottle.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 For The Electronic Gases ammonia (99.99999%).
By method and system of the present invention, can remove the light component and the heavy constituent impurity that in liquefied ammonia, exist simultaneously, and can easily make used in electronic industry high-purity ammon product more than 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 reactor 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 reactor reboiler H-201: heat exchange area 7m
2.
2. logistics parameter is in Table 1.
The preparation of embodiment 2 high-purity hydrogen chlorides
In hydrogen chloride gas prepared by conventional method, generally all contain carbon dioxide impurities, and in hydrogen chloride gas carbon dioxide remove a difficult problem that belongs to generally acknowledged in field, there is no at present effective solution.The conventional absorption method for carbon dioxide removal, reaction method and rectification method, be all not suitable for carbon dioxide removal from anhydrous hydrogen chloride.For absorption method, because carbon dioxide molecule volume is larger, be difficult for entering in adsorbent micropore and adsorbed in a large number, not yet find at present effective absorbing carbon dioxide and do not adsorb the adsorbent of hydrogen chloride; And the reaction method of conventional carbon dioxide removal, i.e. CO
2+ 3H
2=CH
4+ 2H
2o, the water that the method generates can be combined into hydrochloric acid with hydrogen chloride gas, catalyst and equipment is caused to heavy corrosion, but also brought new methane impurities into.Conventional rectification method, carbon dioxide and hydrogen chloride can be separated in theory, but the two boiling point difference is little, during rectifying, need very large capacity of returns, and then need very large 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 hydrogen chloride gas, in fact not people does not adopt.
High-purity hydrogen chloride gas is in the market to obtain by the content of carbon dioxide in the raw material of strict control synthesising hydrogen, for raw material chlorine and the hydrogen of synthesising hydrogen, carry out the processing of deeply removing carbon dioxide, the hydrogen chloride gas that then the synthetic carbon dioxide content of reaction conforms with the regulations.It is numerous and diverse that the method is prepared high-purity hydrogen chloride gas step, strict to equipment requirement, and cost is very high, thereby on market, the price of used in electronic industry high-purity hydrogen chloride product (5.0N level) is very expensive.
Apply the method and system of rectification method purified gases of the present invention, can be under energy and the lower condition of devices consume, (for example easily remove carbon dioxide in hydrogen chloride gas and other impurity, oxygen, nitrogen, methane, carbon monoxide etc.), obtain used in electronic industry high-purity hydrogen chloride product more than 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 pass into system of the present invention as raw material, although also can reach the object that reduces energy consumption, obtains used in electronic industry high-purity hydrogen chloride, but whole system need to be used the equipment of acid corrosion-resistant, thereby equipment cost is still higher.Therefore, preferably first carry out processed, the moisture removal of hydrogen chloride gas raw material, to not having corrosive degree, is preferably removed to water content lower than 10 × 10
-6, such as adopting the disclosed method of patent CN101774543A or additive method.Can avoid like this using expensive corrosion resistant apparatus, reduce equipment cost.The hydrogen chloride gas raw material that the present embodiment is used has passed through processed in advance, and equipment is not had to 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 reactor 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 reactor 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
In chlorine, conventionally there is the impurity such as hydrogen, oxygen, nitrogen, carbon monoxide, carbon dioxide.Traditional chlorine purification process mostly adopts absorption method, and because the purifying degree of depth of product depends on ability and the activation degree of adsorbent, so not only there is a selection difficult problem for adsorbent, and purification effect is not good, operates complicatedly, and energy consumption is high, and cost is high.
Apply the method and system of rectification method purified gases of the present invention, can easily remove the impurity in chlorine, obtain the high-purity chlorine product of used in electronic industry more than 5.0N level.Similar with the hydrogen chloride gas of embodiment 2, moisture chlorine also has certain corrosivity, and therefore first the present embodiment does not extremely have corrosive degree by the moisture removal of chlorine feed, re-uses the inventive method and system and carries 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 reactor 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 reactor 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 (8)
1. rectification method is prepared a method for high-purity gas, comprises the steps:
(1) object gas raw material is passed into lightness-removing column, the gas that described lightness-removing column tower top is discharged is through overhead condenser, and the liquid of condensation is got back to described lightness-removing column as phegma from tower top, and uncooled light component contaminant stream is discharged; The material of described lightness-removing column tower reactor extraction passes into weight-removing column, and from described weight-removing column overhead extraction purifying gas, tower reactor is discharged heavy constituent contaminant stream;
(2) by boil down to Compressed Gas after the cooling medium of described lightness-removing column overhead condenser heat exchange and the merging of the purifying gas of described weight-removing column overhead extraction, described Compressed Gas is divided into three parts, Part I is as the thermal source of lightness-removing column tower reactor reboiler, and Part II is as the thermal source of weight-removing column tower reactor reboiler; Part III Compressed Gas is condensed into liquid, and the liquid forming with described first, second Partial shrinkage condensation of gas merges storage;
(3) liquid step (2) being stored is divided into three parts, and Part I is the cooling medium as described lightness-removing column overhead condenser through throttling expansion, and the purifying gas of discharging with described weight-removing column tower top after heat exchange merges; Part II is the phegma as described weight-removing column through throttling expansion; Part III is as product extraction.
2. method according to claim 1, is characterized in that, described object gas be below pressure 10Mpa and temperature-50～50 ℃ between time the gas that can liquefy.
3. method according to claim 2, is characterized in that, the purity of described object gas raw material is higher than 90%.
4. method according to claim 3, is characterized in that, described high-purity gas is used in electronic industry high-purity gas.
5. method according to claim 3, it is characterized in that, described 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 welding Cutting Gases propylene, propane or welding carbon dioxide; Or industrial gasses carbon dioxide, anhydrous hydrogen fluoride, sulfur hexafluoride, isobutene, ethene, propylene, butadiene, iso-butane (HC-600a) or 1-butylene.
6. method according to claim 5, is characterized in that, described object gas raw material does not have corrosivity.
7. method according to claim 6, is characterized in that, described 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.
8. a system that implements the claims method described in 1-7 any one, comprising:
A lightness-removing column, for removing the light component impurity of object gas raw material;
A lightness-removing column overhead condenser, for by described lightness-removing column tower top Exhaust Gas cooling condensation;
A weight-removing column, for removing the heavy constituent impurity of material of described lightness-removing column tower reactor extraction;
A compressor, for boil down to Compressed Gas after the purifying gas of the cooling medium after the heat exchange of described lightness-removing column overhead condenser and described weight-removing column overhead extraction is merged;
A lightness-removing column tower reactor reboiler, for the heat exchange of Part I and the lightness-removing column tower reactor material of described Compressed Gas;
A weight-removing column tower reactor reboiler, for the heat exchange of Part II and the described weight-removing column tower reactor material of described Compressed Gas;
A condenser, for by the Part III condensation of described Compressed Gas;
A wet tank, the liquid forming for storing Part I, Part II and the Part III condensation of described Compressed Gas;
First throttle valve, for carrying out throttling expansion by the Part I of described wet tank liquid, as the cooling medium of described lightness-removing column overhead condenser;
The second choke valve, for carrying out throttling expansion by the Part II of described wet tank liquid, as the phegma of described weight-removing column;
Described wet tank is connected with product pipeline, for using the Part III of described wet tank liquid as product extraction.
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