CN112808223A - Reaction device for generating gaseous hydride on line - Google Patents
Reaction device for generating gaseous hydride on line Download PDFInfo
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- CN112808223A CN112808223A CN202011520508.6A CN202011520508A CN112808223A CN 112808223 A CN112808223 A CN 112808223A CN 202011520508 A CN202011520508 A CN 202011520508A CN 112808223 A CN112808223 A CN 112808223A
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- hydrogen
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- hydride
- connecting pipe
- gaseous hydride
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- 150000004678 hydrides Chemical class 0.000 title claims abstract description 85
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 72
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 105
- 239000001257 hydrogen Substances 0.000 claims abstract description 79
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 79
- 239000007789 gas Substances 0.000 claims abstract description 63
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 50
- 238000003860 storage Methods 0.000 claims description 35
- 229910052786 argon Inorganic materials 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 18
- 229910052711 selenium Inorganic materials 0.000 claims description 10
- 239000011669 selenium Substances 0.000 claims description 10
- 239000002808 molecular sieve Substances 0.000 claims description 9
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
- 238000009423 ventilation Methods 0.000 claims description 2
- 229910000058 selane Inorganic materials 0.000 abstract description 27
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 16
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract description 16
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 5
- 238000005485 electric heating Methods 0.000 description 4
- 239000002341 toxic gas Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000005987 sulfurization reaction Methods 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000012432 intermediate storage Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000013082 photovoltaic technology Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 150000003342 selenium Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
-
- 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
- B01D53/0407—Constructional details of adsorbing systems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- 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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00132—Controlling the temperature using electric heating or cooling elements
- B01J2219/00135—Electric resistance heaters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Abstract
The utility model relates to a reaction unit who generates gaseous state hydride on line, gaseous state hydride generation zone is located between hydrogen source ionization district and the gaseous state hydride reaction zone, the one end of casing is equipped with the air inlet with hydrogen source ionization district intercommunication, and the other end is equipped with the gas vent with hydride reaction zone intercommunication, the gas vent intercommunication has the first vacuum pump of carrying out evacuation processing to the casing inside, first vacuum pump intercommunication has tail gas processing mechanism, input gaseous hydrogen source in the air inlet, gaseous state hydride generation zone is equipped with elemental selenium or elemental sulfur, be equipped with the heating wire in the hydrogen source ionization district, gaseous state hydride reaction zone's temperature control is in 100 and is increased one's price 400 ℃, gaseous state hydride generation zone's temperature is higher than gaseous state hydride reaction zone's temperature. The reaction device for generating the gaseous hydride on line can improve the problems of safety and cost when hydrogen selenide or hydrogen sulfide needs to be transported and stored in the past.
Description
Technical Field
The application relates to the field of selenization reaction, in particular to a selenization reaction device for generating hydrogen selenide on line.
Background
The selenization (sulfurization) reaction is very key to the copper-indium-gallium-selenium and other photovoltaic technologies, and when elemental selenium (elemental sulfur) is used for selenization (sulfurization), a large number of selenium clusters (sulfur clusters) are easily formed and gathered on the surface of a sample, so that the further selenization (sulfurization) of the sample is influenced. Selenizing (sulfurizing) the sample by using hydrogen selenide (hydrogen sulfide) can effectively avoid the problems. However, both hydrogen selenide and hydrogen sulfide gases are toxic, and the transportation and storage of these toxic gases is both a safety and cost issue.
Disclosure of Invention
In order to improve the problems of safety and cost of hydrogen selenide or hydrogen sulfide during transportation and storage, the application provides a reaction device for generating gaseous hydride on line.
