CN117463096A - High-purity nitrogen trifluoride preparation system - Google Patents
High-purity nitrogen trifluoride preparation system Download PDFInfo
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- CN117463096A CN117463096A CN202310732950.2A CN202310732950A CN117463096A CN 117463096 A CN117463096 A CN 117463096A CN 202310732950 A CN202310732950 A CN 202310732950A CN 117463096 A CN117463096 A CN 117463096A
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- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 78
- 238000010438 heat treatment Methods 0.000 claims abstract description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000004227 thermal cracking Methods 0.000 claims abstract description 40
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 31
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 31
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 24
- 238000000926 separation method Methods 0.000 claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000003860 storage Methods 0.000 claims abstract description 6
- 230000033116 oxidation-reduction process Effects 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 10
- 239000002033 PVDF binder Substances 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 description 22
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 20
- YPDSOAPSWYHANB-UHFFFAOYSA-N [N].[F] Chemical compound [N].[F] YPDSOAPSWYHANB-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 13
- 239000007788 liquid Substances 0.000 description 11
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 229910052731 fluorine Inorganic materials 0.000 description 10
- 239000011737 fluorine Substances 0.000 description 10
- 239000010410 layer Substances 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005336 cracking Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 230000006872 improvement Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 238000002161 passivation Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910000792 Monel Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002238 carbon nanotube film Substances 0.000 description 2
- 239000010962 carbon steel Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 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
- 244000020998 Acacia farnesiana Species 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 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
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D50/00—Combinations of methods or devices for separating particles from gases or vapours
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/245—Fluorine; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention provides a high-purity nitrogen trifluoride preparation system which comprises an electrolytic tank device, a thermal cracking device, an oxidation-reduction tower, an alkaline washing device, a steam-water separation device, an adsorption device and a rectifying device which are connected in sequence; wherein, the electrolysis trough device includes: the top of the closed electrolytic tank is provided with a first gas outlet, a second gas outlet, a feed inlet and heating pieces arranged around the electrolytic tank; the cathode, the diaphragm and the anode are arranged in the electrolytic tank, wherein the diaphragm is used for isolating the cathode and the anode; a negative pressure storage arranged at the second gas outlet; the anode is a composite electrode formed by a carbon nano tube and a carbon electrode.
Description
The invention relates to a division application with the application number of 202310690484.6 and the application date of 2023-06-12, namely a steam-water separation device for preparing nitrogen trifluoride and a preparation system.
Technical Field
The invention relates to a high-purity nitrogen trifluoride preparation system.
Background
Nitrogen trifluoride is an excellent plasma etching gas in the microelectronics industry, and does not cause contamination of the surface of semiconductor materials such as silicon and silicon nitride, especially semiconductor materials having a thickness of less than 1.5 μm. With the development of nanotechnology and the large-scale development of electronic industry technology, the demand for nitrogen trifluoride will be increasing. With the improvement of the performance of electronic products, the international semiconductor industry has higher and higher requirements on the nitrogen trifluoride preparation process. There are two general methods for preparing nitrogen trifluoride gas: direct fluorine gas and electrolytic processes. The direct fluorine gas method mainly comprises fluorine gas and NH 3 And (3) directly carrying out chemical combination reaction. However, fluorine gas is particularly active, the reaction heat release is large and is not easy to control, the content of byproducts is large, the yield of nitrogen trifluoride is low, and the method is not suitable for industrial production. In the electrolytic process, ammonium bifluoride is directly used as raw material to prepare NF through electrolytic fluorination under mild condition 3 . However, the existing electrolysis method generally uses a carbon electrode or a nickel electrode, a large amount of carbon tetrafluoride gas is generated by using the carbon electrode, the subsequent separation is seriously affected, and the nickel electrode is consumed, so that the cost is obviously increased.
Disclosure of Invention
The invention provides a high-purity nitrogen trifluoride preparation system which can effectively solve the problems.
The invention is realized in the following way:
a high-purity nitrogen trifluoride preparation system comprises an electrolytic tank device, a thermal cracking device, an oxidation-reduction tower, an alkaline washing device, a steam-water separation device, an adsorption device and a rectifying device which are connected in sequence; wherein, the electrolysis trough device includes:
the top of the closed electrolytic tank is provided with a first gas outlet, a second gas outlet, a feed inlet and heating pieces arranged around the electrolytic tank;
the cathode, the diaphragm and the anode are arranged in the electrolytic tank, wherein the diaphragm is used for isolating the cathode and the anode;
a negative pressure storage arranged at the second gas outlet;
the anode is a composite electrode formed by a carbon nano tube and a carbon electrode.
