CN102435045A - Liquid nitrogen washing purified synthetic gas and device for cryogenically separating and recovering LNG (liquefied natural gas) thereof - Google Patents
Liquid nitrogen washing purified synthetic gas and device for cryogenically separating and recovering LNG (liquefied natural gas) thereof Download PDFInfo
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- CN102435045A CN102435045A CN2011104173858A CN201110417385A CN102435045A CN 102435045 A CN102435045 A CN 102435045A CN 2011104173858 A CN2011104173858 A CN 2011104173858A CN 201110417385 A CN201110417385 A CN 201110417385A CN 102435045 A CN102435045 A CN 102435045A
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- liquid nitrogen
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000007789 gas Substances 0.000 title claims abstract description 61
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 47
- 239000007788 liquid Substances 0.000 title claims abstract description 27
- 238000005406 washing Methods 0.000 title abstract description 10
- 239000003949 liquefied natural gas Substances 0.000 title description 14
- 238000000926 separation method Methods 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 12
- 238000007781 pre-processing Methods 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 21
- 238000003786 synthesis reaction Methods 0.000 claims description 21
- 230000002194 synthesizing Effects 0.000 claims description 21
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 230000008929 regeneration Effects 0.000 claims description 12
- 238000011069 regeneration method Methods 0.000 claims description 12
- 210000000038 chest Anatomy 0.000 claims description 10
- 238000005201 scrubbing Methods 0.000 claims description 10
- 239000002808 molecular sieve Substances 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000003507 refrigerant Substances 0.000 abstract description 2
- 238000005057 refrigeration Methods 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 239000002737 fuel gas Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000003337 fertilizer Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 241000282326 Felis catus Species 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- DVARTQFDIMZBAA-UHFFFAOYSA-O Ammonium nitrate Chemical compound [NH4+].[O-][N+]([O-])=O DVARTQFDIMZBAA-UHFFFAOYSA-O 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003139 buffering Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QDHHCQZDFGDHMP-UHFFFAOYSA-N monochloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 1
- 150000002829 nitrogen Chemical class 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 230000002035 prolonged Effects 0.000 description 1
Abstract
The invention belongs to the technical field of low temperature cryogenic separation and purification and discloses a liquid nitrogen washing purified synthetic gas and a device for cryogenically separating and recovering LNG thereof, comprising a raw material gas pre-processing system, a purifying cryogenic separating cool box and a mixing refrigerant refrigeration cycle system, wherein raw material gas in a cool box system is washed by a nitrogen washing tower to obtain the qualified synthetic gas; the synthetic gas is returned, recycled, cooled and output from a device; high purified LNG liquid is obtained at the bottom of a rectifying tower; and the LNG liquid is served as product and transmitted to a storage system after being cool-throttled. The separation system substitutes former two independent systems of a liquid nitrogen purification system and an LNG single liquefied system, simultaneously achieves to the aims of purifying the synthetic gas and recovering LNG, reduces one-time equipment investment and operation cost, and greatly prolongs the operation period. The liquid nitrogen washing purified synthetic gas and the device have stable operation and outstanding advantage for large-scale device.
Description
Technical field
The invention belongs to low-temperature deep isolation of purified technical field, related in particular to a kind of scrubbing with liquid nitrogen and purified synthesis gas and cryogenic separation recovery LNG device thereof.
Background technology
Ammonia is one of important inorganic chemical product, in national economy, occupies critical role.Except that liquefied ammonia directly the as fertilizer sources, the nitrogenous fertilizer that uses on the agricultural, for example urea, ammonium nitrate, ammonium phosphate, ammonium chloride and the various nitrogen composite fertilizer that contains all are raw material with ammonia.Synthetic ammonia is one of large chemical products, and the annual synthetic ammonia output in the world has reached more than 100,000,000 tons, wherein has 80% ammonia to be used for producing chemical fertilizer, 20% raw material as other chemical products approximately.
The purification of synthetic ammonia is used diverse ways according to the different mining of overall craft, and present flow process mostly adopts liquid nitrogen washing, and the gas that backflows after conventional liquid nitrogen washing will be washed goes out device as fuel gas, goes fuel gas system, and wherein the component change is bigger, and calorific value can't guarantee.Along with day being becoming tight of the energy, the methane benefit that reclaims in the fuel gas is obvious, and adopt again of device obtains liquefied natural gas with the fuel gas cryogenic separation of liquefying more at present.
