CN109282576A - A kind of device and production method with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide - Google Patents
A kind of device and production method with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide Download PDFInfo
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- CN109282576A CN109282576A CN201811166292.0A CN201811166292A CN109282576A CN 109282576 A CN109282576 A CN 109282576A CN 201811166292 A CN201811166292 A CN 201811166292A CN 109282576 A CN109282576 A CN 109282576A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 201
- 238000004821 distillation Methods 0.000 title claims abstract description 127
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 100
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 92
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 38
- 239000007789 gas Substances 0.000 claims abstract description 361
- 230000008676 import Effects 0.000 claims abstract description 139
- 239000012071 phase Substances 0.000 claims abstract description 133
- 239000007788 liquid Substances 0.000 claims abstract description 125
- 239000007791 liquid phase Substances 0.000 claims abstract description 105
- 239000000463 material Substances 0.000 claims abstract description 51
- 230000003009 desulfurizing effect Effects 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 230000001105 regulatory effect Effects 0.000 claims description 103
- 238000000746 purification Methods 0.000 claims description 29
- 239000007792 gaseous phase Substances 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 21
- 238000000926 separation method Methods 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 18
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 6
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 6
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 6
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 8
- 239000005864 Sulphur Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 235000010210 aluminium Nutrition 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000019086 sulfide ion homeostasis Effects 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000003407 synthetizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
-
- 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
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
- Y02B30/52—Heat recovery pumps, i.e. heat pump based systems or units able to transfer the thermal energy from one area of the premises or part of the facilities to a different one, improving the overall efficiency
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention belongs to a kind of devices and production method with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide；Including unstripped gas surge tank, product pump, products pot, liquefied ammonia heat pump and desulfurizing tower, unstripped gas surge tank passes sequentially through the raw material gas inlet of First Heat Exchanger, the unstripped gas outlet of First Heat Exchanger, the first material liquid import of the raw material gas inlet of first rectifying column middle and lower part, the liquid-phase outlet of first rectifying column bottom, Second distillation column, the outlet of Second distillation column top gas phase, the tube side of third heat exchanger, the first threeway and product pump and is connected with products pot；Have the advantages that structure is simple, purity easy to operate, stable and that can prepare liquid phase hydrogen sulfide product is not less than 99.999%.
Description
Technical field
The invention belongs to high-pure hydrogen sulfide production technical fields, and in particular to one kind is able to produce purity and is not less than
The device and production method with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide of 99.999% hydrogen sulfide.
Background technique
Hydrogen sulfide has important in multiple industrial fields such as chemical industry, organic synthesis industry, metallurgical industry, electronics industries
Purposes.It is usually used in synthesizing sulphur and sulfuric acid, vulcanized sodium and NaHS, heavy water, methyl mercaptan, dimethyl sulfoxide, thioglycol, sulphur
The products such as urea.In semiconductor field, it is mainly used as doping gas, is used as synthetizing phosphor powder, electricity gives out light, optical conductor, photo-optical exposure meter
Deng manufacture.The method of industrial production hydrogen sulfide has " preparing hydrogen sulfide with sulphur hydrogenation reaction ", " is reacted with barium sulfate and hydrochloric acid
Prepare hydrogen sulfide ", " preparing hydrogen sulfide with methane and reaction of Salmon-Saxl ", " recycle sulphur from natural gas and industrial gas containing acid gas
Change hydrogen ", " preparing hydrogen sulfide with sodium hydrosulfide aqueous solution and sulfuric acid reaction ".
(1) hydrogen sulfide is prepared with sulphur hydrogenation reaction: S+H2→H2S, general H2The yield of S is up to 98% or more, if feed hydrogen is
Pure hydrogen, raw material sulphur are top grade product, then H2The purity of S is up to 98%~99.9%.
(2) hydrogen sulfide is prepared with barium sulfate and hydrochloric acid reaction: BaS+2HCl → BaCl2+H2S, H2The purity of S be 98%~
99%.
(3) hydrogen sulfide is prepared with methane and reaction of Salmon-Saxl: CH4+4S→2H2S+CS2, 2CS2+H2O→2H2S+CO2, product H2S
Purity be 79%.
(4) hydrogen sulfide is recycled from natural gas and industrial gas containing acid gas: utilizing chemical solvent selective absorbing sulphur
Change a kind of important method that hydrogen is commercial scale hydrogen sulfide.General chemical solvent has alkyl alcoholamine and basic carbonate
Aqueous solution.The H of this method preparation2Contain moisture content in S product, H more serious to the corrosion of equipment, pipeline2The purity of S is 99%.
(5) hydrogen sulfide is prepared with sodium hydrosulfide aqueous solution and sulfuric acid reaction: the H of preparation2S concentration is 99%, and process needs
Handle a large amount of H2S waste liquid.
Summary of the invention
A kind of side using heat pump and two-tower rectification is provided it is an object of the invention to overcome defect in the prior art
Formula, its structure be simple, purity that is easy to operate, stable and can preparing liquid phase hydrogen sulfide product is not less than 99.999%
The device and production method with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide.
The object of the present invention is achieved like this: including unstripped gas surge tank, product pump, products pot, liquefied ammonia heat pump and taking off
Sulphur tower, the unstripped gas surge tank pass sequentially through the raw material gas inlet of First Heat Exchanger, the unstripped gas outlet of First Heat Exchanger, the
The raw material gas inlet of one rectifying column middle and lower part, the liquid-phase outlet of first rectifying column bottom, Second distillation column the first material liquid into
Mouth, the outlet of Second distillation column top gas phase, the tube side of third heat exchanger, the first threeway and product pump are connected with products pot；First
The third end of threeway is connected with the second material liquid import of Second distillation column；
Gaseous phase outlet at the top of first rectifying column passes through the import phase of the tube side and the first gas-liquid separator of the second heat exchanger
Even, the liquid-phase outlet of the first gas-liquid separator is connected with the material liquid import of first rectifying column middle and upper part；First gas-liquid separator
Gaseous phase outlet pass through the import phase of the first inlet exhaust gas of First Heat Exchanger and the first offgas outlet of First Heat Exchanger and desulfurizing tower
Even；
The liquid-phase outlet of Second distillation column bottom passes through the second tail of the second inlet exhaust gas of First Heat Exchanger and First Heat Exchanger
Gas outlet is connected with the import of desulfurizing tower；
The circulating air outlet of liquefied ammonia heat pump passes sequentially through the second threeway, the first reboiler of first rectifying column bottom, second
The first circulation gas import of the shell side, First Heat Exchanger of heat exchanger and the first circulation gas outlet of First Heat Exchanger and liquefied ammonia heat pump
Global cycle gas import be connected；The third end of second threeway passes sequentially through the second reboiler of Second distillation column bottom, third is changed
The second circulation gas import of the shell side, First Heat Exchanger of hot device and the second circulation gas outlet of First Heat Exchanger and liquefied ammonia heat pump
Global cycle gas import is connected.
Preferably, the first regulating valve is equipped between the unstripped gas surge tank and the raw material gas inlet of First Heat Exchanger, the
The unstripped gas of one heat exchanger is exported is equipped with the second regulating valve, the first rectifying between the raw material gas inlet of first rectifying column middle and lower part
Third regulating valve, the third of the first threeway are equipped between first material liquid import of the liquid-phase outlet and Second distillation column of tower bottom
It is equipped with the 4th regulating valve between end and the second material liquid import of Second distillation column, the 5th is equipped between the first threeway and product pump
Regulating valve, the entrance of desulfurizing tower are equipped with the 6th regulating valve, and the is equipped between the circulating air outlet of liquefied ammonia heat pump and the second threeway
Seven regulating valves, between the first reboiler of first rectifying column bottom and the shell side of the second heat exchanger be equipped with first throttle valve, second
Second throttle, the liquid of Second distillation column bottom are equipped between second reboiler of rectifier bottoms and the shell side of third heat exchanger
The 8th regulating valve is mutually equipped between outlet and the second inlet exhaust gas of First Heat Exchanger.