The beneficial effects of the invention are as follows: in the electrolytic cell device of the present invention, a composite electrode is formed by a carbon nanotube and a carbon electrode. Due to the protective effect of the carbon nano tube layer, the carbon electrode cannot be easily oxidized to generate carbon tetrafluoride gas in the electrolysis process, so that the content of carbon tetrafluoride in the product is greatly reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of a high purity NF provided in an embodiment of the present invention 3 A system architecture diagram of the preparation system of (a).
FIG. 2 is a schematic illustration of a high purity NF provided by an embodiment of the present invention 3 Is a schematic structural diagram of an electrolytic cell device in the preparation system.
FIG. 3 is a high purity NF provided by an embodiment of the present invention 3 Is a schematic structural diagram of a thermal cracking device in the preparation system.
FIG. 4 is the present inventionThe high purity NF provided in the examples 3 Is a schematic structural diagram of a part of the structure of the steam-water separation device in the preparation system.
FIG. 5 is a diagram of a high purity NF provided by an embodiment of the present invention 3 Is a schematic structural diagram of a steam-water separation device in the preparation system.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Referring to FIGS. 1-2, embodiments of the present invention provide a high purity NF 3 Comprises an electrolytic tank device 10, a thermal cracking device 20, a redox tower 30, an alkaline washing device 40, a steam-water separation device 50, an adsorption device 60 and a rectification device 70 which are connected in sequence.
Referring to FIG. 2, the method is used for NF 3 An electrolyzer apparatus 10 was prepared comprising:
the electrolysis cell 11 is sealed, a first gas outlet 111, a second gas outlet 112, a feed inlet 113 and heating pieces 110 arranged around the electrolysis cell 11 are arranged at the top of the electrolysis cell 11;
a cathode 12, a diaphragm 13, and an anode 14 disposed in the electrolytic cell 11, wherein the diaphragm 13 is configured to isolate the cathode 12 and the anode 14;
a negative pressure reservoir 17 arranged at said second gas outlet 112.
The structure and shape of the closed electrolytic cell 11 are not limited as long as they have a corrosion preventing and sealing function. In one embodiment, the electrolytic tank 11 includes a tank body and a cover body matched with the tank body, where the tank body and the cover body are made of corrosion-resistant alloy, such as monel or passivated carbon steel alloy, and the like, and the disclosure is not limited thereto. The feed inlet 113 is used for feeding NH according to the proportion 3 HF feedstock. In one embodiment, the feed port 113 includes NH 3 Feed line 1130, HF feed line 1132, NH 4 HF 2 Feed conduit 1134. The benefit of arranging the inlet 113 into three channels is: NH (NH) 4 HF 2 The feed conduit 1134 may be the feed conduit for the initial feedstock, i.e., NH 4 HF 2 After being fully mixed, the mixture is prepared from the NH 4 HF 2 A feed conduit 1134 for feeding; in the electrolytic process, due to HF and NH 3 Is required to be frequently and periodically replenished with HF and NH 3 Raw materials for maintaining NH in the system 3 The ratio of/HF is within a predetermined range. The heating element 110 may be a resistance wire or a hydrothermal heating element, and is not limited herein, and the heating element 110 is used for controlling the temperature of the electrolytic tank 11 to be 60-110 ℃ so as to enable the NH 4 HF 2 Melting. The first gas outlet 111 and the second gas outlet 112 are isolated from each other by the diaphragm 13.
The number of the cathodes 12 and the anodes 14 is not limited, and may be arranged according to actual needs. The cathode 12 may be made of carbon steel or monel; the anode 14 may be made of carbon rod or the like. The diaphragm is used for isolating the hydrogen and the fluorine gas and preventing the hydrogen and the fluorine gas from being mutually interfered to cause explosion. Specifically, the cathode 12 is disposed at the bottom of the electrolytic cell 11, and extends from the bottom of the electrolytic cell 11 into the electrolytic cell 11. The anode 14 is arranged on top of the electrolytic cell 11 and extends from the top of the electrolytic cell 11 into the electrolytic cell 11.