The reaction device for generating the gaseous hydride on line provided by the application adopts the following technical scheme:
a reaction device for generating gaseous hydride on line comprises a shell, wherein the shell comprises a hydrogen source ionization area, a gaseous hydride generation area and a gaseous hydride reaction area which are mutually communicated, the gaseous hydride generation area is positioned between the hydrogen source ionization area and the gaseous hydride reaction area, one end of the shell is provided with an air inlet communicated with the hydrogen source ionization area, the other end of the shell is provided with an air outlet communicated with the hydride reaction area, the air outlet is communicated with a first vacuum pump for vacuumizing the interior of the shell, the first vacuum pump is communicated with a tail gas treatment mechanism, the gaseous hydrogen source is input into the air inlet, the gaseous hydride generation area is provided with elemental selenium or elemental sulfur, the temperature in the hydrogen source ionization area is controlled by an electric heating wire, the temperature in the gaseous hydride generation area is controlled at 400 ℃ of 100-, the temperature of the gaseous hydride generation zone is higher than the temperature of the gaseous hydride reaction zone.
By adopting the technical scheme, a nontoxic gaseous hydrogen source directly enters the hydrogen source ionization area from the air inlet, the heating wire is electrified and heated to generate hydrogen free radicals, the hydrogen free radicals enter the gaseous hydride generation area to react with elemental selenium or elemental sulfur at high temperature to generate hydrogen selenide or hydrogen sulfide, the generated hydrogen selenide or hydrogen sulfide enters the gaseous hydride reaction area to selenize or sulfide a sample, and the reaction device can generate the hydrogen selenide or hydrogen sulfide on line, so that the safety and cost problems caused by transporting and storing the hydrogen sulfide or hydrogen selenide before the original selenization or sulfide reaction are effectively solved.
Optionally, a heat-insulating gas-permeable plate is arranged between the gaseous hydride generation region and the hydrogen source ionization region and between the gaseous hydride generation region and the gaseous hydride reaction region.
Through adopting above-mentioned technical scheme, thermal radiation influence between two adjacent regions can be reduced in the setting of thermal-insulated ventilative board.
Optionally, the heat-insulating gas-permeable plate comprises a plurality of first baffle plates and second baffle plates fixed in the shell, through holes for gas to pass through are formed between every two adjacent first baffle plates, the second baffle plates correspond to the through holes one to one, and the through holes are covered by the projection surfaces of the second baffle plates from the hydrogen source ionization region to the gaseous hydride reaction region.
Through adopting above-mentioned technical scheme, the air current can pass from the through-hole, but the heat radiation can block through first baffle and second baffle, and the thermal-insulated ventilation effect of such thermal-insulated ventilative board can be better.
Optionally, the tail gas treatment mechanism includes first box, the one end of first box is equipped with the intake pipe with first vacuum pump intercommunication, and the other end is equipped with the outlet duct, the first box intussuseption is filled with 4A molecular sieve.
Through adopting above-mentioned technical scheme, the gas of discharging into in the box can have hydrogen sulfide or hydrogen selenide toxic gas, and 4A molecular sieve in the box can adsorb hydrogen sulfide or hydrogen selenide for the toxic gas is difficult to be discharged in the air.
Optionally, a first heating plate is arranged in the first box body, the first box body is further communicated with a first connecting pipe, the other end of the first connecting pipe, which is opposite to the first box body, is communicated with a gaseous hydride gas storage tank, and the first connecting pipe, the gas outlet pipe and the gas inlet pipe are all provided with valve bodies.
Through adopting above-mentioned technical scheme, at the in-process of selenizing or vulcanizing, valve body on the first connecting pipe is closed, first hot plate also does not heat, thereby 4A molecular sieve in the box can normally adsorb hydrogen selenide or hydrogen sulfide, when reaction unit does not work, can close the valve body in outlet duct and the intake pipe, make first hot plate heat again, make hydrogen selenide or hydrogen sulfide resolve out from 4A molecular sieve and flow into gaseous hydride gas holder and store, such structure can carry out recycle to hydrogen selenide or hydrogen sulfide, and production cost is reduced.
Optionally, the gaseous hydrogen source input into the gas inlet is a mixed gas of hydrogen and argon.
By adopting the technical scheme, the argon and the hydrogen are mixed and enter the reaction device, so that the reaction is safer.