Preferably, the 9th regulating valve is equipped between the product pump and products pot.
A kind of production method of the device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, includes the following steps:
Step 1: the unstripped gas in unstripped gas surge tank pass sequentially through the first regulating valve, First Heat Exchanger unstripped gas into
The unstripped gas outlet of mouth, First Heat Exchanger enters in first rectifying column, the main composition of the unstripped gas: carbon dioxide,
Hydrogen sulfide, methanol, nitrogen, carbon monoxide, carbonyl sulfur, sulfur dioxide, methane, ethane, ethylene, propane and propylene；Unstripped gas
Temperature: 35~40 DEG C, pressure: 0.7Mpa, flow: 600Nm3/ h, gas phase fraction: 1, H2S molar fraction: 35%；First heat exchange
The unstripped gas temperature of device unstripped gas outlet: -41~-45 DEG C, gas phase fraction is 0.6, H2S molar fraction: 35%；
Step 2: make to enter in step 1 rectification and purification of unstripped gas progress, a rectification and purification in first rectifying column
Gas phase afterwards is entered in the first gas-liquid separator by the tube side of the outlet of first rectifying column top gas phase and the second heat exchanger to be carried out
Gas-liquid separation, the liquid phase after gas-liquid separation pass through the liquid-phase outlet of the first gas-liquid separator and the raw material of first rectifying column middle and upper part
Liquid import enters in first rectifying column；The gas phase temperature of the first rectifying column top gas phase outlet: -41~-39 DEG C, H2S rubs
That score: 6~10%；By the material liquid import of first rectifying column middle and upper part enter the liquidus temperature in first rectifying column be-
48~-45 DEG C, H2S molar fraction: 20~25%, gas phase fraction: 0.
Step 3: the bottom liquid phases after entering first rectifying column purification in step 2 enter the second essence by third regulating valve
It evaporates in tower, the liquid-phase product temperature of the bottom liquid phases outlet of the first rectifying column: -15~-10 DEG C, flow: 145~
166Nm3/ h, H2S molar fraction: 99.5~99.9%；
Step 4: making to enter in step 3 liquid phase in Second distillation column and carry out secondary rectification and purification, after secondary rectification and purification
Gas phase entered in the first threeway by the outlet of Second distillation column top gas phase and the tube side of third heat exchanger, into the one or three
Liquid phase in leading to is divided into two strands, one liquid phase passes through the second of the third end of the first threeway, the 4th regulating valve and Second distillation column
Material liquid import enters in Second distillation column, and another burst of liquid phase is adjusted by the first threeway, the 5th regulating valve, product pump and the 9th
Valve enters in products pot；The gas phase temperature of the Second distillation column top gas phase outlet: -19~-21 DEG C, gas phase fraction: 1；The
Liquidus temperature in second material liquid import of two rectifying columns: -19~-21 DEG C, gas phase fraction: 0；The liquid phase of product pump entrance
Temperature: -19~-21 DEG C, H2S product purity is not less than 99.999%；
Step 5: the first gas is passed sequentially through by the gas phase after progress gas-liquid separation in the first gas-liquid separator in step 2
The gaseous phase outlet of liquid/gas separator, the first inlet exhaust gas of First Heat Exchanger, the first offgas outlet of First Heat Exchanger, the 6th regulating valve and
The import of desulfurizing tower enters in desulfurizing tower；The gas phase temperature of the gaseous phase outlet of first gas-liquid separator: -45~-48 DEG C, stream
Amount: 434~455Nm3/ h, gas phase fraction: 1；
Step 6: the liquid phase after the secondary rectification and purification of Second distillation column in step 4 passes through the liquid of Second distillation column bottom
Mutually outlet, the 8th regulating valve, the second inlet exhaust gas of First Heat Exchanger, the second offgas outlet of First Heat Exchanger, the 6th regulating valve
Import with desulfurizing tower enters in desulfurizing tower；The liquidus temperature of the liquid-phase outlet of the Second distillation column bottom: -21~-18 DEG C,
Flow: 18~25Nm3/ h, gas phase fraction: 0；
Step 7: the circulating air in liquefied ammonia heat pump enters second by the circulating air outlet of liquefied ammonia heat pump and the 7th regulating valve
It is divided into two strands in threeway, one circulating air passes through the first reboiler, first throttle valve, the second heat exchanger of first rectifying column bottom
Shell side, the first circulation gas import of First Heat Exchanger, the first circulation gas outlet of First Heat Exchanger and always following for liquefied ammonia heat pump
Ring gas import enters in liquefied ammonia heat pump, another strand of circulating air by the third end of the second threeway, Second distillation column bottom second
Reboiler, second throttle, the shell side of third heat exchanger, the second circulation gas import of First Heat Exchanger, the outlet of second circulation gas
Global cycle gas import with liquefied ammonia heat pump enters in liquefied ammonia heat pump；The component of the circulating air: liquefied ammonia, liquefied ammonia molar fraction:
100%；The circulating air temperature of the shell side of second heat exchanger: -48~-51 DEG C, gas phase fraction: 0.9；The shell side of third heat exchanger
Circulating air temperature: -21~-24 DEG C, gas phase fraction: 0.9；The circulation fluid temperature of the first reboiler outlet: -11~-8 DEG C,
Gas phase fraction: 0；The circulation fluid temperature of second reboiler outlet: -18~-15 DEG C, second adjusts the circulation fluid temperature of valve outlet: -
21~-24 DEG C.
The present invention uses heat pump distillation technology to provide cooling capacity and heat for whole system, and two-tower rectification produces high-pure hydrogen sulfide
Device and production method, product liquid phase vulcanize hydrogen purity and be not less than 99.999%, filled up the production of domestic high-pure hydrogen sulfide
Blank has established the basis of electronics industry and semicon industry development, has had great importance.Compared with conventional process techniques,
The present invention has the advantage that 1. use liquefied ammonia heat pump distillations, capacity usage ratio is improved, and heat pump distillation is by by the steam of tower top
Pressurization heating, and then thermic load is provided to tower reactor, and recycle the condensation latent heat of tower top, low energy consumption；2. using the life of two-tower rectification
Production mode, more traditional single production model, production technology is more relative complex, but this is to meet high-purity grade of product mark
Standard, most of impurity contained by first rectifying column removing system, Second distillation column technical grade hydrogen sulfide rectification and purification again；3. producing
Product purity fills up the production blank of domestic high-pure hydrogen sulfide, solves conventionally produced hydrogen sulfide up to 99.999% or more
The problem of purity not high (highest 99.9%).The present invention not only greatly improves thermodynamics utilization efficiency, while solving simple
Rectifier unit product quality the problem of high-purity grade of specification is not achieved；With easy to operate, stable, high degree of automation and
The characteristics of product purity capable of being improved to 99.999% high-purity rank；Research and semiconductor field to electronics industry special gas
Development provide safeguard, have good economic and social benefit.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention.
Specific embodiment
For a clearer understanding of the technical characteristics, objects and effects of the present invention, this hair of Detailed description of the invention is now compareed
Bright specific embodiment, identical label indicates identical component in the various figures.To make simplified form, in each figure only schematically
Ground indicates part relevant to invention, they do not represent its practical structures as product.