In other embodiments, the method is used for NF 3 The prepared electrolyzer apparatus 10 further comprises: the liquid level sensor 15 may be disposed inside or outside the diaphragm 13, and is not limited herein. In one embodiment, the liquid level sensor 15 is disposed outside the diaphragm 13, so that the liquid level L outside the diaphragm 13 can be obtained 2 。
In other embodiments, as a further improvement, the anode 14 is a composite electrode formed by carbon nanotubes and a carbon electrode, and the specific preparation process is as follows:
s10, dispersing pure carbon nano tube powder in an organic solvent;
s11, adding a binder, and continuously stirring and dispersing to form a mixed solution;
and S12, finally, coating the mixed solution on the surface of the carbon electrode, and drying to remove the redundant solvent to finally form the composite electrode.
In step S10, the carbon nanotube powder is carbon nanotubes with a length of 100 micrometers to 1000 micrometers. The organic solvent may be selected from NMP and analogues thereof. The concentration of the carbon nano tube powder can be 0.05 kg-0.15 kg/L, and the concentration is too large, so that the dispersion of the carbon nano tube is not facilitated.
In step S11, the binder is selected from inert binders, such as PVDF, and the like. The weight of the binder is about 10% -50% of the weight of the carbon nano tube. Preferably, the weight of the binder is about 15% -25% of the weight of the carbon nanotubes. Too low a content of the binder may cause a decrease in adhesion properties, and too high a content may decrease the conductive properties of the carbon nanotube layer.
In one example, 0.1kg of pure carbon nanotube powder was dispersed in 1L of NMP (N-methylpyrrolidone) with an ultrasonic dispersion; then adding 0.02kg of polyvinylidene fluoride (PVDF or polyvinylidene fluoride) into the mixture, and continuously stirring and dissolving the mixture to form a mixed solution; and (3) coating the mixed solution on the surface of the carbon electrode to form a coating with the thickness of 0.1 mm-1 mm, and finally drying at the temperature of 150-200 ℃ to remove redundant NMP. Preferably, the mixed solution is coated on the surface of the carbon electrode to form a coating with the thickness of 0.4-0.6 mm, because the electrolysis efficiency is reduced and the cost is increased remarkably with the increase of the thickness of the coating. It is understood that the protective layer is formed by bonding the carbon nanotubes to the surface of the carbon electrode. Due to the protective effect of the carbon nano tube layer, the carbon electrode cannot be easily oxidized to generate carbon tetrafluoride gas in the electrolysis process, so that the content of carbon tetrafluoride in a product is greatly reduced; the carbon nanotubes in the carbon nanotube layer are not easily oxidized to generate carbon tetrafluoride because of the relatively stable structure. Further, the efficiency of electrolysis can be improved.
According to the invention, the existing carbon electrode is simply modified, so that on one hand, the content of carbon tetrafluoride in a product can be greatly reduced, and on the other hand, the service life of the carbon electrode can be prolonged.
The embodiment of the invention further provides a method for NF 3 A method of controlling the prepared electrolyzer apparatus 10 comprising the steps of:
s1, introducing molten NH through the feed inlet 113 4 HF 2 ；
S2, controlling the pressure of the electrolytic tank device 10 to be +/-1 kPa, the electrolytic temperature to be 100-130 ℃ and the electrolytic voltage to be 5-7V, and enabling the electrolytic tank device to pass through the feed inlet 113 in the reaction process according to NH 3 The ratio of HF to molten salt in the electrolyte was maintained at a molar ratio of 1:3 by feeding the electrolyzer unit 10.
In step S1, molten NH is added 4 HF 2 Providing a initiator of the reaction for the initial reaction. If ammonia and hydrogen fluoride are directly introduced, side reactions are increased.
In step S2, the reaction chemistry equation is as follows:
NH 4 HF 2 +HF-->NF 3 +3H 2 ；
NH 3 +2HF-->NH 4 HF 2 。
as can be seen from the above reaction equation, HF introduced during electrolysis is on the one hand reacted with NH 4 HF 2 Generating reaction to generate NF 3 The method comprises the steps of carrying out a first treatment on the surface of the On the other hand, the supplied HF is continuously connected to NH in the electrolyzer unit 10 3 React to generate NH 4 HF 2 Molten salt, therefore, is required to be fed through the feed port 113 in accordance with NH during the reaction 3 The ratio of HF to molten salt in the electrolyte was maintained at a molar ratio of 1:3 by feeding the electrolyzer unit 10. Side reactions can be generated in the reaction process to generate fluorine-nitrogen impurity gases, such as N 2 F 2 ，N 2 F 4 And (3) waiting for impurity products; carbon tetrafluoride gas, and nitrogen oxides, e.g. N 2 O is the main component.
