CN111039294A - Automatic 6N-level high-purity silicon tetrafluoride purification device and purification method - Google Patents
Automatic 6N-level high-purity silicon tetrafluoride purification device and purification method Download PDFInfo
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- CN111039294A CN111039294A CN201911353383.XA CN201911353383A CN111039294A CN 111039294 A CN111039294 A CN 111039294A CN 201911353383 A CN201911353383 A CN 201911353383A CN 111039294 A CN111039294 A CN 111039294A
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- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000000746 purification Methods 0.000 title claims abstract description 28
- 238000001179 sorption measurement Methods 0.000 claims abstract description 53
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 21
- 239000010959 steel Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims description 23
- 238000012856 packing Methods 0.000 claims description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 17
- 229910000792 Monel Inorganic materials 0.000 claims description 16
- 239000003463 adsorbent Substances 0.000 claims description 15
- 239000002808 molecular sieve Substances 0.000 claims description 14
- 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 14
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 71
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- -1 potassium silicate ester Chemical class 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
- C01B33/10784—Purification by adsorption
-
- 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
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- 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
- B01D53/0454—Controlling adsorption
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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
- B01J19/0006—Controlling or regulating processes
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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
- B01J19/30—Loose or shaped packing elements, e.g. Raschig rings or Berl saddles, for pouring into the apparatus for mass or heat transfer
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10705—Tetrafluoride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
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- 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
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2047—Hydrofluoric acid
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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Abstract
The invention discloses a 6N-level high-purity silicon tetrafluoride automatic purification device and a purification method, and belongs to the technical field of gas purification. The device comprises: the adsorption tower, remove light tower, remove heavy tower, gas detector, signal reception and feedback device, controller, circulation pipeline, fill dress pneumatic valve, circulation pneumatic valve, fill dress steel bottle and raw materials steel bottle. The method comprises the following steps: (1) setting the temperature of the adsorption tower as follows, and introducing silicon tetrafluoride gas; (2) the adsorbed silicon tetrafluoride gas enters a light component removing tower and a heavy component removing tower in sequence; (3) the gas detector detects the purity of the silicon tetrafluoride gas from the de-weighting tower, sends a signal to the receiving and feedback device, and sends an instruction whether to start the circulating pipeline to the controller. The device saves manpower, reduces production cost, improves working efficiency and is easy to realize industrial production; the purity of 95-99 percent of silicon tetrafluoride gas can be improved to more than 6N grade.
Description
Technical Field
The invention belongs to the technical field of gas purification, and particularly relates to a 6N-grade high-purity silicon tetrafluoride automatic purification device and a purification method.
Background
The silicon tetrafluoride has wide application fields and can be used as a hardening agent, a photosensitizer, electronic grade silane or polycrystalline silicon and the like for producing high-purity quartz glass, solar cells, a photosensitive drum of a copying machine, fluosilicic acid, aluminum fluoride, magnesium fluoride, potassium silicate ester, ammonium bifluoride, electronic materials, cement and marble. Silicon tetrafluoride is mainly used in the fields of electronics and semiconductors for etching agents of silicon nitride, tantalum silicide, and the like, P-type dopants, epitaxial deposition diffusion silicon sources, and the like. The processes for preparing silicon tetrafluoride which have been disclosed in the prior documents include a method for synthesizing a fluorine-containing substance and a silicon-containing substance, a pyrolysis method, a sulfuric acid method, a hydrofluoric acid method, and the like.
With the continuous development of the integrated circuit industry, the requirement on the purity of the electronic gas is increasingly improved, and the impurity index is from 10-6To 10-9Even higher purity is developed, and the crude silicon tetrafluoride prepared by the existing preparation method cannot meet the use requirement, so that purification treatment is required. Due to different preparation methodsThe types of impurities are different, and many purification methods adopted in the prior art include a rectification method, an adsorption method, a freezing method, a fluorination method, a catalysis method, an ion exchange method and the like.
However, with respect to the common process, on one hand, the purification effect is not good, the removal effect is not stable, the cost is high, and it is difficult to completely remove hydrogen fluoride and organic impurities in the silicon tetrafluoride gas; on the other hand, once the filling analysis monitoring index does not meet the requirement in the filling process, the unqualified gas can only be filled continuously, so that the qualified steel cylinder is polluted, the unqualified gas filled in the steel cylinder has to be returned to the system for re-feeding, the manpower waste and the financial waste are caused, and the rectification efficiency is greatly reduced.