Optionally, the outlet duct intercommunication has the blending tank, the blending tank still communicates there is the second connecting pipe, the second connecting pipe is equipped with hydrogen tank for the other one end of blending tank, the second connecting pipe is connected with the second vacuum pump, the intercommunication has the third connecting pipe between blending tank and the air inlet, the second connecting pipe is connected with hydrogen concentration detector.
By adopting the technical scheme, the gas discharged from the box body contains hydrogen and argon, and the part of gas is further recycled, so that the production cost is further reduced.
Optionally, a middle storage tank is further communicated with the gas outlet pipe between the mixing tank and the first tank body, the middle storage tank is connected with a pressure release valve, the other end of the pressure release valve relative to the middle storage tank is connected with a 3A molecular sieve mechanism, a fourth connecting pipe is communicated between the 3A molecular sieve mechanism and the hydrogen tank, and the fourth connecting pipe is provided with a valve body.
Through adopting above-mentioned technical scheme, after the atmospheric pressure in the well storage tank risees to a definite value, in the gas in the well storage tank just can run into 3A molecular sieve mechanism through the relief valve, 3A molecular sieve mechanism can adsorb hydrogen to can retrieve the hydrogen that the pressure release came out, follow-up can recycle.
Optionally, the 3A molecular sieve machine includes the second box, the second box intussuseption is filled with the 3A molecular sieve, still be equipped with the second hot plate in the second box, the second box communicates with well storage tank and hydrogen jar respectively, the second box still communicates there is the fifth connecting pipe, the fifth connecting pipe has argon gas jar for the other end intercommunication of second box, the fifth connecting pipe is connected with the valve body.
By adopting the technical scheme, the valve body on the fourth connecting pipe is closed and the valve body on the fifth connecting pipe is opened in normal work, so that argon released from the storage tank can directly enter the argon tank; when reaction unit stop work, can open the valve body on the fourth connecting pipe to make the second hot plate heat, close the valve body on the fifth connecting pipe simultaneously, make the hydrogen that adsorbs in the 3A molecular sieve can resolve out and come to flow into and store in the hydrogen jar.
In summary, the present application includes at least one of the following beneficial technical effects:
the reaction device can generate hydrogen selenide or hydrogen sulfide on line, and the problems of safety and cost caused by the transportation and storage of hydrogen selenide or hydrogen sulfide in the prior art are solved.
The reaction device can recycle the generated hydrogen, argon, hydrogen selenide and hydrogen sulfide, and reduces the production cost.
Drawings
FIG. 1 is a schematic diagram of a gaseous hydride generation reaction mechanism in accordance with an embodiment.
FIG. 2 is a flow chart of the first embodiment.
FIG. 3 is a schematic structural diagram of an exhaust gas treatment mechanism according to the first embodiment.
FIG. 4 is a schematic diagram of the structure of the 3A molecular sieve mechanism of the first embodiment.
Fig. 5 is a schematic structural diagram of a selenium nest in accordance with the first embodiment.
Fig. 6 is a schematic structural diagram of a selenium nest in the second embodiment.
Description of reference numerals: 1. a housing; 2. a hydrogen ionization zone; 3. a gaseous hydride generation zone; 4. a gaseous hydride reaction zone; 5. an air inlet; 6. an exhaust port; 7. a first vacuum pump; 8. a tail gas treatment mechanism; 81. a first case; 82. an air inlet pipe; 83. an air outlet pipe; 84. 4A molecular sieve; 85. a first heating plate; 9. a selenium nest; 10. a first channel; 11. a heat-insulating air-permeable plate; 111. a first baffle plate; 112. a second baffle; 113. a through hole; 12. a first connecting pipe; 13. a gaseous hydride storage tank; 14. a valve body; 15. a mixing tank; 16. a second connecting pipe; 17. a hydrogen tank; 18. a second vacuum pump; 19. a third connecting pipe; 20. a hydrogen concentration detector; 21. a middle storage tank; 22. a pressure relief valve; 23. a 3A molecular sieve mechanism; 231. a second case; 232. a second heating plate; 233. a fifth connecting pipe; 234. an argon tank; 235. 3A molecular sieve; 24. a fourth connecting pipe; 25. a sample; 26. a vacuum gauge; 27. a gaseous hydride generating reaction mechanism; 28. a second channel; 29. an electrical heating rod; 30. a heating plate; 31. a through hole; 32. a sixth connecting pipe; 33. a seventh connecting pipe; 34. an electric heating wire.