As shown in Figure 1, the present invention is a kind of device and producer with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide
Method, device part include unstripped gas surge tank 10, product pump 19, products pot 20, liquefied ammonia heat pump 22 and desulfurizing tower 21, the original
Material gas surge tank 10 passes sequentially through the unstripped gas outlet 25, the of the raw material gas inlet 24 of First Heat Exchanger 11, First Heat Exchanger 11
First original of the raw material gas inlet of one rectifying column, 12 middle and lower part, the liquid-phase outlet of 12 bottom of first rectifying column, Second distillation column 16
Liquor inlet 38, the outlet of 16 top gas phase of Second distillation column, the tube side of third heat exchanger 18, the first threeway 27 and product pump 19 with
Products pot 20 is connected；The third end of first threeway 27 is connected with the second material liquid import 33 of Second distillation column 16；First rectifying
The gaseous phase outlet at 12 top of tower is connected by the tube side of the second heat exchanger 14 with the import of the first gas-liquid separator 15, the first gas-liquid
The liquid-phase outlet of separator 15 is connected with the material liquid import of 12 middle and upper part of first rectifying column；The gas phase of first gas-liquid separator 15
Outlet by 11 first inlet exhaust gas 34 of First Heat Exchanger and 11 first offgas outlet 35 of First Heat Exchanger and desulfurizing tower 21 into
Mouth is connected；The liquid-phase outlet of 16 bottom of Second distillation column passes through 11 second inlet exhaust gas 37 of First Heat Exchanger and First Heat Exchanger 11
Second offgas outlet 36 is connected with the import of desulfurizing tower 21；Liquefied ammonia heat pump 22 circulating air outlet pass sequentially through the second threeway 28,
First reboiler 13 of 12 bottom of first rectifying column, the shell side of the second heat exchanger 14, First Heat Exchanger 14 first circulation gas into
The first circulation gas of mouth 31 and First Heat Exchanger 14 outlet 32 is connected with the global cycle gas import of liquefied ammonia heat pump 22；Second threeway 28
Third end pass sequentially through the second reboiler 17, the shell side of third heat exchanger 18, First Heat Exchanger of 16 bottom of Second distillation column
The global cycle gas of the second circulation gas of 11 second circulation gas import 29 and First Heat Exchanger 11 outlet 30 and liquefied ammonia heat pump 22 into
Mouth is connected.Between the unstripped gas surge tank 10 and the raw material gas inlet 24 of First Heat Exchanger 11 be equipped with the first regulating valve 1, first
The second regulating valve 2 is equipped between the unstripped gas outlet 25 of heat exchanger 11 and the raw material gas inlet of 12 middle and lower part of first rectifying column, the
Third regulating valve 3 is equipped between first material liquid import 38 of the liquid-phase outlet and Second distillation column 16 of one rectifying column, 12 bottom,
Between the third end of first threeway 27 and the second material liquid import 33 of Second distillation column 16 be equipped with the 4th regulating valve 4, the one or three
The 5th regulating valve 5 is equipped between logical 27 and product pump 19, the entrance of desulfurizing tower 21 is equipped with the 6th regulating valve 6, liquefied ammonia heat pump 22
Circulating air outlet the second threeway 28 between be equipped with the 7th regulating valve 7,13 He of the first reboiler of 12 bottom of first rectifying column
First throttle valve 8 is equipped between the shell side of second heat exchanger 14, the second reboiler 17 and third of 16 bottom of Second distillation column change
Second throttle 9, the liquid-phase outlet and First Heat Exchanger 11 second of 16 bottom of Second distillation column are equipped between the shell side of hot device 18
The 8th regulating valve 23 is equipped between inlet exhaust gas 37.The 9th regulating valve 26 is equipped between the product pump 19 and products pot 20.
A kind of production method of the device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, includes the following steps:
Step 1: the unstripped gas in unstripped gas surge tank 10 passes sequentially through the raw material of the first regulating valve 1, First Heat Exchanger 11
Gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11 enter in first rectifying columns 12, the main composition of the unstripped gas at
Part: carbon dioxide, hydrogen sulfide, methanol, nitrogen, carbon monoxide, carbonyl sulfur, sulfur dioxide, methane, ethane, ethylene, propane and
Propylene；The temperature of unstripped gas: 35~40 DEG C, pressure: 0.7Mpa, flow: 600Nm3/ h, gas phase fraction: 1, H2S molar fraction:
35%；The unstripped gas temperature of 11 unstripped gas of First Heat Exchanger outlet 25: -41~-45 DEG C, gas phase fraction is 0.6, H2S moles point
Number: 35%；
Step 2: make to enter in step 1 rectification and purification of unstripped gas progress, a rectifying in first rectifying column 12 and mention
Gas phase after pure enters the first gas-liquid separator by the tube side of the outlet of 12 top gas phase of first rectifying column and the second heat exchanger 14
Gas-liquid separation is carried out in 15, the liquid phase after gas-liquid separation passes through the liquid-phase outlet and first rectifying column 12 of the first gas-liquid separator 15
The material liquid import of middle and upper part enters in first rectifying column 12；The gas phase temperature of 12 top gas phase of the first rectifying column outlet :-
41~-39 DEG C, H2S molar fraction: 6~10%；Enter the first rectifying by the material liquid import of 12 middle and upper part of first rectifying column
Liquidus temperature in tower 12 is -48~-45 DEG C, H2S molar fraction: 20~25%, gas phase fraction: 0.
Step 3: enter the bottom liquid phases after first rectifying column 12 purifies in step 2 and enter the by third regulating valve 3
In two rectifying columns 16, the liquid-phase product temperature of the bottom liquid phases outlet of the first rectifying column 12: -15~-10 DEG C, flow: 145
~166Nm3/ h, H2S molar fraction: 99.5~99.9%；
Step 4: make to enter in step 3 the secondary rectification and purification of liquid phase progress, secondary rectification and purification in Second distillation column 16
Gas phase afterwards is entered in the first threeway 27 by the tube side of the outlet of 16 top gas phase of Second distillation column and third heat exchanger 18, into
The liquid phase entered in the first threeway 27 is divided into two strands, one liquid phase passes through the third end of the first threeway 27, the 4th regulating valve 4 and second
Second material liquid import 33 of rectifying column 16 enters in Second distillation column 16, and another burst of liquid phase is adjusted by the first threeway the 27, the 5th
Valve 5, product pump 19 and the 9th regulating valve 26 is saved to enter in products pot 20；The gas phase of 16 top gas phase of the Second distillation column outlet
Temperature: -19~-21 DEG C, gas phase fraction: 1；Liquidus temperature in second material liquid import 33 of Second distillation column 16: -19~-
21 DEG C, gas phase fraction: 0；The liquidus temperature of 19 entrance of product pump: -19~-21 DEG C, H2S product purity is not less than
99.999%；
Step 5: first is passed sequentially through by the gas phase after progress gas-liquid separation in the first gas-liquid separator 15 in step 2
The gaseous phase outlet of gas-liquid separator 15,11 first inlet exhaust gas 34 of First Heat Exchanger, 11 first offgas outlet 35 of First Heat Exchanger,
The import of 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The gas of the gaseous phase outlet of first gas-liquid separator 15
Phase temperature: -45~-48 DEG C, flow: 434~455Nm3/ h, gas phase fraction: 1；
Step 6: the liquid phase after 16 2 rectification and purifications of Second distillation column in step 4 passes through 16 bottom of Second distillation column
Liquid-phase outlet, the 8th regulating valve 23,11 second inlet exhaust gas 37 of First Heat Exchanger, First Heat Exchanger 11 the second offgas outlet
36, the import of the 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The liquid-phase outlet of 16 bottom of Second distillation column
Liquidus temperature: -21~-18 DEG C, flow: 18~25Nm3/ h, gas phase fraction: 0；
Step 7: circulating air in liquefied ammonia heat pump 22 by the circulating air outlet of liquefied ammonia heat pump 22 and the 7th regulating valve 7 into
Enter in the second threeway 28 and be divided into two strands, one circulating air passes through the first reboiler 13, the first throttle of 12 bottom of first rectifying column
Valve 8, the shell side of the second heat exchanger 14, the first circulation gas import 31 of First Heat Exchanger 14, First Heat Exchanger 14 first circulation
Gas outlet 32 and the global cycle gas import of liquefied ammonia heat pump 22 enter in liquefied ammonia heat pump 22, and another strand of circulating air passes through the second threeway 28
Third end, the second reboiler 17 of 16 bottom of Second distillation column, second throttle 9, the shell side of third heat exchanger 18, first change
Second circulation gas import 29, second circulation gas outlet 30 and the global cycle gas import of liquefied ammonia heat pump 22 of hot device 11 enter liquefied ammonia heat
In pump 22；The component of the circulating air: liquefied ammonia, liquefied ammonia molar fraction: 100%；The circulation temperature of the shell side of second heat exchanger 14
Degree: -48~-51 DEG C, gas phase fraction: 0.9；The circulating air temperature of the shell side of third heat exchanger 18: -21~-24 DEG C, gas phase point
Rate: 0.9；The circulation fluid temperature that first reboiler 13 exports: -11~-8 DEG C, gas phase fraction: 0；The outlet of second reboiler 17
Circulation fluid temperature: -18~-15 DEG C, second throttle 9 export circulation fluid temperature: -21~-24 DEG C.