Disclosure of Invention
In view of the above, the present invention provides an automatic purification apparatus and a purification method for 6N-grade high-purity silicon tetrafluoride. The device of the invention saves manpower, reduces production cost, improves working efficiency, is beneficial to product quality control, and is easy to realize industrial production; the method can improve the purity of 95-99 percent of silicon tetrafluoride gas to more than 6N level.
The purpose of the invention is realized by the following technical scheme:
an automated 6N-grade high-purity silicon tetrafluoride purification apparatus, the apparatus comprising: the adsorption tower, remove light tower, remove heavy tower, gas detector, signal reception and feedback device, controller, circulation pipeline, fill dress pneumatic valve, circulation pneumatic valve, fill dress steel bottle and raw materials steel bottle.
The connection relationship is as follows: the raw material steel cylinder, the adsorption tower, the light removing tower, the heavy removing tower, the gas detector, the filling pneumatic valve and the filling steel cylinder are sequentially connected through pipelines; one end of a circulating pipeline is connected to a pipeline between the raw material steel cylinder and the adsorption tower, the other end of the circulating pipeline is connected to a pipeline between the gas detector and the charging pneumatic valve, and the circulating pipeline is connected with the circulating pneumatic valve; the signal receiving and feedback device is respectively connected with the gas detector and the controller, and the controller is also connected with the filling pneumatic valve and the circulating pneumatic valve and used for controlling the opening and closing of the filling pneumatic valve and the circulating pneumatic valve.
And the tower body of the adsorption tower is filled with an adsorbent.
The gas detector, the signal receiving and feedback device, the controller, the circulating pipeline, the filling pneumatic valve and the circulating pneumatic valve form a filling system, the filling system is used for detecting the purity index of the silicon tetrafluoride, and automatic switching of the filling state of the silicon tetrafluoride is realized according to the detection result.
Preferably, the light-weight removing tower and the heavy-weight removing tower are packed towers.
Preferably, the tower bodies of the adsorption tower, the light-weight removal tower and the heavy-weight removal tower are made of monel.
Preferably, the packing used in the light and heavy removal columns is structured packing.
Wherein, the material of the regular packing is Monel.
A6N-grade high-purity silicon tetrafluoride automatic purification method comprises the following steps:
(1) setting the temperature of an adsorption tower at 50-70 ℃, and introducing silicon tetrafluoride gas from the bottom of the adsorption tower; the silicon tetrafluoride gas flows from bottom to top and is fully contacted with the adsorbent in the adsorption tower to remove hydrogen fluoride and trace organic matters in the silicon tetrafluoride gas;
(2) the adsorbed silicon tetrafluoride gas sequentially enters a light component removing tower and a heavy component removing tower to respectively remove light component impurities and heavy component impurities;
(3) the gas detector detects the purity of the silicon tetrafluoride gas from the de-heavy tower, and sends the purity index information detected by the gas detector to the signal receiving and feedback device, and the signal receiving and feedback device sends an instruction whether to start the circulating pipeline to the controller;
if the purity index of the silicon tetrafluoride gas does not meet the filling requirement, the controller sends a control instruction, closes the filling pneumatic valve, opens the circulating pneumatic valve, namely stops the filling operation, and starts the internal circulation operation of the circulating pipeline; and if the purity index of the silicon tetrafluoride gas meets the filling requirement, the controller sends a control instruction, closes the circulating pneumatic valve, opens the filling pneumatic valve and continues normal filling operation.
And (3) performing internal circulation operation, namely specifically, returning the silicon tetrafluoride gas which does not meet the filling requirement to the adsorption tower through a circulation pipeline, repeating the steps (1) to (3), and adjusting each process parameter.
Preferably, the flow rate of the silicon tetrafluoride gas introduced in the step (1) is 5-30 Kg/h, and the purity is 95-99%.
Further, the flow rate of the silicon tetrafluoride gas introduced in the step (1) is 20-30 Kg/h.
Preferably, the adsorbent in the adsorption tower 1 in the step (1) is a mixture of a molecular sieve and hollow activated carbon fibers, wherein the mass ratio of the molecular sieve to the hollow activated carbon fibers is 1: 3.