Detailed Description
The present application is described in further detail below with reference to figures 1-6.
In a first embodiment, the present application discloses a reaction apparatus for generating a gaseous hydride on-line. Referring to fig. 1, the reaction device for generating gaseous hydride on line comprises a gaseous hydride generation reaction mechanism 27, the gaseous hydride generation reaction mechanism 27 further comprises a housing 1, the interior of the housing 1 is sequentially divided into a hydrogen source ionization region 2, a gaseous hydride generation region 3 and a gaseous hydride reaction region 4 from bottom to top, the bottom of the housing 1 is provided with an air inlet 5 communicated with the hydrogen source ionization region 2, and the top side wall of the housing 1 is provided with an air outlet 6 communicated with the gaseous hydride reaction region 4; a heating wire 34 is arranged in the hydrogen source ionization region 2, so that the temperature in the hydrogen source ionization region 2 is controlled to be more than 1000 ℃ (the preferred temperature is 1200 ℃); a selenium nest 9 is arranged in the gaseous hydride generation zone 3, and the temperature is controlled at 400 ℃ (the preferred temperature is 100 ℃, 200 ℃ and 400 ℃); an electric heating wire 34 is also installed in the gaseous hydride reaction zone 4 so that the temperature of the gaseous hydride reaction zone 4 is controlled at 100 ℃ to 400 ℃ (preferably at 100 ℃, 170 ℃ and 400 ℃). A hydrogen source (the hydrogen source may be hydrogen gas, hydrogen nitride, hydrogen chloride, or a mixture thereof) is introduced into the gas inlet 5, the hydrogen source in this embodiment is a mixture of 90% argon gas and 10% hydrogen gas, the sample 25 to be selenized is first placed into the gaseous hydride reaction region 4, the hydrogen gas enters the hydrogen source ionization region 2 and generates hydrogen radicals after high temperature, the hydrogen radicals then enter the gaseous hydride generation region 3 and react with elemental selenium at high temperature to generate hydrogen selenide, and the generated hydrogen selenide then enters the gaseous hydride reaction region 4 to selenize the sample 25.
Referring to fig. 1, heat-insulating gas-permeable plates 11 are respectively arranged between the gaseous hydride generation region 3 and the hydrogen source ionization region 2 and between the gaseous hydride generation region 3 and the gaseous hydride reaction region 4, and the heat-insulating gas-permeable plates 11 can reduce the influence of heat radiation between the two adjacent regions. The heat-insulating air-permeable plate 11 comprises a plurality of first baffle plates 111 fixed on the inner wall of the shell 1, in the embodiment, the first baffle plates 111 are arranged into four blocks, the four first baffle plates 111 are located on the same horizontal plane, and a through hole 113 is formed between two adjacent first baffle plates 111, a plurality of second baffle plates 112 are further arranged in the shell 1, in the embodiment, the second baffle plates 112 are arranged into two layers, two layers of the second baffle plates 112 are respectively located on the upper side and the lower side of the first baffle plates 111, each layer is provided with 4 blocks, and the two layers of the second baffle plates 112 correspond to each other up and down, the through hole 113 is covered by the orthographic projection of the second baffle plates 112, so that the heat-.
Referring to fig. 1 and 2, a first vacuum pump 7 for pumping air from the inside of the housing 1 is installed at the exhaust port 6, a vacuum gauge 26 for monitoring the air pressure inside the housing 1 is also installed on the housing 1, and the air pressure inside the housing 1 is smaller than 100Pa by the first vacuum pump 7, so that the toxic gas is not easy to leak. And a tail gas treatment mechanism 8 is further installed at one end of the first vacuum pump 7 for exhausting, and the tail gas treatment mechanism 8 can remove hydrogen selenide gas in the airflow.