Scrubbing with liquid nitrogen of the present invention purifies the system of synthesis gas and cryogenic separation recovery LNG thereof; When the liquid nitrogen washing purification obtains qualified synthesis gas, reclaim and obtain qualified liquefied natural gas, adopt same set of device; Reduce cost greatly; Synthesis gas goes out CO≤2PPM in the device, and the purity of liquefied natural gas is 99%, the rate of recovery " 95%.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of cost, and the ice chest apparatus arrangement is simple, and energy consumption is low, and heat exchanger efficiency is high, stable operation, and the scrubbing with liquid nitrogen that has prolonged the cycle of operation greatly purifies synthesis gas and cryogenic separation recovery LNG device thereof.
In order to solve the problems of the technologies described above, the present invention is able to solve through following technical proposals:
Scrubbing with liquid nitrogen purifies synthesis gas and the LNG device is reclaimed in cryogenic separation; Comprise that feed gas preprocessing system, cryogenic purification separate ice chest, azeotrope cooling cycle system; The feed gas preprocessing system comprises regeneration gas heaters, molecular sieve adsorber, regeneration gas cooler; Regeneration gas heaters, molecular sieve adsorber and regeneration gas cooler link to each other through pipeline successively; Said cryogenic purification separates ice chest and comprises main heat exchanger, knockout drum, nitrogen wash column, methane rectifying column and be arranged on the tower bottom reboiler in the methane rectifying column; Said main heat exchanger, knockout drum, nitrogen wash column, methane rectifying column connect through pipeline successively; Methane rectifying column top is connected into main heat exchanger through pipeline; Said azeotrope cooling cycle system comprises cryogen compensator, cryogen compressor, compressor one-level knockout drum, compressor secondary knockout drum, three grades of knockout drums of compressor and cooler, and said molecular sieve adsorber is connected through pipeline with main heat exchanger, and three grades of knockout drums of said compressor are connected through pipeline with main heat exchanger.
As preferably; Described cooler comprises compressor one-level cooler, compressor secondary coolers, three grades of coolers of compressor; The cryogen compressor comprises first order cryogen compressor, second level cryogen compressor, third level cryogen compressor, and said cryogen compensator, first order cryogen compressor, compressor one-level cooler, compressor one-level knockout drum, second level cryogen compressor, compressor secondary coolers, compressor secondary knockout drum, third level cryogen compressor, three grades of knockout drums of compressor connect through pipeline successively.
As preferably, be connected with cryogenic fluid pump on the described compressor secondary coolers.
As preferably, described tower bottom reboiler adopts thermal siphon formula evaporimeter.
The present invention has significant technique effect owing to adopted above technical scheme:
Adopt this nitrogen washing to purify the system that LNG is reclaimed in synthesis gas and cryogenic separation thereof, obtain clean synthesis gas at the nitrogen wash column top, synthesis gas goes out system after reclaiming cold and matching well nitrogen according to correct chemistry.Simultaneously with at the bottom of the nitrogen wash column tower with the separator tower at the bottom of the CH4 logistics that is rich in send into rectifying column, at the bottom of rectifying column, obtain highly purified liquefied natural gas, the rectifying column tower bottom reboiler adopts thermal siphon formula evaporimeter; Improved separating effect; Reduced ice chest apparatus arrangement difficulty, provided convenience for the device of big specification, thermal siphon formula evaporimeter is placed on heat exchanger the outside of rectifying column; Cut down the consumption of energy; Improve heat exchanger efficiency, also reduced ice chest apparatus arrangement difficulty simultaneously, making progress for the big specification of device provides convenience.
Description of drawings
Fig. 1 is that device of the present invention connects sketch map.
The specific embodiment
The present invention is described in further detail with embodiment below in conjunction with accompanying drawing 1:
Embodiment 1
Scrubbing with liquid nitrogen purifies synthesis gas and the LNG device is reclaimed in cryogenic separation; As shown in Figure 1; Comprise that feed gas preprocessing system, cryogenic purification separate ice chest, azeotrope cooling cycle system; The feed gas preprocessing system comprises regeneration gas heaters 1, molecular sieve adsorber 2, regeneration gas cooler 3; Regeneration gas heaters 1, molecular sieve adsorber 2 and regeneration gas cooler 3 link to each other through pipeline successively; Said cryogenic purification separates ice chest and comprises main heat exchanger 4, knockout drum 5, nitrogen wash column 6, methane rectifying column 7 and be arranged on the thermal siphon formula evaporimeter 8 in the methane rectifying column 7; Said main heat exchanger 4, knockout drum 5, nitrogen wash column 6, methane rectifying column 7 connect through pipeline successively, and methane rectifying column 7 tops are connected into main heat exchanger 4 through pipeline, and said azeotrope cooling cycle system comprises cryogen compensator 9, cryogen compressor 10, compressor one-level knockout drum 11, compressor secondary knockout drum 12, three grades of knockout drums 13 of compressor and cooler; Said molecular sieve adsorber 2 and main heat exchanger 4 are connected through pipeline, and three grades of knockout drums 13 of said compressor and main heat exchanger 4 are connected through pipeline.