The present invention is the device and production method of a kind of high-purity grade of hydrogen sulfide of mode of manufacture with liquefied ammonia heat pump two-tower rectification,
Wherein high-purity grade of hydrogen sulfide product quality does not have national standard, referring to " Chinese industrial gas is complete works of " and the height of external gas companies
Pure hydrogen sulfide company standard, domestic enterprise's standard: >=99.9%, foreign standard: >=99.999% (E-1 grades), bibliography:
" Chinese industrial gas is complete works of " the 4th, the 3753rd country page table II.3.51-14 high-pure hydrogen sulfide product and same kind of products at abroad
Compare.The book is write by Chinese industrial gas industry association, and publishing house of Dalian University of Technology publishes.Present invention process method it is excellent
Gesture is on the one hand to realize to synthesize ammonia sour gas as high-purity grade of hydrogen sulfide of raw material production quality 99.999% to tail gas
Recycling and reusing reduces damage of the sulfide to atmospheric environment, on the other hand also there is a degree of mention in product quality
It is high.First with most of impurity in first rectifying column removing system, secondly, using a small amount of in Second distillation column removing system
Sulfur dioxide meets high-purity grade of hydrogen sulfide product purity requirement.It again, is system by heat pump techniques using liquefied ammonia as refrigerant
Heat and cooling capacity are provided, realize recycling for energy.The utilization efficiency for the energy that above-mentioned mode greatly improves reduces energy
Waste.This last process uses heat pump distillation, two-tower rectification, and configuring product pump inlet and outlet setting regulating valve has behaviour
Make the feature that simplicity, operating cost are low, device stablizes safety.In addition, the present invention simultaneously or can be adopted using manual control
It is controlled, is preferably controlled using automation remote since hydrogen sulfide toxicity is II grades, especially product pump 19 with automation remote
It is filled using canned motor pump and complete No leakage can be achieved, being in addition respectively equipped with self-adjusting valve in the import and outlet of product pump 19 can be real
Existing teletransmission is opened from termination of pumping certainly；In addition the rectifying column interior conduit material in the present invention uses A grades of aluminiums, with low temperature resistant rectifying ring
Border corrosion, while can reduce resultant metal ion micro content, to achieve the purpose that improve product purity.
For the more detailed explanation present invention, the present invention is further elaborated now in conjunction with embodiment.Specific embodiment
It is as follows:
Embodiment one
A kind of device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, including unstripped gas surge tank 10, product pump
19, products pot 20, liquefied ammonia heat pump 22 and desulfurizing tower 21, the unstripped gas surge tank 10 pass sequentially through the raw material of First Heat Exchanger 11
Raw material gas inlet, the first rectifying column of gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11,12 middle and lower part of first rectifying column
The first material liquid import 38, the outlet of 16 top gas phase of Second distillation column, third of the liquid-phase outlet, Second distillation column 16 of 12 bottoms
The tube side of heat exchanger 18, the first threeway 27 and product pump 19 are connected with products pot 20；The third end of first threeway 27 and the second essence
The the second material liquid import 33 for evaporating tower 16 is connected；The gaseous phase outlet at 12 top of first rectifying column passes through the tube side of the second heat exchanger 14
It is connected with the import of the first gas-liquid separator 15, liquid-phase outlet and 12 middle and upper part of first rectifying column of the first gas-liquid separator 15
Material liquid import is connected；The gaseous phase outlet of first gas-liquid separator 15 passes through 11 first inlet exhaust gas 34 and first of First Heat Exchanger
11 first offgas outlet 35 of heat exchanger is connected with the import of desulfurizing tower 21；The liquid-phase outlet of 16 bottom of Second distillation column passes through first
11 second inlet exhaust gas 37 of heat exchanger and 11 second offgas outlet 36 of First Heat Exchanger are connected with the import of desulfurizing tower 21；Liquefied ammonia heat
The circulating air outlet of pump 22 passes sequentially through the first reboiler 13, the second heat exchanger of the second threeway 28,12 bottom of first rectifying column
The first circulation gas import 31 of 14 shell side, First Heat Exchanger 14 and the first circulation gas outlet 32 of First Heat Exchanger 14 and liquefied ammonia
The global cycle gas import of heat pump 22 is connected；What the third end of the second threeway 28 passed sequentially through 16 bottom of Second distillation column second boils again
Device 17, the shell side of third heat exchanger 18, the second circulation gas import 29 of First Heat Exchanger 11 and First Heat Exchanger 11 second follow
Ring gas outlet 30 is connected with the global cycle gas import of liquefied ammonia heat pump 22.The original of the unstripped gas surge tank 10 and First Heat Exchanger 11
Expect to be equipped with the first regulating valve 1 between gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11 and 12 middle and lower part of first rectifying column
Raw material gas inlet between be equipped with the second regulating valve 2, the of the liquid-phase outlet of 12 bottom of first rectifying column and Second distillation column 16
Third regulating valve 3, the third end of the first threeway 27 and the second raw material of Second distillation column 16 are equipped between one material liquid import 38
It is equipped with the 4th regulating valve 4 between liquid import 33, the 5th regulating valve 5, desulfurizing tower 21 are equipped between the first threeway 27 and product pump 19
Entrance be equipped with the 6th regulating valve 6, liquefied ammonia heat pump 22 circulating air outlet the second threeway 28 between be equipped with the 7th regulating valve
7, between the first reboiler 13 of 12 bottom of first rectifying column and the shell side of the second heat exchanger 14 be equipped with first throttle valve 8, second
Second throttle 9, Second distillation column are equipped between the second reboiler 17 and the shell side of third heat exchanger 18 of 16 bottom of rectifying column
The 8th regulating valve 23 is equipped between 11 second inlet exhaust gas 37 of liquid-phase outlet and First Heat Exchanger of 16 bottoms.The product pump 19
The 9th regulating valve 26 is equipped between products pot 20.
A kind of production method of the device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, includes the following steps:
Step 1: the unstripped gas in unstripped gas surge tank 10 passes sequentially through the raw material of the first regulating valve 1, First Heat Exchanger 11
Gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11 enter in first rectifying columns 12, the main composition of the unstripped gas at
Part: carbon dioxide, hydrogen sulfide, methanol, nitrogen, carbon monoxide, carbonyl sulfur, sulfur dioxide, methane, ethane, ethylene, propane and
Propylene；The temperature of unstripped gas: 35~40 DEG C, pressure: 0.7Mpa, flow: 600Nm3/ h, gas phase fraction: 1, H2S molar fraction:
35%；The unstripped gas temperature of 11 unstripped gas of First Heat Exchanger outlet 25: -41 DEG C, gas phase fraction is 0.6, H2S molar fraction:
35%:
Step 2: make to enter in step 1 rectification and purification of unstripped gas progress, a rectifying in first rectifying column 12 and mention
Gas phase after pure enters the first gas-liquid separator by the tube side of the outlet of 12 top gas phase of first rectifying column and the second heat exchanger 14
Gas-liquid separation is carried out in 15, the liquid phase after gas-liquid separation passes through the liquid-phase outlet and first rectifying column 12 of the first gas-liquid separator 15
The material liquid import of middle and upper part enters in first rectifying column 12；The gas phase temperature of 12 top gas phase of the first rectifying column outlet :-
41 DEG C, H2S molar fraction: 6%；Enter the liquid in first rectifying column 12 by the material liquid import of 12 middle and upper part of first rectifying column
Phase temperature is -48 DEG C, H2S molar fraction: 20%, gas phase fraction: 0.