Referring to fig. 2 and 3, the exhaust gas treatment mechanism 8 includes a first tank 81, an inlet pipe 82 connected to the first vacuum pump 7 is provided at the left end of the first tank 81, an outlet pipe 83 is provided at the other end, a 4A molecular sieve 84 is filled in the first box body 81, four first heating plates 85 are also arranged in the first box body 81, a bent first channel 10 is formed between the four first heating plates 85 and the inner wall of the first box body 81, the left end of the first channel 10 is connected with an air inlet pipe 82, the other end is connected with an air outlet pipe 83, the first box 81 is also communicated with a first connecting pipe 12, the first connecting pipe 12 comprises four branch pipes, the four branch pipes are all communicated with the first box 81, the four branch pipes, the air outlet pipe 83 and the air inlet pipe 82 are all provided with valve bodies 14, the valve bodies 14 are electromagnetic valves, a gaseous hydride storage tank 13 is provided at the other end of the first connection pipe 12 with respect to the first tank 81. When the reaction apparatus stops operating, the valve bodies 14 on the gas outlet pipe 83 and the gas inlet pipe 82 can be closed, the valve body 14 on the first connecting pipe 12 is opened, and the first heating plate 85 is energized and heated, so that the hydrogen selenide adsorbed in the 4A molecular sieve 84 can be analyzed out and flows into the gaseous hydride gas storage tank 13 for storage, and the first connecting pipe 12 can be provided with a vacuum pump. A sixth connecting pipe 32 is further communicated between the gaseous hydride gas storage tank 13 and the shell 1, and a valve body 14 is arranged on the sixth connecting pipe 32, so that the collected hydrogen selenide can be directly used in the shell 1.
Referring to fig. 2 and 3, a middle storage tank 21 is disposed at the other end of the gas outlet pipe 83 opposite to the first tank 81, the middle storage tank 21 is further communicated with a mixing tank 15, the mixing tank 15 is communicated with the gas inlet 5 of the housing 1 to form a third connecting pipe 19, a hydrogen concentration detector 20 and a valve body 14 are mounted on the third connecting pipe 19, an external hydrogen source pipeline is communicated with the third connecting pipe 19, a hydrogen tank 17 is further included in the reaction device for generating gaseous hydride on line, a second connecting pipe 16 is communicated between the hydrogen tank 17 and the mixing tank 15, and the valve body 14 and a second vacuum pump 18 are mounted on the second connecting pipe 16. Contain hydrogen and argon gas in the gas of back processing back through tail gas processing mechanism 8, hydrogen reduces after the reaction after content, and hydrogen in the hydrogen tank 17 can be mended into blending tank 15, and hydrogen concentration detector 20 can carry out hydrogen content detection to the gas that blending tank 15 flows out, lets in again in casing 1 after reaching the standard to make and to utilize exhaust hydrogen and argon gas once more.
