Classifications

• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
  • C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
  • C12N1/20—Bacteria; Culture media therefor
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
  • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
  • B01D53/047—Pressure swing adsorption
  • B01D53/0476—Vacuum pressure swing adsorption
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/102—Carbon
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/106—Silica or silicates
  • B01D2253/108—Zeolites
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2256/00—Main component in the product gas stream after treatment
  • B01D2256/12—Oxygen
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2256/00—Main component in the product gas stream after treatment
  • B01D2256/18—Noble gases
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2257/00—Components to be removed
  • B01D2257/10—Single element gases other than halogens
  • B01D2257/102—Nitrogen
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40001—Methods relating to additional, e.g. intermediate, treatment of process gas
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
  • B01D2259/40013—Pressurization
  • B01D2259/40015—Pressurization with two sub-steps
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
  • B01D2259/40013—Pressurization
  • B01D2259/40018—Pressurization with more than three sub-steps
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
  • B01D2259/4002—Production
  • B01D2259/40022—Production with two sub-steps
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
  • B01D2259/40028—Depressurization
  • B01D2259/4003—Depressurization with two sub-steps
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
  • B01D2259/40058—Number of sequence steps, including sub-steps, per cycle
  • B01D2259/40067—Seven
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
  • B01D2259/40058—Number of sequence steps, including sub-steps, per cycle
  • B01D2259/40069—Eight
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/402—Further details for adsorption processes and devices using two beds

Definitions

• the present invention relates to a method and an apparatus for separating a mixed gas.
• the present invention uses a mixed gas containing a plurality of components as a raw material gas, and a target product by a pressure difference adsorption method in which an impurity component in the raw material gas is selectively adsorbed by an adsorbent.
• the present invention relates to a method and an apparatus for separating a mixed gas for recovering gas.
• the method is suitable for removing unburned components in various source gases and recovering a product gas rich in argon, hydrogen, oxygen, nitrogen, low-boiling hydrocarbons, and the like.
• a method for separating a mixed gas by a pressure difference adsorption method and an apparatus therefor have been proposed, for example, in Japanese Patent Publication No. 42-2S164, Japanese Patent Publication No. 57-42367 or Japanese Patent Publication No. 57-50722.
• the product gas is collected using a pressure difference adsorption unit that includes an adsorption tower filled with an adsorbent and that sequentially repeats pressure adsorption operation and pressure reduction desorption operation as basic operations.
• a single pressure difference adsorption unit consisting of a plurality of adsorption towers is arranged, and feed gas of the same composition and the same purity is introduced in parallel into each adsorption tower.
• the pressurization operation for increasing the pressure of the adsorption tower in order to perform the pressure adsorption operation is based on the raw material gas or the movement of the gas remaining in the adsorption tower after the pressure adsorption operation is completed.
• the amount of product gas taken out could not be increased due to the large disturbance of the death zone due to the pressure rise in the adsorption tower.
• the separation of the mixed gas according to the prior art described above is as follows.When argon is recovered using a raw material gas composed of 70% argon and 30% nitrogen, the argon bluntness in the product gas is at most 95%. The argon recovery was also 3% for S. Products with an argon dullness exceeding 95% in the product gas could not be recovered.
• An object of the present invention is to provide a method and an apparatus for separating a mixed gas capable of recovering a product gas at a high degree of insensitivity. You.
• Another object of the present invention is to recover product gas in high yield.
• the first feature of the present invention is that pressure adsorption operation and pressure reduction
• the feed gas sequentially to separate the raw material gas and the purified gas.
• the adsorption operation and the desorption / desorption operation are performed sequentially, and the above purification is performed.
• the gas is separated to recover the concentrated purified gas and the pressure is reduced.
• the second feature of the present invention is that the raw material gas inlet and the purified gas
• An adsorption tower having an outlet and filled with an adsorbent
• Adsorption tower and the exhaust gas outlet connected to the adsorption tower Adsorption tower and the exhaust gas outlet connected to the adsorption tower
• a mixed gas separation device comprising:
• the present invention relates to various source gases containing a plurality of components and their sources.
• Adsorbents that improperly adsorb impurity components in feed gas Adsorbents that improperly adsorb impurity components in feed gas
• adsorbent synthetic zeolite 5 A (maximum diameter
• Argon has almost the same adsorption selectivity as oxygen.
• Product gas can be recovered.
• the product gas rich in Qin can be recycled.
• adsorbents for example, a molecular sieve that separates gas by the difference in gas adsorption rate, and air as the raw material gas are combined, the product gas rich in nitrogen is recovered.