Step 3: enter the bottom liquid phases after first rectifying column 12 purifies in step 2 and enter the by third regulating valve 3
In two rectifying columns 16, the liquid-phase product temperature of the bottom liquid phases outlet of the first rectifying column 12: -15 DEG C, flow: 166Nm3/
H, H2S molar fraction: 99.5%；
Step 4: make to enter in step 3 the secondary rectification and purification of liquid phase progress, secondary rectification and purification in Second distillation column 16
Gas phase afterwards is entered in the first threeway 27 by the tube side of the outlet of 16 top gas phase of Second distillation column and third heat exchanger 18, into
The liquid phase entered in the first threeway 27 is divided into two strands, one liquid phase passes through the third end of the first threeway 27, the 4th regulating valve 4 and second
Second material liquid import 33 of rectifying column 16 enters in Second distillation column 16, and another burst of liquid phase is adjusted by the first threeway the 27, the 5th
Valve 5, product pump 19 and the 9th regulating valve 26 is saved to enter in products pot 20；The gas phase of 16 top gas phase of the Second distillation column outlet
Temperature: -21 DEG C, gas phase fraction: 1；Liquidus temperature in second material liquid import 33 of Second distillation column 16: -21 DEG C, gas phase point
Rate: 0；The liquidus temperature of 19 entrance of product pump: -21 DEG C, H2S product purity 99.999%；
Step 5: first is passed sequentially through by the gas phase after progress gas-liquid separation in the first gas-liquid separator 15 in step 2
The gaseous phase outlet of gas-liquid separator 15,11 first inlet exhaust gas 34 of First Heat Exchanger, 11 first offgas outlet 35 of First Heat Exchanger,
The import of 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The gas of the gaseous phase outlet of first gas-liquid separator 15
Phase temperature: -48 DEG C, flow: 434Nm3/ h, gas phase fraction: 1；
Step 6: the liquid phase after 16 2 rectification and purifications of Second distillation column in step 4 passes through 16 bottom of Second distillation column
Liquid-phase outlet, the 8th regulating valve 23,11 second inlet exhaust gas 37 of First Heat Exchanger, First Heat Exchanger 11 the second offgas outlet
36, the import of the 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The liquid-phase outlet of 16 bottom of Second distillation column
Liquidus temperature: -18 DEG C, flow: 18Nm3/ h, gas phase fraction: 0；
Step 7: circulating air in liquefied ammonia heat pump 22 by the circulating air outlet of liquefied ammonia heat pump 22 and the 7th regulating valve 7 into
Enter in the second threeway 28 and be divided into two strands, one circulating air passes through the first reboiler 13, the first throttle of 12 bottom of first rectifying column
Valve 8, the shell side of the second heat exchanger 14, the first circulation gas import 31 of First Heat Exchanger 14, First Heat Exchanger 14 first circulation
Gas outlet 32 and the global cycle gas import of liquefied ammonia heat pump 22 enter in liquefied ammonia heat pump 22, and another strand of circulating air passes through the second threeway 28
Third end, the second reboiler 17 of 16 bottom of Second distillation column, second throttle 9, the shell side of third heat exchanger 18, first change
Second circulation gas import 29, second circulation gas outlet 30 and the global cycle gas import of liquefied ammonia heat pump 22 of hot device 11 enter liquefied ammonia heat
In pump 22；The component of the circulating air: liquefied ammonia, liquefied ammonia molar fraction: 100%；The circulation temperature of the shell side of second heat exchanger 14
Degree: -51 DEG C, gas phase fraction: 0.9；The circulating air temperature of the shell side of third heat exchanger 18: -24 DEG C, gas phase fraction: 0.9；It is described
The circulation fluid temperature of first reboiler 13 outlet: -111 DEG C, gas phase fraction: 0；The circulation fluid temperature of second reboiler 17 outlet :-
15 DEG C, the circulation fluid temperature that second throttle 9 exports: -24 DEG C.
Embodiment two
A kind of device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, including unstripped gas surge tank 10, product pump
19, products pot 20, liquefied ammonia heat pump 22 and desulfurizing tower 21, the unstripped gas surge tank 10 pass sequentially through the raw material of First Heat Exchanger 11
Raw material gas inlet, the first rectifying column of gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11,12 middle and lower part of first rectifying column
The first material liquid import 38, the outlet of 16 top gas phase of Second distillation column, third of the liquid-phase outlet, Second distillation column 16 of 12 bottoms
The tube side of heat exchanger 18, the first threeway 27 and product pump 19 are connected with products pot 20；The third end of first threeway 27 and the second essence
The the second material liquid import 33 for evaporating tower 16 is connected；The gaseous phase outlet at 12 top of first rectifying column passes through the tube side of the second heat exchanger 14
It is connected with the import of the first gas-liquid separator 15, liquid-phase outlet and 12 middle and upper part of first rectifying column of the first gas-liquid separator 15
Material liquid import is connected；The gaseous phase outlet of first gas-liquid separator 15 passes through 11 first inlet exhaust gas 34 and first of First Heat Exchanger
11 first offgas outlet 35 of heat exchanger is connected with the import of desulfurizing tower 21；The liquid-phase outlet of 16 bottom of Second distillation column passes through first
11 second inlet exhaust gas 37 of heat exchanger and 11 second offgas outlet 36 of First Heat Exchanger are connected with the import of desulfurizing tower 21；Liquefied ammonia heat
The circulating air outlet of pump 22 passes sequentially through the first reboiler 13, the second heat exchanger of the second threeway 28,12 bottom of first rectifying column
The first circulation gas import 31 of 14 shell side, First Heat Exchanger 14 and the first circulation gas outlet 32 of First Heat Exchanger 14 and liquefied ammonia
The global cycle gas import of heat pump 22 is connected；What the third end of the second threeway 28 passed sequentially through 16 bottom of Second distillation column second boils again
Device 17, the shell side of third heat exchanger 18, the second circulation gas import 29 of First Heat Exchanger 11 and First Heat Exchanger 11 second follow
Ring gas outlet 30 is connected with the global cycle gas import of liquefied ammonia heat pump 22.The original of the unstripped gas surge tank 10 and First Heat Exchanger 11
Expect to be equipped with the first regulating valve 1 between gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11 and 12 middle and lower part of first rectifying column
Raw material gas inlet between be equipped with the second regulating valve 2, the of the liquid-phase outlet of 12 bottom of first rectifying column and Second distillation column 16
Third regulating valve 3, the third end of the first threeway 27 and the second raw material of Second distillation column 16 are equipped between one material liquid import 38
It is equipped with the 4th regulating valve 4 between liquid import 33, the 5th regulating valve 5, desulfurizing tower 21 are equipped between the first threeway 27 and product pump 19
Entrance be equipped with the 6th regulating valve 6, liquefied ammonia heat pump 22 circulating air outlet the second threeway 28 between be equipped with the 7th regulating valve
7, between the first reboiler 13 of 12 bottom of first rectifying column and the shell side of the second heat exchanger 14 be equipped with first throttle valve 8, second
Second throttle 9, Second distillation column are equipped between the second reboiler 17 and the shell side of third heat exchanger 18 of 16 bottom of rectifying column
The 8th regulating valve 23 is equipped between 11 second inlet exhaust gas 37 of liquid-phase outlet and First Heat Exchanger of 16 bottoms.The product pump 19
The 9th regulating valve 26 is equipped between products pot 20.