Referring to fig. 2 and 4, a pressure relief valve 22 is further installed on the intermediate storage tank 21, the pressure relief valve 22 is communicated with a 3A molecular sieve mechanism 23, the 3A molecular sieve mechanism 23 includes a second tank 231 communicated with the pressure relief valve 22, a fourth connecting pipe 24 is communicated between the second tank 231 and the hydrogen tank 17, the second tank 231 is further communicated with a fifth connecting pipe 233, an argon tank 234 is communicated with the fifth connecting pipe 233, a valve body 14 and a pump body are respectively arranged on the fourth connecting pipe 24 and the fifth connecting pipe 233, the second tank 231 is filled with the 3A molecular sieve 235, four second heating plates 232 are further arranged in the second tank 231, a curved second channel 28 is formed between the four second heating plates 232 and the inner wall of the second tank 231, the left end of the second channel 28 is connected with the fourth connecting pipe 24, and the other end of the second channel is connected with the pressure relief valve 22. The fifth connection pipe 233 includes four branched pipes, and the four branched pipes are all communicated with the second case 231. During the operation of the reaction apparatus, the valve body 14 on the fourth connection pipe 24 is closed, the valve body 14 on the fifth connection pipe 233 is opened, when the pressure in the middle storage tank 21 is too high, the gas in the middle storage tank 21 can flow into the second tank 231 through the pressure release valve 22, the 3A molecular sieve 235 in the second tank 231 can adsorb hydrogen, and the argon can flow into the argon tank 234 for storage; when the reaction apparatus stops operating, valve 14 on fourth connecting pipe 24 may be opened, valve 14 on fifth connecting pipe 233 may be closed, and second heating plate 232 may be electrically heated, so that hydrogen adsorbed in 3A molecular sieve 235 may be desorbed and pumped into hydrogen tank 17 for storage. A seventh connecting pipe 33 is communicated between the argon tank 234 and the housing 1, a valve body 14 is arranged on the seventh connecting pipe 33, and after the sample 25 is installed, the valve body 14 on the seventh connecting pipe 33 can be opened, so that the argon in the argon tank 234 can be introduced into the housing 1, and the gas in the housing 1 can be discharged.
Referring to fig. 5, the cross section of the selenium nest 9 is circular, a plurality of electric heating rods 29 are inserted into the selenium nest 9, and a plurality of through holes 31 are further formed in the selenium nest 9, so that the hydrogen radicals and the elemental selenium can react more fully.
The implementation principle of the reaction device for generating the gaseous hydride on line in the embodiment of the application is as follows: when the reaction device works for a plurality of times, a sample 25 to be selenized can be placed into the gaseous hydride reaction zone 4, after a nontoxic external hydrogen source enters the shell 1 from the air inlet 5 and exhausts the air inside the shell 1, the heating wire 34 and the heating rod inside the shell 1 are electrified and heated, hydrogen can generate hydrogen free radicals after the heating wire 34, the hydrogen free radicals enter the gaseous hydride generation zone 3 to react with elemental selenium at high temperature to generate hydrogen selenide, and the generated hydrogen selenide enters the gaseous hydride reaction zone 4 again to selenize the sample 25; the gas discharged from the gas outlet 6 contains hydrogen selenide, argon gas and hydrogen gas, the hydrogen selenide can be removed after passing through the tail gas treatment mechanism 8, the hydrogen gas and the argon gas can be introduced into the middle storage tank 21, the pressure in the middle storage tank 21 can be greater than the external atmospheric pressure, the hydrogen gas and the argon gas in the middle storage tank 21 subsequently flow into the mixing tank 15, meanwhile, the hydrogen gas in the hydrogen tank 17 is supplemented into the mixing tank 15, the mixed hydrogen gas and the argon gas are introduced into the shell 1 for reuse, when the pressure in the middle storage tank 21 is too high, the gas in the middle storage tank 21 flows into the second box 231 through the pressure release valve 22, the 3A molecular sieve 235 in the second box 231 can adsorb the hydrogen gas, and the argon gas can be pumped into the argon gas tank 234, and the cycle is carried out; when the reaction device stops working, the gas outlet pipe 83, the valve body 14 on the fifth connecting pipe 233 and the gas inlet pipe 82 can be closed, and then the first heating plate 85 and the second heating plate 232 are heated, so that hydrogen selenide can be analyzed from the 4A molecular sieve 84 to flow into the gaseous hydride gas storage tank 13 for storage, hydrogen can be analyzed from the 3A molecular sieve 235 to be pumped into the hydrogen tank 17 for storage, and then the outside hydrogen source is not needed to be introduced after enough gas exists in the reaction device, and the gas in the reaction device can be recycled.
The selenium nest 9 inside the housing 1 can be directly replaced by a sulfur nest so that the sample 25 can be subjected to a vulcanization reaction.