Further, the molecular sieve is a 5A molecular sieve, the inner diameter of the hollow activated carbon fiber is 30um, and the wall thickness is 8 um.
Preferably, the temperature of the light-weight removal tower in the step (2) is-140 to-120 ℃, and the pressure is 0.2 to 0.3 MPa.
Preferably, the temperature of the weight removing tower in the step (2) is-135 to-115 ℃, and the pressure is 0.1 to 0.2 MPa.
The requirement for achieving filling in the step (3) means that the requirement for achieving the purity of 6N-grade high-purity silicon tetrafluoride gas is met, and specifically comprises the following steps: h2<0.5ppm,O2<0.5ppm,N2<0.5ppm,CO<0.3ppm,CO2<0.5ppm,CH4Less than 0.1ppm and HF less than 0.2 ppm. If any one of the purity requirement indexes is not met, the filling requirement is not met.
The invention has the following beneficial effects:
(1) the method for purifying the silicon tetrafluoride can improve the purity of 95-99% of the silicon tetrafluoride gas to 99.9999%, namely the purity requirement of 6N-grade high-purity silicon tetrafluoride gas.
(2) The adsorption tower provided by the invention adopts a 5A molecular sieve and hollow activated carbon fiber mixture as filler, has strong selectivity and adsorptivity, and can remove acidity, trace organic matters and other impurities in silicon tetrafluoride.
(3) The filling system is provided with the gas detector, the controller and the internal circulation pipeline, the switching of the filling state can be automatically realized according to the detection index of the gas detector, once the filling index is found to be unqualified, the filling can be immediately stopped, the internal circulation is started, the filling is continuously started until the filling exhaust is qualified through the internal circulation, the operation and the quality control are facilitated, the labor is saved, the production cost is reduced, and the production efficiency is greatly improved.
Drawings
FIG. 1 is a schematic diagram of the mechanism of the device of the present invention.
The system comprises an adsorption tower 1, a light removing tower 2, a heavy removing tower 3, a gas detector 4, a signal receiving and feedback device 5, a controller 6, a circulating pipeline 7, a charging pneumatic valve 8, a circulating pneumatic valve 9, a charging steel cylinder 10 and a raw material steel cylinder 11.
Detailed Description
The invention is described in detail below by way of example with reference to the accompanying drawings.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the experimental materials and equipment, unless otherwise specified, are commercially available.
An automatic purification device of 6N-grade high-purity silicon tetrafluoride, as shown in FIG. 1, comprises: the device comprises an adsorption tower 1, a light-weight removing tower 2, a heavy-weight removing tower 3, a gas detector 4, a signal receiving and feedback device 5, a controller 6, a circulating pipeline 7, a charging pneumatic valve 8, a circulating pneumatic valve 9, a charging steel cylinder 10 and a raw material steel cylinder 11.
The connection relationship is as follows: a raw material steel cylinder 11, an adsorption tower 1, a light removing tower 2, a heavy removing tower 3, a gas detector 4, a charging pneumatic valve 8 and a charging steel cylinder 10 are sequentially connected by pipelines; one end of a circulating pipeline 7 is connected to a pipeline between the raw material steel cylinder 11 and the adsorption tower 1, the other end of the circulating pipeline is connected to a pipeline between the gas detector 4 and the charging pneumatic valve 8, and a circulating pneumatic valve 9 is connected in the circulating pipeline 7; the signal receiving and feedback device 5 is respectively connected with the gas detector 4 and the controller 6, and the controller 6 is also connected with the filling pneumatic valve 8 and the circulating pneumatic valve 9 for controlling the opening and closing of the filling pneumatic valve 8 and the circulating pneumatic valve 9.
And an adsorbent is arranged in the tower body of the adsorption tower 1.
And the gas detector 4, the signal receiving and feedback device 5, the controller 6, the circulating pipeline 7, the filling pneumatic valve 8 and the circulating pneumatic valve 9 form a filling system for detecting the purity index of the silicon tetrafluoride and realizing automatic switching of the filling state of the silicon tetrafluoride according to the detection result.
Preferably, the light-weight removal tower 2 and the heavy-weight removal tower 3 are packed towers.
Preferably, the tower bodies of the adsorption tower 1, the light-weight removal tower 2 and the heavy-weight removal tower 3 are made of monel.