Since the fluorine nitrogen impurity gas is unstable and is liable to explode after accumulating to a certain extent, it is necessary to eliminate the gas in the subsequent thermal cracking step.
In example A-1, the pressure of the electrolyzer unit 10 was controlled to.+ -.1 kPa, the electrolysis temperature was 100.+ -.2 ℃ and the electrolysis voltage was 7V, and NH was applied to the reaction mixture through the feed port 113 3 The ratio of HF was 1:3 and the molten salt ratio (anode skin, 0.1kg of pure carbon nanotube powder/0.02 kg of polyvinylidene fluoride, film thickness 0.5 mm) in the electrolyte was maintained in the electrolyzer unit 10. The volume content of each gas tested was: NF (NF) 3 : about 75.79%; NH (NH) 3 HF: about 1.6%; n (N) 2 +O 2 : about 21.5%; CF (compact flash) 4 :0.01%; fluorine nitrogen impurity gas: about 0.2%; CO 2 ：0.1％；N 2 O: 0.6%; other: about 0.2%. From the above volume contents, NH 3 HF is reacted substantially in the theoretical molar ratio. Further, the anode was stable for 60 days at a current of 1500A in the cell.
In example A-2, the pressure of the electrolyzer unit 10 was controlled to.+ -.1 kPa, the electrolysis temperature was 100.+ -.2 ℃ and the electrolysis voltage was 7V, and NH was applied to the reaction mixture through the feed port 113 3 The HF ratio isA molar ratio of 1:3 was fed to the electrolyzer unit 10 to maintain the molten salt ratio in the electrolyte (anode skin, 0.1kg pure carbon nanotube powder/0.02 kg polyvinylidene fluoride, film thickness 0.1 mm). The volume content of each gas tested was: NF (NF) 3 : about 75.95%; NH (NH) 3 HF: about 1.2%; n (N) 2 +O 2 : about 21.48%; CF (compact flash) 4 :0.03%; fluorine nitrogen impurity gas: about 0.4%; CO 2 ：0.1％；N 2 O: 0.62%; other: about 0.22%. The anode was stable for about 30 days at 1500A in the cell, and the carbon tetrafluoride content increased significantly after about 30 days, indicating that the carbon nanotube composite layer may be consumed as the electrolysis time increased.
In example A-3, the pressure of the electrolyzer unit 10 was controlled to.+ -.1 kPa, the electrolysis temperature was 100.+ -.2 ℃ and the electrolysis voltage was 7V, and NH was applied to the reaction mixture through the feed port 113 3 The ratio of HF was 1:3 and the molten salt ratio in the electrolyte (anode skin, 0.1kg pure carbon nanotube powder/0.02 kg polyvinylidene fluoride, film thickness 0.3 mm) was maintained in the electrolyzer unit 10. The volume content of each gas tested was: NF (NF) 3 : about 25.86%; NH (NH) 3 HF: about 1.4%; n (N) 2 +O 2 : about 21.49%; CF (compact flash) 4 :0.02%; fluorine nitrogen impurity gas: about 0.3%; CO 2 ：0.1％；N 2 O: 0.62%; other: about 0.21%. The anode was stable at 1500A in the cell and at 45 days or so, the carbon tetrafluoride content increased significantly after 45 days, indicating that the carbon nanotube composite layer may be consumed as the electrolysis time increased.
In example A-4, the pressure of the electrolyzer unit 10 was controlled to.+ -.1 kPa, the electrolysis temperature was 100.+ -.2 ℃ and the electrolysis voltage was 7V, and NH was applied to the reaction mixture through the feed port 113 3 The ratio of HF was 1:3 and the molten salt ratio in the electrolyte (anode skin, 0.1kg pure carbon nanotube powder/0.02 kg polyvinylidene fluoride, film thickness 1 mm) was maintained in the electrolyzer unit 10. The volume content of each gas tested was: NF (NF) 3 : about 74.65%; NH (NH) 3 /HF：About 2.1%; n (N) 2 +O 2 : about 21.65%; CF (compact flash) 4 :0.01%; fluorine nitrogen impurity gas: about 0.2%; CO 2 ：0.3％；N 2 O: 0.91%; other: about 0.18%. The anode was stable at 1500A in the cell for about 70 days with a significant increase in carbon tetrafluoride content after about 70 days, indicating that the carbon nanotube composite layer may be consumed as electrolysis time increases.