• OMPI I can get it.
• Activated carbon was used as the adsorbent, and methane, ethane, and prono were used as raw material gases.
• mixed gas of hydrocarbons such as butane and butane
• higher boiling hydrocarbons are adsorbed and removed, and low boiling hydrocarbons such as methane or methane and ethane are removed.
• Product gas rich in mixed gas can be collected.
• the raw material gas is separated by the first-stage pressure difference adsorption unit, the purified gas is recovered, and the purified gas is successively introduced into the second and subsequent pressure difference adsorption units. Separation into concentrated purified gas, and the final concentrated purified gas is taken out as product gas, so the length of the adsorption zone in the adsorption tower can be shortened, and highly dull product gas can be obtained.
• the first-stage pressure difference adsorption unit the purified gas is recovered, and the purified gas is successively introduced into the second and subsequent pressure difference adsorption units. Separation into concentrated purified gas, and the final concentrated purified gas is taken out as product gas, so the length of the adsorption zone in the adsorption tower can be shortened, and highly dull product gas can be obtained.
• FIG. 1 is a system diagram of a mixed gas separation device when a two-stage pressure difference adsorption unit according to the present invention is used.
• FIG. 2 is a system diagram of a mixed gas separation device when three or more pressure difference adsorption units according to the present invention are used.
• FIGS. 3 and 4 are each a system diagram of a mixed gas separation device showing another embodiment of the present invention when a three-stage pressure difference adsorption unit is used.
• FIG. 5 and FIG. 6 are configuration diagrams of the mixed gas separation device according to the present invention.
• FIG. 7 is a graph showing the relationship between the argon concentration (C out) in the product gas and the argon recovery in the product according to the present invention in the case of argon and according to the conventional example. Best form
• Fig. 1 shows the system diagram of the mixed gas separation device when the two-stage pressure difference deposition units UA and UB are introduced.
• the pressurized raw material gas from piping 1 is supplied to the first-stage pressure difference adsorption unit UA to perform the adsorption treatment.
• the processing gas (purified gas) from the first stage pressure difference adsorption unit U ⁇ is directly supplied to the second stage pressure difference adsorption unit UB via the pipe 2A. Purified gas is again subjected to pressure adsorption treatment and concentrated in the second-stage pressure difference adsorption unit UB After purifying the purified gas, this concentrated purified gas is
• the first stage pressure difference adsorption unit U A The first stage pressure difference adsorption unit U A
• the second stage pressure difference The exhaust gas flowing through the pipe 3B from the adsorption unit UB is temporarily stored along the way, and then the first stage pressure difference It was confirmed that the method of feeding the dying unit UA could optimize both the pressure reduction operation and the buck desorption operation.
• the reservoir 4A in the exhaust gas passage of the second-stage pressure difference unit UB is a huge one.
• the reservoir uses a container whose volume can change according to the amount of exhaust gas.
• the pressurizing operation of the first-stage pressure difference adsorption unit UA includes (1) the operation using the exhaust gas of the second-stage pressure difference adsorption unit UB, and (2) the completion of the adsorption process. It is desirable to use a combination of three types, one based on the movement of residual gas in the tower, and the other (3) based on the source gas. In this case, the steps are usually performed in the order of (1), (2) and (3).
• the pressurizing operation may be performed in a plurality of times.
• the pressurizing operation using (1) is performed after the pressurizing operation using a part of the gas, and then the pressurizing operation using the remaining gas is performed (2).
• the power pressure operation using the raw material gas is performed.
• Part of the purified gas in the pressure adsorption operation of the pressure difference adsorption unit UA of the first stage may be used for the pressure operation of the unit UA.
• Exhaust gas from the pressure desorption operation of the second-stage pressure difference adsorption unit UB is returned to the first-stage pressure difference adsorption unit UA
• Fig. 2 shows a system diagram of a mixed gas separation device when three or more pressure adsorption units are used.
• the purified gas of the first stage pressure difference adsorption unit U A is piped.
• the concentrated purified gas of the pressure difference adsorption unit UB,... of the former stage is directly surrounded by the pressure difference units..., XIX of the latter stage via piping 2B,... respectively.
• the concentrated purified gas in the final stage is exhausted as product gas from the piping 2 X of the pressure difference adsorption unit UX in the final stage.
• the mixed gas separator a is effective for recovering a higher purity product gas in a high yield.