Cooler comprises compressor one-level cooler 141, compressor secondary coolers 142, three grades of coolers 143 of compressor; Cryogen compressor 10 comprises first order cryogen compressor 101, second level cryogen compressor 102, third level cryogen compressor 103, and said cryogen compensator 9, first order cryogen compressor 101, compressor one-level cooler 141, compressor one-level knockout drum 11, second level cryogen compressor 102, compressor secondary coolers 142, compressor secondary knockout drum 12, third level cryogen compressor 103, three grades of knockout drums 13 of compressor connect through pipeline successively.Be connected with cryogenic fluid pump 15 on the compressor secondary coolers 142.
Unstrpped gas after pretreatment system is handled is sent into 2 main heat exchangers in the ice chest successively; In this synthesis gas that is backflowed, fuel gas and azeotrope cooling; Get into knockout drum then and carry out gas-liquid separation, the back of continuing to be cooled of gas phase wherein gets into the nitrogen wash column bottom, wherein contained impurity as: carbon monoxide, argon and methane etc. are washed out by the liquid nitrogen that the top is come in nitrogen wash column; The synthesis gas that contains small amount of nitrogen after the purification leaves from the nitrogen wash column cat head; Through the main heat exchanger re-heat, allocate the nitrogen that comes in the high pressure nitrogen pipeline into (being that gas phase is joined nitrogen) then, reach hydrogen and nitrogen gas stoicheiometry 3:1 basically after; Wherein a part of synthesis gas leads to the low-temperature rectisol operation, returns the cold that is brought from the low-temperature rectisol operation by unstrpped gas; Another part synthesis gas continues cooling box after through main heat exchanger re-heat to environment temperature, and sends into the ammonia synthesis operation as product gas after joining the correct hydrogen of nitrogen realization, nitrogen stoicheiometry with converging from the synthesis gas after the re-heat of low-temperature rectisol operation through smart again.
High pressure nitrogen is from the air separation unit outside the battery limit (BL), and after main heat exchanger was backflowed gas cooled, wherein major part was directly mixed with the nitrogen gas washing that comes from the nitrogen wash column top through throttling, reaches hydrogen and nitrogen gas stoicheiometry 3:1 basically; Remainder continues cooling and liquefaction in main heat exchanger, and liquid nitrogen gets into the nitrogen wash column top, as washing agent, in nitrogen wash column, the impurity in the unstrpped gas is washed.
The liquid of knockout drum bottom and nitrogen wash column bottom gets into rectifying column through decompression; In rectifying column, separate; Obtain highly purified LNG at the bottom of the tower, the liquid of the gas phase of cat head and nitrogen wash column bottom returns the re-heat cooling box after the valve decompression, and pneumatic transmission to full factory fuel gas system acts as a fuel.
It is that system provides cold that the present invention adopts the azeotrope cooling cycle system.Azeotrope is made up of the mixture of N2 and C1～C5; Azeotrope after interstage cooler is cooled to 40 ℃, gets into the one-level knockout drum through the compression of the compressor first order subsequently, and gas phase partly gets into the azeotrope compressor second level and continues pressurization; After secondary coolers is cooled to 40 ℃, getting into the secondary knockout drum separates; Gas phase partly continues to get into the cryogen compressor pressurizes, and is cooled to 40 ℃ through aftercooler, gets into the final stage separator again and separates.Become to enter into the precooling zone of main heat exchanger after the liquid mixing that the liquid that the I and II separator comes out goes out with the final stage separator separates respectively after cryogenic fluid pump is got to certain pressure; Cross cold after choke valve throttling cooling at precooling zone; With turn back to precooling zone after the follow-up cryogen that backflows mixes and for this section cold be provided jointly, cooling unstripped gas, high pressure nitrogen, gaseous state cryogen and needed cold liquid refrigerant; The entering cold catch pot separated after the gaseous state cryogen entering main heat exchanger precooling zone that the final stage separator comes out cooled off, and turned back to main heat exchanger after liquid phase part continuation entering main heat exchanger is crossed cold and throttling is lowered the temperature with after the follow-up gas that backflows mixes, for this section provides cold; The gas phase part of cold catch pot is cooled to uniform temperature through main heat exchanger successively, after the choke valve throttling, becomes the gas that backflows again and gets into main heat exchanger, for this section provides cold.The low pressure azeotrope of in main heat exchanger, having participated in after the heat exchange gets into the azeotrope suction port of compressor through cryogen suction tank buffering back, so circulates repeatedly, for system purification and cryogenic separation provide cold.