A kind of production method of the device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, includes the following steps:
Step 1: the unstripped gas in unstripped gas surge tank 10 passes sequentially through the raw material of the first regulating valve 1, First Heat Exchanger 11
Gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11 enter in first rectifying columns 12, the main composition of the unstripped gas at
Part: carbon dioxide, hydrogen sulfide, methanol, nitrogen, carbon monoxide, carbonyl sulfur, sulfur dioxide, methane, ethane, ethylene, propane and
Propylene；The temperature of unstripped gas: 35~40 DEG C, pressure: 0.7Mpa, flow: 600Nm3/ h, gas phase fraction: 1, H2S molar fraction:
35%；The unstripped gas temperature of 11 unstripped gas of First Heat Exchanger outlet 25: -43 DEG C, gas phase fraction is 0.6, H2S molar fraction:
35%；
Step 2: make to enter in step 1 rectification and purification of unstripped gas progress, a rectifying in first rectifying column 12 and mention
Gas phase after pure enters the first gas-liquid separator by the tube side of the outlet of 12 top gas phase of first rectifying column and the second heat exchanger 14
Gas-liquid separation is carried out in 15, the liquid phase after gas-liquid separation passes through the liquid-phase outlet and first rectifying column 12 of the first gas-liquid separator 15
The material liquid import of middle and upper part enters in first rectifying column 12；The gas phase temperature of 12 top gas phase of the first rectifying column outlet :-
40 DEG C, H2S molar fraction: 8%；Enter the liquid in first rectifying column 12 by the material liquid import of 12 middle and upper part of first rectifying column
Phase temperature is -46.5 DEG C, H2S molar fraction: 23%, gas phase fraction: 0.
Step 3: enter the bottom liquid phases after first rectifying column 12 purifies in step 2 and enter the by third regulating valve 3
In two rectifying columns 16, the liquid-phase product temperature of the bottom liquid phases outlet of the first rectifying column 12: -12 DEG C, flow: 155Nm3/
H, H2S molar fraction: 99.7%；
Step 4: make to enter in step 3 the secondary rectification and purification of liquid phase progress, secondary rectification and purification in Second distillation column 16
Gas phase afterwards is entered in the first threeway 27 by the tube side of the outlet of 16 top gas phase of Second distillation column and third heat exchanger 18, into
The liquid phase entered in the first threeway 27 is divided into two strands, one liquid phase passes through the third end of the first threeway 27, the 4th regulating valve 4 and second
Second material liquid import 33 of rectifying column 16 enters in Second distillation column 16, and another burst of liquid phase is adjusted by the first threeway the 27, the 5th
Valve 5, product pump 19 and the 9th regulating valve 26 is saved to enter in products pot 20；The gas phase of 16 top gas phase of the Second distillation column outlet
Temperature: -20 DEG C, gas phase fraction: 1；Liquidus temperature in second material liquid import 33 of Second distillation column 16: -20 DEG C, gas phase point
Rate: 0；The liquidus temperature of 19 entrance of product pump: -20 DEG C, H2S product purity 99.9993%；
Step 5: first is passed sequentially through by the gas phase after progress gas-liquid separation in the first gas-liquid separator 15 in step 2
Gaseous phase outlet, 11 first inlet exhaust gas 34 of First Heat Exchanger, 111 first offgas outlet of First Heat Exchanger of gas-liquid separator 15
35, the import of the 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The gaseous phase outlet of first gas-liquid separator 15
Gas phase temperature: -47 DEG C, flow: 444Nm3/ h, gas phase fraction: 1；
Step 6: the liquid phase after 16 2 rectification and purifications of Second distillation column in step 4 passes through 16 bottom of Second distillation column
Liquid-phase outlet, the 8th regulating valve 23,11 second inlet exhaust gas 37 of First Heat Exchanger, First Heat Exchanger 111 the second tail gas go out
The import of mouth the 36, the 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The liquid-phase outlet of 16 bottom of Second distillation column
Liquidus temperature: -20 DEG C, flow: 22Nm3/ h, gas phase fraction: 0；
Step 7: circulating air in liquefied ammonia heat pump 22 by the circulating air outlet of liquefied ammonia heat pump 22 and the 7th regulating valve 7 into
Enter in the second threeway 28 and be divided into two strands, one circulating air passes through the first reboiler 13, the first throttle of 12 bottom of first rectifying column
Valve 8, the shell side of the second heat exchanger 14, the first circulation gas import 31 of First Heat Exchanger 14, First Heat Exchanger 14 first circulation
Gas outlet 32 and the global cycle gas import of liquefied ammonia heat pump 22 enter in liquefied ammonia heat pump 22, and another strand of circulating air passes through the second threeway 28
Third end, the second reboiler 17 of 16 bottom of Second distillation column, second throttle 9, the shell side of third heat exchanger 18, first change
Second circulation gas import 29, second circulation gas outlet 30 and the global cycle gas import of liquefied ammonia heat pump 22 of hot device 11 enter liquefied ammonia heat
In pump 22；The component of the circulating air: liquefied ammonia, liquefied ammonia molar fraction: 100%；The circulation temperature of the shell side of second heat exchanger 14
Degree: -50 DEG C, gas phase fraction: 0.9；The circulating air temperature of the shell side of third heat exchanger 18: -23 DEG C, gas phase fraction: 0.9；It is described
The circulation fluid temperature of first reboiler 13 outlet: -9 DEG C, gas phase fraction: 0；The circulation fluid temperature of second reboiler 17 outlet: -17
DEG C, the circulation fluid temperature that second throttle 9 exports: -23 DEG C.
Embodiment three
A kind of device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, including unstripped gas surge tank 10, product pump
19, products pot 20, liquefied ammonia heat pump 22 and desulfurizing tower 21, the unstripped gas surge tank 10 pass sequentially through the raw material of First Heat Exchanger 11
Raw material gas inlet, the first rectifying column of gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11,12 middle and lower part of first rectifying column
The first material liquid import 38, the outlet of 16 top gas phase of Second distillation column, third of the liquid-phase outlet, Second distillation column 16 of 12 bottoms
The tube side of heat exchanger 18, the first threeway 27 and product pump 19 are connected with products pot 20；The third end of first threeway 27 and the second essence
The the second material liquid import 33 for evaporating tower 16 is connected；The gaseous phase outlet at 12 top of first rectifying column passes through the tube side of the second heat exchanger 14
It is connected with the import of the first gas-liquid separator 15, liquid-phase outlet and 12 middle and upper part of first rectifying column of the first gas-liquid separator 15
Material liquid import is connected；The gaseous phase outlet of first gas-liquid separator 15 passes through 11 first inlet exhaust gas 34 and first of First Heat Exchanger
11 first offgas outlet 35 of heat exchanger is connected with the import of desulfurizing tower 21；The liquid-phase outlet of 16 bottom of Second distillation column passes through first
11 second inlet exhaust gas 37 of heat exchanger and 11 second offgas outlet 36 of First Heat Exchanger are connected with the import of desulfurizing tower 21；Liquefied ammonia heat
The circulating air outlet of pump 22 passes sequentially through the first reboiler 13, the second heat exchanger of the second threeway 28,12 bottom of first rectifying column
The first circulation gas import 31 of 14 shell side, First Heat Exchanger 14 and the first circulation gas outlet 32 of First Heat Exchanger 14 and liquefied ammonia
The global cycle gas import of heat pump 22 is connected；What the third end of the second threeway 28 passed sequentially through 16 bottom of Second distillation column second boils again
Device 17, the shell side of third heat exchanger 18, the second circulation gas import 29 of First Heat Exchanger 11 and First Heat Exchanger 11 second follow
Ring gas outlet 30 is connected with the global cycle gas import of liquefied ammonia heat pump 22.The original of the unstripped gas surge tank 10 and First Heat Exchanger 11
Expect to be equipped with the first regulating valve 1 between gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11 and 12 middle and lower part of first rectifying column
Raw material gas inlet between be equipped with the second regulating valve 2, the of the liquid-phase outlet of 12 bottom of first rectifying column and Second distillation column 16
Third regulating valve 3, the third end of the first threeway 27 and the second raw material of Second distillation column 16 are equipped between one material liquid import 38
It is equipped with the 4th regulating valve 4 between liquid import 33, the 5th regulating valve 5, desulfurizing tower 21 are equipped between the first threeway 27 and product pump 19
Entrance be equipped with the 6th regulating valve 6, liquefied ammonia heat pump 22 circulating air outlet the second threeway 28 between be equipped with the 7th regulating valve
7, between the first reboiler 13 of 12 bottom of first rectifying column and the shell side of the second heat exchanger 14 be equipped with first throttle valve 8, second
Second throttle 9, Second distillation column are equipped between the second reboiler 17 and the shell side of third heat exchanger 18 of 16 bottom of rectifying column
The 8th regulating valve 23 is equipped between 11 second inlet exhaust gas 37 of liquid-phase outlet and First Heat Exchanger of 16 bottoms.The product pump 19
The 9th regulating valve 26 is equipped between products pot 20.