Preferably, the packing used in the light-weight removal column 2 and the heavy-weight removal column 3 is structured packing.
Wherein, the material of the regular packing is Monel.
Example 1
Firstly, setting the temperature of a silicon tetrafluoride feeding adsorption tower to be 50 ℃, introducing silicon tetrafluoride gas with the purity of 95% from the bottom of the adsorption tower, wherein the gas flow is 30Kg/h, and the silicon tetrafluoride gas flows from bottom to top and is fully contacted with an adsorbent in the adsorption tower to remove hydrogen fluoride and trace organic matters in the silicon tetrafluoride gas. And the adsorbed silicon tetrafluoride gas sequentially enters a light component removing tower and a heavy component removing tower to remove light component impurities and heavy component impurities. The temperature of the light-removing tower is 140 ℃ below zero, the pressure is 0.2MPa, the temperature of the heavy-removing tower is 135 ℃ below zero, and the pressure is 0.1 MPa.
The mass ratio of the adsorbent 5A molecular sieve to the hollow activated carbon fiber in the adsorption tower is 1: 3. The internal diameter of the hollow activated carbon fiber is 30um, and the wall thickness is 8 um.
The tower bodies of the adsorption tower, the light-weight removing tower and the heavy-weight removing tower are made of Monel alloy; the packing is structured packing made of Monel alloy.
The silicon tetrafluoride gas from the de-heavy tower is detected by a gas detector, and the index of each impurity is H2:0.1ppm;O2:0.05ppm;N20.12 ppm; CO < Dl (not detected); CO 22:0.19ppm;CH4Less than Dl (not detected), HF is 0.06ppm, and the purity of the silicon tetrafluoride gas meets the requirement of 6N-grade high-purity silicon tetrafluoride, and normal filling is carried out.
Example 2
Firstly, setting the temperature of a silicon tetrafluoride feeding adsorption tower to be 70 ℃, introducing silicon tetrafluoride gas with the purity of 99% from the bottom of the adsorption tower, wherein the gas flow is 20Kg/h, and the silicon tetrafluoride gas flows from bottom to top and is fully contacted with an adsorbent in the adsorption tower to remove hydrogen fluoride and trace organic matters in the silicon tetrafluoride gas. And the adsorbed silicon tetrafluoride gas sequentially enters a light component removing tower and a heavy component removing tower to remove light component impurities and heavy component impurities. The temperature of the light-removing tower is-130 ℃, the pressure is 0.3MPa, the temperature of the heavy-removing tower is-125 ℃, and the pressure is 0.2 MPa.
The mass ratio of the adsorbent 5A molecular sieve to the hollow activated carbon fiber in the adsorption tower is 1: 3. The internal diameter of the hollow activated carbon fiber is 30um, and the wall thickness is 8 um.
The tower bodies of the adsorption tower, the light-weight removing tower and the heavy-weight removing tower are made of Monel alloy; the packing is structured packing made of Monel alloy.
The silicon tetrafluoride gas from the de-heavy tower is detected by a gas detector, and the index of each impurity is H2:0.09ppm;O2:0.04ppm;N2:0.1ppm;CO<Dl;CO2:0.12ppm;CH4Less than Dl, HF 0.05, and the purity of the silicon tetrafluoride gas meets the requirement of 6N-grade high-purity silicon tetrafluoride, and normal filling is carried out.
Example 3
Firstly, setting the temperature of a silicon tetrafluoride feeding adsorption tower to be 60 ℃, introducing silicon tetrafluoride gas with the purity of 97% from the bottom of the adsorption tower, wherein the gas flow is 25Kg/h, and the silicon tetrafluoride gas flows from bottom to top and is fully contacted with an adsorbent in the adsorption tower to remove hydrogen fluoride and trace organic matters in the silicon tetrafluoride gas. And the adsorbed silicon tetrafluoride gas sequentially enters a light component removing tower and a heavy component removing tower to remove light component impurities and heavy component impurities. The temperature of the light-removing tower is-120 ℃, the pressure is 0.25MPa, the temperature of the heavy-removing tower is-115 ℃, and the pressure is 0.15 MPa.
The mass ratio of the adsorbent 5A molecular sieve to the hollow activated carbon fiber in the adsorption tower is 1: 3. The internal diameter of the hollow activated carbon fiber is 30um, and the wall thickness is 8 um.