In a word, the above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (4)
1. scrubbing with liquid nitrogen purifies synthesis gas and cryogenic separation recovery LNG device thereof; Comprise that feed gas preprocessing system, cryogenic purification separate ice chest, azeotrope cooling cycle system; It is characterized in that: described feed gas preprocessing system comprises regeneration gas heaters (1), molecular sieve adsorber (2), regeneration gas cooler (3); Regeneration gas heaters (1), molecular sieve adsorber (2) and regeneration gas cooler (3) link to each other through pipeline successively; Said cryogenic purification separates ice chest and comprises main heat exchanger (4), knockout drum (5), nitrogen wash column (6), methane rectifying column (7) and be arranged on the tower bottom reboiler (8) in the methane rectifying column (7); Said main heat exchanger (4), knockout drum (5), nitrogen wash column (6), methane rectifying column (7) connect through pipeline successively; Methane rectifying column (7) top is connected into main heat exchanger (4) through pipeline; Said azeotrope cooling cycle system comprises cryogen compensator (9), cryogen compressor (10), compressor one-level knockout drum (11), compressor secondary knockout drum (12), three grades of knockout drums of compressor (13) and cooler; Said molecular sieve adsorber (2) is connected through pipeline with main heat exchanger (4), and three grades of knockout drums of said compressor (13) are connected through pipeline with main heat exchanger (4).
2. scrubbing with liquid nitrogen according to claim 1 purifies synthesis gas and the LNG device is reclaimed in cryogenic separation; It is characterized in that: described cooler comprises compressor one-level cooler (141), compressor secondary coolers (142), three grades of coolers of compressor (143); Cryogen compressor (10) comprises first order cryogen compressor (101), second level cryogen compressor (102), third level cryogen compressor (103), and said cryogen compensator (9), first order cryogen compressor (101), compressor one-level cooler (141), compressor one-level knockout drum (11), second level cryogen compressor (102), compressor secondary coolers (142), compressor secondary knockout drum (12), third level cryogen compressor (103), three grades of knockout drums of compressor (13) connect through pipeline successively.
3. scrubbing with liquid nitrogen according to claim 1 and 2 purifies synthesis gas and the LNG device is reclaimed in cryogenic separation, it is characterized in that: be connected with cryogenic fluid pump (15) on the described compressor secondary coolers (142).
4. scrubbing with liquid nitrogen according to claim 1 purifies synthesis gas and the LNG device is reclaimed in cryogenic separation, it is characterized in that: described tower bottom reboiler (8) adopts thermal siphon formula evaporimeter.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104173858A CN102435045A (en) | 2011-12-14 | 2011-12-14 | Liquid nitrogen washing purified synthetic gas and device for cryogenically separating and recovering LNG (liquefied natural gas) thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104173858A CN102435045A (en) | 2011-12-14 | 2011-12-14 | Liquid nitrogen washing purified synthetic gas and device for cryogenically separating and recovering LNG (liquefied natural gas) thereof |
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| CN102435045A true CN102435045A (en) | 2012-05-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104251600A (en) * | 2013-06-26 | 2014-12-31 | 航天长征化学工程股份有限公司 | Liquid nitrogen washing device |
| CN106185801A (en) * | 2016-07-04 | 2016-12-07 | 华陆工程科技有限责任公司 | A kind of scrubbing with liquid nitrogen devices and methods therefor that can reclaim methane |
| CN106369934A (en) * | 2016-10-25 | 2017-02-01 | 杭州中泰深冷技术股份有限公司 | Frozen blocking preventing co-production LNG liquid nitrogen wash device combined with mixed refrigerant system and method thereof |
| CN111886465A (en) * | 2018-03-21 | 2020-11-03 | 乔治洛德方法研究和开发液化空气有限公司 | Method and apparatus for separating synthesis gas by cryogenic distillation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104251600A (en) * | 2013-06-26 | 2014-12-31 | 航天长征化学工程股份有限公司 | Liquid nitrogen washing device |
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| CN106369934A (en) * | 2016-10-25 | 2017-02-01 | 杭州中泰深冷技术股份有限公司 | Frozen blocking preventing co-production LNG liquid nitrogen wash device combined with mixed refrigerant system and method thereof |
| CN106369934B (en) * | 2016-10-25 | 2022-04-26 | 杭州中泰深冷技术股份有限公司 | Anti-freezing and anti-blocking co-production LNG liquid nitrogen washing device and method combined with mixed refrigerant system |
| CN111886465A (en) * | 2018-03-21 | 2020-11-03 | 乔治洛德方法研究和开发液化空气有限公司 | Method and apparatus for separating synthesis gas by cryogenic distillation |
| CN111886465B (en) * | 2018-03-21 | 2022-06-24 | 乔治洛德方法研究和开发液化空气有限公司 | Method and apparatus for separating synthesis gas by cryogenic distillation |
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Application publication date: 20120502 |