A kind of production method of the device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, includes the following steps:
Step 1: the unstripped gas in unstripped gas surge tank 10 passes sequentially through the raw material of the first regulating valve 1, First Heat Exchanger 11
Gas import 24, the unstripped gas outlet 25 of First Heat Exchanger 11 enter in first rectifying columns 12, the main composition of the unstripped gas at
Part: carbon dioxide, hydrogen sulfide, methanol, nitrogen, carbon monoxide, carbonyl sulfur, sulfur dioxide, methane, ethane, ethylene, propane and
Propylene；The temperature of unstripped gas: 35~40 DEG C, pressure: 0.7Mpa, flow: 600Nm3/ h, gas phase fraction: 1, H2S molar fraction:
35%；The unstripped gas temperature of 11 unstripped gas of First Heat Exchanger outlet 25: -41 DEG C, gas phase fraction is 0.6, H2S molar fraction:
35%；
Step 2: make to enter in step 1 rectification and purification of unstripped gas progress, a rectifying in first rectifying column 12 and mention
Gas phase after pure enters the first gas-liquid separator by the tube side of the outlet of 12 top gas phase of first rectifying column and the second heat exchanger 14
Gas-liquid separation is carried out in 15, the liquid phase after gas-liquid separation passes through the liquid-phase outlet and first rectifying column 12 of the first gas-liquid separator 15
The material liquid import of middle and upper part enters in first rectifying column 12；The gas phase temperature of 12 top gas phase of the first rectifying column outlet :-
39 DEG C, H2S molar fraction: 10%；Entered in first rectifying column 12 by the material liquid import of 12 middle and upper part of first rectifying column
Liquidus temperature is -45 DEG C, H2S molar fraction: 25%, gas phase fraction: 0.
Step 3: enter the bottom liquid phases after first rectifying column 12 purifies in step 2 and enter the by third regulating valve 3
In two rectifying columns 16, the liquid-phase product temperature of the bottom liquid phases outlet of the first rectifying column 12: -10 DEG C, flow: 166Nm3/
H, H2S molar fraction: 99.9%；
Step 4: make to enter in step 3 the secondary rectification and purification of liquid phase progress, secondary rectification and purification in Second distillation column 16
Gas phase afterwards is entered in the first threeway 27 by the tube side of the outlet of 16 top gas phase of Second distillation column and third heat exchanger 18, into
The liquid phase entered in the first threeway 27 is divided into two strands, one liquid phase passes through the third end of the first threeway 27, the 4th regulating valve 4 and second
Second material liquid import 33 of rectifying column 16 enters in Second distillation column 16, and another burst of liquid phase is adjusted by the first threeway the 27, the 5th
Valve 5, product pump 19 and the 9th regulating valve 26 is saved to enter in products pot 20；The gas phase of 16 top gas phase of the Second distillation column outlet
Temperature: -19 DEG C, gas phase fraction: 1；Liquidus temperature in second material liquid import 33 of Second distillation column 16: -19 DEG C, gas phase point
Rate: 0；The liquidus temperature of 19 entrance of product pump: -19 DEG C, H2S product purity 99.9995%；
Step 5: first is passed sequentially through by the gas phase after progress gas-liquid separation in the first gas-liquid separator 15 in step 2
The gaseous phase outlet of gas-liquid separator 15,11 first inlet exhaust gas 34 of First Heat Exchanger, 11 first offgas outlet 35 of First Heat Exchanger,
The import of 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The gas of the gaseous phase outlet of first gas-liquid separator 15
Phase temperature: -45 DEG C, flow: 455Nm3/ h, gas phase fraction: 1；
Step 6: the liquid phase after 16 2 rectification and purifications of Second distillation column in step 4 passes through 16 bottom of Second distillation column
Liquid-phase outlet, the 8th regulating valve 23,11 second inlet exhaust gas 37 of First Heat Exchanger, First Heat Exchanger 11 the second offgas outlet
36, the import of the 6th regulating valve 6 and desulfurizing tower 21 enters in desulfurizing tower 21；The liquid-phase outlet of 16 bottom of Second distillation column
Liquidus temperature: -21 DEG C, flow: 25Nm3/ h, gas phase fraction: 0；
Step 7: circulating air in liquefied ammonia heat pump 22 by the circulating air outlet of liquefied ammonia heat pump 22 and the 7th regulating valve 7 into
Enter in the second threeway 28 and be divided into two strands, one circulating air passes through the first reboiler 13, the first throttle of 12 bottom of first rectifying column
Valve 8, the shell side of the second heat exchanger 14, the first circulation gas import 31 of First Heat Exchanger 14, First Heat Exchanger 14 first circulation
Gas outlet 32 and the global cycle gas import of liquefied ammonia heat pump 22 enter in liquefied ammonia heat pump 22, and another strand of circulating air passes through the second threeway 28
Third end, the second reboiler 17 of 16 bottom of Second distillation column, second throttle 9, the shell side of third heat exchanger 18, first change
Second circulation gas import 29, second circulation gas outlet 30 and the global cycle gas import of liquefied ammonia heat pump 22 of hot device 11 enter liquefied ammonia heat
In pump 22；The component of the circulating air: liquefied ammonia, liquefied ammonia molar fraction: 100%；The circulation temperature of the shell side of second heat exchanger 14
Degree: -48 DEG C, gas phase fraction: 0.9；The circulating air temperature of the shell side of third heat exchanger 18: -21 DEG C, gas phase fraction: 0.9；It is described
The circulation fluid temperature of first reboiler 13 outlet: -8 DEG C, gas phase fraction: 0；The circulation fluid temperature of second reboiler 17 outlet: -18
DEG C, the circulation fluid temperature that second throttle 9 exports: -21 DEG C.
The series of detailed descriptions listed above only for feasible embodiment of the invention specifically
Protection scope bright, that they are not intended to limit the invention, it is all without departing from equivalent implementations made by technical spirit of the present invention
Or change should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide, including unstripped gas surge tank (10), product pump
(19), products pot (20), liquefied ammonia heat pump (22) and desulfurizing tower (21), it is characterised in that: the unstripped gas surge tank (10) is successively
(25), first rectifying column are exported by the unstripped gas of the raw material gas inlet (24) of First Heat Exchanger (11), First Heat Exchanger (11)
(12) the first raw material of the liquid-phase outlet, Second distillation column (16) of raw material gas inlet, first rectifying column (12) bottom of middle and lower part
Liquid import (38), the outlet of Second distillation column (16) top gas phase, the tube side of third heat exchanger (18), the first threeway (27) and product
Pump (19) is connected with products pot (20)；The second material liquid import at the third end and Second distillation column (16) of the first threeway (27)
(33) it is connected；
Gaseous phase outlet at the top of first rectifying column (12) passes through the tube side and the first gas-liquid separator (15) of the second heat exchanger (14)
Import be connected, the liquid-phase outlet and the material liquid import phase of first rectifying column (12) middle and upper part of the first gas-liquid separator (15)
Even；The gaseous phase outlet of first gas-liquid separator (15) passes through (11) first inlet exhaust gas (34) of First Heat Exchanger and First Heat Exchanger
(11) first offgas outlets (35) are connected with the import of desulfurizing tower (21)；
The liquid-phase outlet of Second distillation column (16) bottom passes through (11) second inlet exhaust gas (37) of First Heat Exchanger and the first heat exchange
(11) second offgas outlet (36) of device is connected with the import of desulfurizing tower (21)；
The circulating air outlet of liquefied ammonia heat pump (22) passes sequentially through the second threeway (28), first rectifying column (12) bottom first is boiled again
Device (13), the shell side of the second heat exchanger (14), the first circulation gas import (31) of First Heat Exchanger (14) and First Heat Exchanger
(14) first circulation gas outlet (32) is connected with the global cycle gas import of liquefied ammonia heat pump (22)；The third end of second threeway (28)
Pass sequentially through second reboiler (17) of Second distillation column (16) bottom, shell side, the First Heat Exchanger of third heat exchanger (18)
(11) the second circulation gas outlet (30) and liquefied ammonia heat pump (22) of second circulation gas import (29) and First Heat Exchanger (11)
Global cycle gas import is connected.