• the exhaust gas of the plurality of pressure difference adsorption units at the subsequent stage may be conveniently used for the operation of the pressure difference adsorption unit at the stage preceding them.
• the mixed gas separator equipped with the three-stage differential adsorption units UA, UB, and UC shown in Fig. 3 is composed of the second-stage differential pressure adsorption unit UB and the third-stage differential adsorption unit.
• the three-stage pressure difference adsorption unit UA shown in Fig. 4,
• the mixed gas separation device equipped with UB and UC uses the exhaust gas from the second-stage pressure difference adsorption unit U3 and the third-stage pressure difference adsorption unit UC to pipe 3B and pipe 3, respectively.
• the pressure difference in the first stage consisting of two adsorption towers A 1 and A 2
• Adsorption tower A 1 has switching valves 11 A 1, 12 A 1, and 13 A 1 in the lower piping, and switching valves 14 A 1, 15 A ⁇ in the upper piping.
• OMPI Vacuum pump provided at the outlet of 8 A, piping 9 A for connecting the switching valves 13 A 1 and 13 A 2, piping 9 for connecting the lower switching valves 12 A 1, 12 2 6 A and 3 A pipes are provided to exhaust the exhaust gas from the vacuum pump 6 A to the outside of the system.
• the adsorption tower B 1 has switching valves 1 1 B 1, L2B I, 13 B 1 in the lower piping, and switching valves 14 B 1, 15 B 1, in the upper piping.
• Drum tower B 2 has switching valves I 2 B 2, 13 B 2 in the lower piping, and switching valves 14 B 2, I ⁇ B 2, 16 B 2 in the upper piping, respectively. .
• the piping connecting the upper selector valve 15 B 1 and 15 B 2 7 mm, the upper selector valve 16 3 1 and 16 B 2 and the lower selector valve 13 B 1 and 13 B A pipe 8 ⁇ that communicates with 2, a pipe 9 ⁇ that communicates with the lower selector valve 12 B 1, 12 B 2, and a vacuum pump 6 ⁇ are provided at the outlet of the pipe 9 ⁇ .
• the two-stage pressure difference adsorption unit described above consists of the first-stage pressure difference adsorption unit, the source gas supply to the dying unit, the piping 1, the first-stage pressure difference adsorption unit, and the second-stage pressure difference adsorption unit. 2 ⁇ of purified gas delivery piping that communicates with the
• the product gas which is a concentrated purified gas, is dared from the adsorption unit.
• Table 1 shows the pressure difference death cycle for operating the mixed gas separator shown in Fig. 5.
• the operation is pressurization I-13 process and adsorption I process, the depressurization desorption operation is exhaust I process, the reflux pressurization operation is heating I-11 process, and the column equalization operation is equalization I process or pressurization. Each of them will be implemented in I-12 process.
• the pressure adsorption operation is pressurization ⁇ — 2 process and adsorption H process
• the depressurization desorption operation is the exhaust gas process
• the pressure equalization operation between columns is equal.
• the adsorption tower A 1 for the pressure difference adsorption unit in the L-th stage and the adsorption tower 31 for the pressure difference adsorption unit in the second stage are the following. Operate as follows.
• the raw material gas pressurized above the atmosphere from the pipe 1 is supplied to the deposition tower A 1 via the switching valve 11 A 1 to adsorb and remove the insoluble components and switch.
• the residual gas in the delicate tower A 1 after the adsorption I process is switched to the switching valve 15 A 1, the piping 7 A and the switching valve 15 A 2 line or the switching valve LA 1, and the piping 8 A And feed to adsorption tower A 2 via one of the lines of switching valve 13 A 2.
• the residual gas in the adsorption tower A 1 after the pressure equalization I process is passed through the switching valve 12 A 1 and the pipe 9 A.
• the adsorbent is regenerated by dying with the vacuum pump SA, and the gas discharged from the vacuum pump 6A is exhausted out of the system from the pipe 3A.
• the purified gas held in the reservoir 4 A is supplied to the adsorption tower A 1 after the exhaust I process, piping 5 A, switching valve 17 A, piping 1 OA and switching valve 16 It is supplied via A 1 and the pressure in adsorption tower A 1 is increased.
• the residual gas of the adsorption tower A2 is placed on the adsorption tower A after the pressurization I_1 step is completed, and the switching valve 15A2, piping 7A and switching valve 15A1 Or switching valve 16 A 2. Supply pressure via piping 8 A and the line of switching valve 13 A 1 to depressurize adsorption tower A 1.