The tower bodies of the adsorption tower, the light-weight removing tower and the heavy-weight removing tower are made of Monel alloy; the packing is structured packing made of Monel alloy.
The silicon tetrafluoride gas from the de-heavy tower is detected by a gas detector, and the index of each impurity is H2:0.08ppm;O2:0.05ppm;N2:0.15ppm;CO<Dl;CO2:0.12ppm;CH4Less than Dl, HF less than Dl, and the purity of the silicon tetrafluoride gas meets the requirement of 6N-grade high-purity silicon tetrafluoride, and normal filling is carried out.
Example 4
Firstly, setting the temperature of a silicon tetrafluoride feeding adsorption tower to be 30 ℃, introducing silicon tetrafluoride gas with the purity of 95% from the bottom of the adsorption tower, wherein the gas flow is 30Kg/h, and the silicon tetrafluoride gas flows from bottom to top and is fully contacted with an adsorbent in the adsorption tower to remove hydrogen fluoride and trace organic matters in the silicon tetrafluoride gas. And the adsorbed silicon tetrafluoride gas sequentially enters a light component removing tower and a heavy component removing tower to remove light component impurities and heavy component impurities. The temperature of the light-removing tower is-135 ℃, the pressure is 0.3MPa, the temperature of the heavy-removing tower is-122 ℃, and the pressure is 0.2 MPa.
The mass ratio of the adsorbent 5A molecular sieve to the hollow activated carbon fiber in the adsorption tower is 1: 3. The internal diameter of the hollow activated carbon fiber is 30um, and the wall thickness is 8 um.
The tower bodies of the adsorption tower, the light-weight removing tower and the heavy-weight removing tower are made of Monel alloy; the packing is structured packing made of Monel alloy.
The silicon tetrafluoride gas from the de-heavy tower is detected by a gas detector, and the index of each impurity is H2:0.2ppm;O2:0.09ppm;N2:0.19ppm;CO<Dl;CO2:0.2ppm;CH4< Dl, HF: 0.35. because the HF index can not meet the requirement, the filling pneumatic valve is automatically closed, the internal circulation pneumatic valve is automatically opened, the system internal circulation is started, and the silicon tetrafluoride gas which can not meet the filling requirement returns to the adsorption tower from the circulation pipeline 7.
And (3) adjusting the temperature of the silicon tetrafluoride feeding adsorption tower to 60 ℃, introducing silicon tetrafluoride gas with the purity of 95% from the bottom of the adsorption tower, wherein the gas flow is 30Kg/h, and the adsorbed silicon tetrafluoride gas sequentially enters a light component removal tower and a heavy component removal tower to complete the removal of light component impurities and heavy component impurities. The temperature of the light-removing tower is-130 ℃, the pressure is 0.3MPa, the temperature of the heavy-removing tower is-120 ℃, and the pressure is 0.2 MPa.
The mass ratio of the adsorbent 5A molecular sieve to the hollow activated carbon fiber in the adsorption tower is 1: 3. The internal diameter of the hollow activated carbon fiber is 30um, and the wall thickness is 8 um.
The tower bodies of the adsorption tower, the light-weight removing tower and the heavy-weight removing tower are made of Monel alloy; the packing is structured packing made of Monel alloy.
The silicon tetrafluoride gas from the de-heavy tower is detected by a gas detector, and the index of each impurity is H2:0.13ppm;O2:0.07ppm;N2:0.15ppm;CO<Dl;CO2:0.18ppm;CH4< Dl, HF: 0.03. because all indexes all meet the requirements, the circulating pneumatic valve is automatically closed at the moment, and the filling pneumatic valve is automatically opened to continue filling.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An automatic purification device of 6N-grade high-purity silicon tetrafluoride, which is characterized by comprising: the device comprises an adsorption tower (1), a light-weight removing tower (2), a heavy-weight removing tower (3), a gas detector (4), a signal receiving and feedback device (5), a controller (6), a circulating pipeline (7), a charging pneumatic valve (8), a circulating pneumatic valve (9), a charging steel cylinder (10) and a raw material steel cylinder (11);
the connection relationship is as follows: the raw material steel cylinder (11), the adsorption tower (1), the light removing tower (2), the heavy removing tower (3), the gas detector (4), the charging pneumatic valve (8) and the charging steel cylinder (10) are sequentially connected through pipelines; one end of a circulating pipeline (7) is connected to a pipeline between the raw material steel cylinder (11) and the adsorption tower (1), the other end of the circulating pipeline is connected to a pipeline between the gas detector (4) and the filling pneumatic valve (8), and a circulating pneumatic valve (9) is connected to the circulating pipeline (7); the signal receiving and feedback device (5) is respectively connected with the gas detector (4) and the controller (6), and the controller (6) is also connected with the filling pneumatic valve (8) and the circulating pneumatic valve (9) and used for controlling the opening and closing of the filling pneumatic valve (8) and the circulating pneumatic valve (9).