2. a kind of device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide according to claim 1, feature exist
In: it is equipped with the first regulating valve (1) between the unstripped gas surge tank (10) and the raw material gas inlet (24) of First Heat Exchanger (11),
Second is equipped between the raw material gas inlet of unstripped gas outlet (25) and first rectifying column (12) middle and lower part of First Heat Exchanger (11)
Regulating valve (2), the first material liquid import (38) of the liquid-phase outlet and Second distillation column (16) of first rectifying column (12) bottom it
Between be equipped with third regulating valve (3), the second material liquid import (33) at the third end of the first threeway (27) and Second distillation column (16)
Between be equipped with the 4th regulating valve (4), equipped with the 5th regulating valve (5) between the first threeway (27) and product pump (19), desulfurizing tower
(21) entrance is equipped with the 6th regulating valve (6), is equipped between the circulating air outlet and the second threeway (28) of liquefied ammonia heat pump (22)
7th regulating valve (7) is set between first reboiler (13) of first rectifying column (12) bottom and the shell side of the second heat exchanger (14)
Have first throttle valve (8), between second reboiler (17) of Second distillation column (16) bottom and the shell side of third heat exchanger (18)
Equipped with second throttle (9), (11) second inlet exhaust gas of liquid-phase outlet and First Heat Exchanger of Second distillation column (16) bottom
(37) the 8th regulating valve (23) is equipped between.
3. a kind of device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide according to claim 1, feature exist
In: the 9th regulating valve (26) is equipped between the product pump (19) and products pot (20).
4. a kind of producer of the device with liquefied ammonia heat pump distillation mode of manufacture high-pure hydrogen sulfide as described in claim 1-3
Method, characterized by the following steps:
Step 1: the unstripped gas in unstripped gas surge tank (10) passes sequentially through the original of the first regulating valve (1), First Heat Exchanger (11)
Expect that gas import (24), the unstripped gas outlet (25) of First Heat Exchanger (11) are interior into first rectifying column (12), the unstripped gas
Main composition: carbon dioxide, hydrogen sulfide, methanol, nitrogen, carbon monoxide, carbonyl sulfur, sulfur dioxide, methane, ethane, second
Alkene, propane and propylene；The temperature of unstripped gas: 35~40 DEG C, pressure: 0.7Mpa, flow: 600Nm3/ h, gas phase fraction: 1, H2S
Molar fraction: 35%；First Heat Exchanger (11) unstripped gas exports the unstripped gas temperature of (25): -41~-45 DEG C, gas phase fraction is
0.6、H2S molar fraction: 35%；
Step 2: make to enter rectification and purification of first rectifying column (12) interior unstripped gas progress, a rectification and purification in step 1
Gas phase afterwards enters the first gas-liquid separation by the tube side of the outlet of first rectifying column (12) top gas phase and the second heat exchanger (14)
Gas-liquid separation is carried out in device (15), the liquid phase after gas-liquid separation passes through the liquid-phase outlet of the first gas-liquid separator (15) and the first essence
The material liquid import for evaporating tower (12) middle and upper part enters in first rectifying column (12)；First rectifying column (12) the top gas phase outlet
Gas phase temperature: -41~-39 DEG C, H2S molar fraction: 6~10%；By the material liquid of first rectifying column (12) middle and upper part into
The liquidus temperature that mouth enters in first rectifying column (12) is -48~-45 DEG C, H2S molar fraction: 20~25%, gas phase fraction: 0.
Step 3: the bottom liquid phases after entering first rectifying column (12) purification in step 2 enter the by third regulating valve (3)
In two rectifying columns (16), the liquid-phase product temperature of the bottom liquid phases outlet of the first rectifying column (12): -15~-10 DEG C, stream
Amount: 145~166Nm3/ h, H2S molar fraction: 99.5~99.9%；
Step 4: make to enter the secondary rectification and purification of Second distillation column (16) interior liquid phase progress in step 3, after secondary rectification and purification
Gas phase the first threeway (27) are entered by the outlet of Second distillation column (16) top gas phase and the tube side of third heat exchanger (18)
It is interior, it is divided into two strands into the liquid phase in the first threeway (27), one liquid phase passes through the third end of the first threeway (27), the 4th adjusting
Second material liquid import (33) of valve (4) and Second distillation column (16) enters in Second distillation column (16), and another burst of liquid phase passes through
First threeway (27), the 5th regulating valve (5), product pump (19) and the 9th regulating valve (26) enter in products pot (20)；Described
The gas phase temperature of two rectifying columns (16) top gas phase outlet: -19~-21 DEG C, gas phase fraction: 1；The second of Second distillation column (16)
Liquidus temperature in material liquid import (33): -19~-21 DEG C, gas phase fraction: 0；The liquidus temperature of product pump (19) entrance :-
19~-21 DEG C, H2S product purity is not less than 99.999%；
Step 5: the first gas is passed sequentially through by the gas phase after progress gas-liquid separation in the first gas-liquid separator (15) in step 2
Gaseous phase outlet, (11) first inlet exhaust gas (34) of First Heat Exchanger, (11) first tail gas of First Heat Exchanger of liquid/gas separator (15)
The import of outlet (35), the 6th regulating valve (6) and desulfurizing tower (21) enters in desulfurizing tower (21)；First gas-liquid separator
(15) gas phase temperature of gaseous phase outlet: -45~-48 DEG C, flow: 434~455Nm3/ h, gas phase fraction: 1；
Step 6: the liquid phase after Second distillation column (16) secondary rectification and purification in step 4 passes through Second distillation column (16) bottom
Liquid-phase outlet, the 8th regulating valve (23), (11) second inlet exhaust gas (37) of First Heat Exchanger, First Heat Exchanger (11) second
The import of offgas outlet (36), the 6th regulating valve (6) and desulfurizing tower (21) enters in desulfurizing tower (21)；The Second distillation column
(16) liquidus temperature of the liquid-phase outlet of bottom: -21~-18 DEG C, flow: 18~25Nm3/ h, gas phase fraction: 0；
Step 7: the circulating air in liquefied ammonia heat pump (22) passes through the circulating air outlet of liquefied ammonia heat pump (22) and the 7th regulating valve (7)
Into being divided into two strands in the second threeway (28), one circulating air by first reboiler (13) of first rectifying column (12) bottom,
First throttle valve (8), the shell side of the second heat exchanger (14), the first circulation gas import (31) of First Heat Exchanger (14), first are changed
The global cycle gas import of the outlet of first circulation gas (32) and liquefied ammonia heat pump (22) of hot device (14) enters in liquefied ammonia heat pump (22), separately
One circulating air passes through the third end of the second threeway (28), second reboiler (17), the second section of Second distillation column (16) bottom
Stream valve (9), the shell side of third heat exchanger (18), the second circulation gas import (29) of First Heat Exchanger (11), second circulation gas go out
The global cycle gas import of mouth (30) and liquefied ammonia heat pump (22) enters in liquefied ammonia heat pump (22)；The component of the circulating air: liquefied ammonia, liquid
Ammonia molar fraction: 100%；The circulating air temperature of the shell side of second heat exchanger (14): -48~-51 DEG C, gas phase fraction: 0.9；The
The circulating air temperature of the shell side of three heat exchangers (18): -21~-24 DEG C, gas phase fraction: 0.9；First reboiler (13) outlet
Circulation fluid temperature: -11~-8 DEG C, gas phase fraction: 0；The circulation fluid temperature of second reboiler (17) outlet: -18~-15 DEG C,
The circulation fluid temperature of second throttle (9) outlet: -21~-24 DEG C.
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