Further, as can be seen from example A-1~A-4, NF was increased with the thickness of the carbon nanotube film 3 Reduced content (significantly reduced electrolysis efficiency), but CF 4 Also the content of (for CF) 4 Produces a certain inhibition), but when the thickness reaches 0.5mm, CF increases with the film thickness 4 The content of (2) does not change. In addition, as the thickness of the carbon nanotube film increases, the service life of the carbon nanotube composite layer also increases significantly.
Referring to fig. 3, an embodiment of the present invention provides a thermal cracking apparatus 20 including: comprises a thermal cracking tower 21, an air inlet part 23 arranged at the bottom of the thermal cracking tower 21, a filter screen 22 arranged between the air inlet part 23 and the thermal cracking tower 21, a heating coil 24 wound outside the thermal cracking tower 21, an air outlet 25 arranged at the top of the thermal cracking tower 21, and a heating steel ball 26 filled in the thermal cracking tower 21. The thermal cracking device 20 is used for heating NF 3 The gas is thermally cracked to remove fluorine nitrogen impurity gas impurities. The air inlet 23 is detachably connected with the thermal cracking tower 21 through a flange, thereby facilitating the regular cleaning of the filter screen 22.
The heating coil 24 is a high-frequency heating coil, and generates eddy current in the metal coil by electromagnetic induction, so that joule heating of the metal coil is caused by resistance, and the metal coil is uniformly wound around the outer periphery of the thermal cracking tower 21, so that the temperature of the tower body of the thermal cracking tower 21 is uniform, and the situation that the thermal cracking effect is affected due to local overheating or local temperature is not reached can not occur. Meanwhile, because a high-frequency heating mode is adopted, the steel ball 26 can be heated to reach a set temperature value, a better effect of thermally cracking oxidative impurities can be achieved through the steel ball 26, and a dust removal effect can be achieved through the steel ball 26. The particle size of the heated steel balls 26 is 0.5cm to 2cm. The heating coil 24 may be divided into a plurality of heating sections from top to bottom, and each heating section is provided with a temperature measuring instrument, so that the whole thermal cracking tower 21 is heated uniformly with more accurate temperature control.
In one embodiment, the thermal cracking tower 21 has a height of about 1.6 to 2.4 meters and an inner diameter of about 0.3 meters. And the heating coil 24 is divided into a first heating zone, a second heating zone, and a third heating zone from top to bottom. The height of the first heating area is about 0.8-1.2 m, the height of the second heating area is about 0.5-0.7 m, and the height of the third heating area is about 0.3-0.5 m. The temperature of the first heating area is about 160-180 ℃, and the temperature of the second heating area is about 140-160 ℃; the temperature of the third heating area is about 120-140 ℃.
Example B-1: the gas in example 1 was treated through the thermal cracking tower 21, wherein the parameters of the thermal cracking tower 21 were as follows: the thermal cracking tower 21 has a height of about 2 m and an inner diameter of about 0.3 m. And the heating coil 24 is divided into a first heating zone 260, a second heating zone 262, and a third heating zone 264 from top to bottom. The first heating zone 260 has a height of about 1 meter, the second heating zone 262 has a height of about 0.6 meter, and the third heating zone 264 has a height of about 0.4 meter. Wherein the temperature of the first heating zone 260 is about 170 ℃, and the temperature of the second heating zone 262 is about 150 ℃; the temperature of the third heating zone 264 is about 130 ℃.
And (3) detecting: the gas content after the cracking reaction is as follows: NF (NF) 3 : about 75.75%; NH (NH) 3 HF: about 1.4%; n (N) 2 +O 2 : about 21.4%; CF (compact flash) 4 :0.01%; fluorine nitrogen impurity gas: 2 (ppmv); CO 2 ：0.1％；N 2 O: 0.6%; other: about 0.74%. By thermal cracking control of the three heating areas, fluorine-nitrogen impurity gas such as N can be obtained 2 F 2 ，N 2 F 4 The content of the iso-impurity products is controlled to be 2 ppmvFurther, the occurrence of danger such as explosion is greatly reduced. Further, by increasing the temperature layer by layer from low to high, NF due to abrupt temperature change can be avoided 3 Side reactions of gas production, as can be seen from the above data, by three-stage thermal cracking, it is important to NF 3 The effect of (2) is almost negligible, but the content of fluorine-nitrogen impurity gas can be significantly reduced.