• Step 3 is to pressurize the raw material gas pressurized to above atmospheric pressure from piping 1 to adsorption tower A1 after pressurization I-12 step is completed via switching valve 11 A1 Supply and raise the pressure at the death landing tower A 1.
• a switching valve is used to switch the purified gas from pipe 2A.
• the residual gas in the adsorption tower B 1 after the adsorption process has been switched is the switching valve 15 B 1, piping 7 B and the switching valve 15 B 2 line or switching valve 16 B 1, piping 8 B And switching valve 1 3 B 2
• Residual gas is transferred via switching valve 1 2 B 1 and piping 9 B
• the adsorbent is regenerated by suction with the vacuum pump 6B, and the vacuum pump
• the purpose is to make the purified gas discharged from the adsorption tower
• the length of the adsorption tower can be reduced and the processing amount can be reduced accordingly.
• the exhaust gas from the second-stage pressure differential adsorption unit can be used as a raw material for the first-stage pressure differential adsorption unit, so the loss of stray gas by the second-stage pressure differential adsorption unit Loss can be prevented.
• the gas purity in the exhaust gas from the second-stage pressure difference adsorption unit is sufficiently higher than that of the source gas, and this exhaust gas is subjected to the first-stage pressure difference adsorption unit under vacuum.
• the cycle is formed by using the reservoir, the adsorbent in the adsorption tower of the second-stage pressure difference adsorption unit is regenerated and the residual gas is recycled. Can be operated at different times from the pressurization I to 11 times, and the regeneration of the adsorbent can be efficiently performed by prolonging the time of the wandering ⁇ process. And the benefits of exhaust gas utilization.
• Table 2 shows an example of a pressure-diffusion cycle formed by the improved process.
• Adsorption to send purified gas from 14 A1 I 11 Process and sending out purified gas from changeover valve 14 A1 with switching valve 11 A1 closed and flooding of source gas stopped Adsorption I
• a relatively high-purity purified gas can be supplied from one end of the adsorption tower and a relatively low-purity source gas can be supplied from the other end of the adsorption tower.
• OMPI IPO helps to reduce the length of the adsorption zone of the adsorption tower.
• a relatively high-purity concentrated purified gas can be supplied from one end of the deposition tower, and a relatively low-duty purified gas can be supplied from the other end. Helps to reduce the length of the tower's adsorption.
• FIG. 1 Another embodiment of the apparatus for separating a mixed gas of the present invention will be described with reference to FIG.
• the configuration of this embodiment is shown in FIG. It has a configuration in which a flow controller is added to the piping of the device shown.
• flow controllers such as flow control valves and orifices 21, 22 A, 23 A, 24 A, 25 A, 22 A, 22
• Each of the adsorption towers A 1, A 2, B 1, and ⁇ 2 has a cylindrical shape with an inner diameter of 38 m and a packed bed height of 1.7 m.
• the column is filled with zeolite oA. I have.
• the internal volumes of reservoir 4A and product tank 18 are 5 ⁇ and 2 ⁇ , respectively.
• the composition of the source gas is argon 70. /. And nitrogen 30%, pressure 380.0 kPa, temperature 20. C.
• Q in is the amount of raw material gas flooded per cycle (N HI 3 )
• Q out is the amount of product gas removed per cycle (X m 3 )
• C in is the raw material gas.
• Cout is the purity of argon in product gas (%).
• Figure 7 shows the relationship between the argon purity (Cout) in the product gas and the argon recovery (") by a solid line.
• argon recovery was as high as 78% at an argon dullness of 990%.
• the argon recovery rate was 68 even when the argon purity was as high as 99.999%. As a result, high-purity argon-rich product gas could be recovered in high yield.
• Example B Air having a pressure of 250 kPa and a temperature of 20 was used as a source gas in the same apparatus and the same cycle as in Example A.

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• 1983
  • 1983-06-29 JP JP58115913A patent/JPS607920A/ja active Granted
• 1984
  • 1984-06-19 EP EP84902376A patent/EP0151186B1/en not_active Expired - Lifetime
  • 1984-06-19 US US07/020,179 patent/US4737167A/en not_active Expired - Fee Related
  • 1984-06-19 DE DE8484902376T patent/DE3484058D1/de not_active Expired - Lifetime
  • 1984-06-19 WO PCT/JP1984/000319 patent/WO1985000118A1/ja not_active Ceased
  • 1984-06-28 KR KR1019840003697A patent/KR880000803B1/ko not_active Expired
  • 1984-06-28 KR KR1019840003697A patent/KR850000255A/ko active Granted

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