The second embodiment is mainly different from the first embodiment in that: inserted in the selenium nest 9 are a plurality of heating plates 30, and the heating plates 30 are heated electrically.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (9)
1. A reaction apparatus for on-line generation of a gaseous hydride, characterized by: including casing (1), casing (1) is inside including hydrogen source ionization district (2), gaseous state hydride generation district (3) and gaseous hydride reaction zone (4) that communicate each other, gaseous state hydride generation district (3) are located between hydrogen source ionization district (2) and gaseous hydride reaction zone (4), the one end of casing (1) is equipped with air inlet (5) with hydrogen source ionization district (2) intercommunication, and the other end is equipped with gas vent (6) with hydride reaction zone intercommunication, gas vent (6) intercommunication has first vacuum pump (7) to casing (1) inside evacuation processing, first vacuum pump (7) intercommunication has tail gas processing mechanism (8), input gaseous hydrogen source in air inlet (5), gaseous state hydride generation district (3) are equipped with selenium or elemental sulfur, be equipped with heating wire (34) in hydrogen source ionization district (2), the temperature of the gaseous hydride generation zone (3) is controlled to be 100-400 ℃, the temperature of the gaseous hydride reaction zone (4) is controlled to be 100-400 ℃, and the temperature of the gaseous hydride generation zone (3) is higher than that of the gaseous hydride reaction zone (4).
2. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 1, wherein: and heat-insulating air-permeable plates (11) are arranged between the gaseous hydride generation region (3) and the hydrogen source ionization region (2) and between the gaseous hydride generation region (3) and the gaseous hydride reaction region (4).
3. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 2, wherein: the heat-insulating ventilation plate (11) comprises a plurality of first baffle plates (111) and second baffle plates (112) which are fixed in a shell (1), through holes (113) for gas to pass through are formed between every two adjacent first baffle plates (111), the second baffle plates (112) correspond to the through holes (113) one by one, and the through holes (113) are covered by the projection surfaces of the second baffle plates (112) from a hydrogen ionization area (2) to a gaseous hydride reaction area (4).
4. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 1, wherein: tail gas treatment mechanism (8) include first box (81), the one end of first box (81) is equipped with intake pipe (82) with first vacuum pump (7) intercommunication, and the other end is equipped with outlet duct (83), first box (81) intussuseption is filled with 4A molecular sieve (84).
5. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 4, wherein: be equipped with first hot plate (85) in first box (81), first box (81) still communicates first connecting pipe (12), first connecting pipe (12) communicate for the other one end of first box (81) have gaseous state hydride gas holder (13), first connecting pipe (12), outlet duct (83) and intake pipe (82) all are equipped with valve body (14).
6. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 5, wherein: the gaseous hydrogen source input into the gas inlet (5) is a mixed gas of hydrogen and argon.
7. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 6, wherein: outlet duct (83) intercommunication has blending tank (15), blending tank (15) still intercommunication has second connecting pipe (16), second connecting pipe (16) are equipped with hydrogen tank (17) for the other one end of blending tank (15), second connecting pipe (16) are connected with second vacuum pump (18), the intercommunication has third connecting pipe (19) between blending tank (15) and air inlet (5), second connecting pipe (16) are connected with hydrogen concentration detector (20).
8. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 7, wherein: still communicate on outlet duct (83) between blending tank (15) and first box (81) well storage tank (21), well storage tank (21) are connected with relief valve (22), relief valve (22) are connected with 3A molecular sieve mechanism (23) for the other one end of well storage tank (21), the intercommunication has fourth connecting pipe (24) between 3A molecular sieve mechanism (23) and hydrogen tank (17), fourth connecting pipe (24) are equipped with valve body (14).
9. A reaction apparatus for the on-line generation of a gaseous hydride according to claim 8, wherein: the 3A molecular sieve (235) machine comprises a second box body (231), the second box body (231) is filled with the 3A molecular sieve (235), a second heating plate (232) is further arranged in the second box body (231), the second box body (231) is respectively communicated with the middle storage tank (21) and the hydrogen tank (17), the second box body (231) is further communicated with a fifth connecting pipe (233), the fifth connecting pipe (233) is communicated with an argon tank (234) relative to the other end of the second box body (231), and the fifth connecting pipe (233) is connected with a valve body (14).
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