Comparative example C-1: the gas in example 1 was treated through the thermal cracking tower 21, wherein the parameters of the thermal cracking tower 21 were as follows: the thermal cracking tower 21 has a height of about 2 m and an inner diameter of about 0.3 m. And the heating coil 24 is divided into a first heating zone, a second heating zone, and a third heating zone from top to bottom. The height of the first heating area is about 1 meter, the height of the second heating area is about 0.6 meter, and the height of the third heating area is about 0.4 meter. Wherein the temperature of the first heating zone is about 130 ℃, and the temperature of the second heating zone is about 130 ℃; the temperature of the third heating zone is about 130 ℃.
And (3) detecting: the gas content after the cracking reaction is as follows: NF (NF) 3 : about 75.77%; NH (NH) 3 HF: about 1.5%; n (N) 2 +O 2 : about 21.3%; CF (compact flash) 4 :0.01%; fluorine nitrogen impurity gas: about 0.15%; CO 2 ：0.1％；N 2 O: 0.6%; other: about 0.57%.
In comparative example C1, the thermal cracking temperature of about 130℃did not result in a satisfactory cracking reaction of the fluorine nitrogen-based impurity gas.
Comparative example C-2: the gas in example 1 was treated through the thermal cracking tower 21, wherein the parameters of the thermal cracking tower 21 were as follows: the thermal cracking tower 21 has a height of about 2 m and an inner diameter of about 0.3 m. And the heating coil 24 is divided into a first heating zone, a second heating zone, and a third heating zone from top to bottom. The height of the first heating area is about 1 meter, the height of the second heating area is about 0.6 meter, and the height of the third heating area is about 0.4 meter. Wherein the temperature of the first heating zone is about 150 ℃, and the temperature of the second heating zone is about 150 ℃; the temperature of the third heating zone is about 150 ℃.
And (3) detecting: the gas content after the cracking reaction is as follows: NF (NF) 3 : about 74.48%; NH (NH) 3 HF: about 1.4%; n (N) 2 +O 2 : about 21.2%; CF (compact flash) 4 :0.01%; fluorine nitrogen impurity gas: about 15 (ppmv); CO 2 ：0.1％；N 2 O: 0.6%; other: about 2.21%.
From comparative example C2, it was found that the fluorine-nitrogen-based impurity gas was thermally cracked at a thermal cracking temperature of about 150℃and a good thermal cracking effect was obtained, but the NF was caused by a rapid temperature change 3 Also has certain effect to lead NF 3 The content is reduced.
Comparative example C-3: the gas in example 1 was treated through the thermal cracking tower 21, wherein the parameters of the thermal cracking tower 21 were as follows: the thermal cracking tower 21 has a height of about 2 m and an inner diameter of about 0.3 m. And the heating coil 24 is divided into a first heating zone, a second heating zone, and a third heating zone from top to bottom. The height of the first heating area is about 1 meter, the height of the second heating area is about 0.6 meter, and the height of the third heating area is about 0.4 meter. Wherein the temperature of the first heating zone is about 170 ℃, and the temperature of the second heating zone is about 170 ℃; the temperature of the third heating zone is about 170 ℃.
And (3) detecting: the gas content after the cracking reaction is as follows: NF (NF) 3 : about 71.73%; NH (NH) 3 HF: about 1.2%; n (N) 2 +O 2 : about 21.6%; CF (compact flash) 4 :0.01%; fluorine nitrogen impurity gas: about 3 (ppmv); CO 2 ：0.1％；N 2 O: 0.6%; other: about 4.76%.
From comparative example C3, it was found that when the thermal cracking temperature was about 170℃and the thermal cracking effect on the fluorine-nitrogen-based impurity gas was excellent, NF was caused by the rapid temperature change 3 Also has certain effect to lead NF 3 The content is obviously reduced. As can be seen from the above experiments, the temperature of thermal cracking controls the temperature of the p-fluoroazasPlasma gas and NF 3 The effect is great.
The oxidation-reduction column 30 is used for converting N 2 O removal, specifically, the redox column 30 contains a sodium sulfite solution, which is mixed with N 2 O reacts to remove N 2 O gas, the specific chemical equation of which is as follows:
Na 2 SO 3 +2NO 2 =Na 2 SO 4 +N 2 。
the sodium sulfite solution in the redox column 30 may be a dilute solution having a concentration of less than 5wt%, which is advantageous in that it can be combined with N 2 O reacts to remove N 2 The O gas can also play a role of water washing to remove HF gas.