2. The automatic purification device of 6N-level high-purity silicon tetrafluoride according to claim 1, wherein the gas detector (4), the signal receiving and feedback device (5), the controller (6), the circulating pipeline (7), the charging pneumatic valve (8) and the circulating pneumatic valve (9) form a charging system for detecting the purity index of silicon tetrafluoride and realizing automatic switching of the charging state of silicon tetrafluoride according to the detection result.
3. The automatic purification device of the 6N-grade high-purity silicon tetrafluoride according to claim 1, wherein the light removal column (2) and the heavy removal column (3) are packed columns; the tower bodies of the adsorption tower (1), the light-weight removing tower (2) and the heavy-weight removing tower (3) are made of monel alloy.
4. The automatic purification device of 6N-grade high-purity silicon tetrafluoride according to claim 1, wherein the packing used in the light removal column (2) and the heavy removal column (3) is structured packing, and the structured packing is Monel.
5. A6N-grade high-purity silicon tetrafluoride automatic purification method is characterized by comprising the following steps:
(1) setting the temperature of the adsorption tower (1) to be 50-70 ℃, and introducing silicon tetrafluoride gas from the bottom of the adsorption tower (1); the silicon tetrafluoride gas flows from bottom to top and is fully contacted with the adsorbent in the adsorption tower (1);
(2) the adsorbed silicon tetrafluoride gas sequentially enters a light component removing tower (2) and a heavy component removing tower (3) to respectively remove light component impurities and heavy component impurities;
(3) the gas detector (4) detects the purity of the silicon tetrafluoride gas coming out of the weight removal tower (3), the purity index information detected by the gas detector (4) is sent to the signal receiving and feedback device (5), and the signal receiving and feedback device (5) sends an instruction whether to start the circulating pipeline (7) or not to the controller (6);
if the purity index of the silicon tetrafluoride gas does not meet the filling requirement, the controller (6) sends a control instruction, closes the filling pneumatic valve (8), opens the circulating pneumatic valve (9), namely stops the filling operation, and starts the internal circulation operation of the circulating pipeline (7); if the purity index of the silicon tetrafluoride gas meets the filling requirement, the controller (6) sends a control instruction, the circulating pneumatic valve (9) is closed, the filling pneumatic valve (8) is opened, and normal filling operation is continued.
6. The automatic purification method of 6N-grade high-purity silicon tetrafluoride according to claim 5, wherein the flow rate of the silicon tetrafluoride gas introduced in the step (1) is 5-30 Kg/h, and the purity is 95-99%.
7. The automatic purification method of 6N-grade high-purity silicon tetrafluoride according to claim 5, wherein the flow rate of the silicon tetrafluoride gas introduced in the step (1) is 20-30 Kg/h.
8. The automatic purification method of 6N-grade high-purity silicon tetrafluoride according to claim 5, wherein the adsorbent in the adsorption column (1) in step (1) is a mixture of molecular sieve and hollow activated carbon fiber, and the mass ratio of the molecular sieve to the hollow activated carbon fiber is 1: 3.
9. The automatic purification method of 6N-grade high-purity silicon tetrafluoride according to claim 8, wherein the molecular sieve is a 5A molecular sieve, the hollow activated carbon fiber has an inner diameter of 30um and a wall thickness of 8 um.
10. The automatic purification method of 6N-grade high-purity silicon tetrafluoride according to claim 5, wherein the temperature of the light component removal tower (2) in the step (2) is-140 to-120 ℃, and the pressure is 0.2 to 0.3 MPa; the temperature of the de-weighting tower (3) in the step (2) is-135 to-115 ℃, and the pressure is 0.1 to 0.2 MPa.
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