The caustic washing device 40 is used for removing trace acid gases such as HF and CO in the gas 2 Etc. The alkali liquor in the alkali washing device 40 can be KOH alkali liquor with the concentration of 20% -40%.
Referring to fig. 4-5, the steam-water separator 50 is used for removing water vapor in the gas, and specifically, the steam-water separator 50 includes a steam-water separator 51, a cyclone 52, and a freeze dryer 53.
The steam-water separator 51 includes:
a container 510;
a first air inlet 512 provided at the top of the container 510;
the water-vapor separation pipes 511 are vertically arranged at the middle upper part of the container 510 in parallel, wherein each water-vapor separation pipe 511 is further provided with a plurality of water-vapor separation cavities 5110 along the height direction thereof, and the water-vapor separation cavities 5110 are staggered;
a water storage part 518 formed at the middle and lower part of the container 510 and used for receiving the water of the water-vapor separation pipe 511;
an air outlet pipe 514 penetrating through the water-vapor separation pipe 511 from the top of the container 510, and the air outlet pipe 514 is communicated with the water storage part 518;
a first air outlet 515 in communication with the air outlet tube 514;
a drain 516 is provided at the bottom of the container 510.
The water-vapor separation chambers 5110 are cochlear structures and are arranged in two rows in the vertical direction, wherein the top of the cochlear structure of one row is opposite to the middle of the cochlear structure of the other row. When chemical gas flows along the wall surface of the water-vapor separation cavity 5110 with water drops, the water drops adhere to the wall surface of the water-vapor separation cavity 5110 due to the adhesive force, and a liquid film is formed to flow downwards so as to be separated from the chemical gas. Further, in one embodiment, the water vapor separation chamber 5110 is filled with condensed water metal balls 5112. The metal ball 5112 may be made of ferrite stainless steel with carbon content less than 0.01%, such as 1.4024 (SUS 410J1, 1Cr13 Mo), 1.4113 (S43400, SUS 434), 1.4418 (X4 CrNiMo16-5-1, 0Cr16Ni5 Mo). The size of the metal balls 5112 can be selected according to practical needs, and the diameter of the metal balls 5112 is preferably 1 cm-5 cm.
In one embodiment, the metal balls 5112 are made of ferritic stainless steel 1.4418. On the one hand, the ferritic stainless steel 1.4418 has an extremely low carbon content, so that it has optimal hydrophilic performance (the hydrophilic angle with water is about 35 degrees, and the general stainless steel is about 50 degrees), on the other hand, the ferritic stainless steel 1.4418 contains nickel element, and the nickel element can be further passivated by fluorine gas/chlorine gas, so that the service life and the hydrophilicity of the ferritic stainless steel can be improved. Specifically, the step of passivating the ferritic stainless steel 1.4418 by fluorine/chlorine includes:
placing a ferrite stainless steel 1.4418 steel ball into a passivation kettle;
introducing inert gas to expel air in the passivation kettle, and vacuumizing;
heating the passivation kettle to 100-150 ℃, and introducing fluorine/chlorine mixed gas, wherein the ratio of fluorine/chlorine is 1-3:1, the air pressure is controlled to be 2-5 kPa, and passivation is carried out for 2-10 minutes;
and naturally cooling after passivation is finished. Through testing (a planar stainless steel sheet is actually adopted), the hydrophilic angle of the stainless steel sheet and water is reduced from about 35 degrees to about 23 degrees. This may be due to the nano-or micro-scale microstructure created on its surface. According to the Cassie and Wenzel wet state theory, if a liquid is in direct contact with the concave-convex surface of a solid surface microstructure, the droplet is in Wenzel state. The Wenzel state determines that when a liquid directly contacts a microstructured surface, the theta angle is converted to cos (theta w ) R ∗ cos (θ), where r is the ratio of the actual area to the projected area (roughness, roughness factor), θ represents the actual contact angle between the droplet and the surface, θ w Is the angle after the transition. The equation for Wenzel's state shows that microstructured one surface will amplify the surface tension. The hydrophobic surface (having a contact angle greater than 90 °) will become more hydrophobic after microstructured and its new contact angle will increase than before. However, a hydrophilic surface (having a contact angle less than 90 °) will become more hydrophilic after microstructuring, and its new contact angle will be reduced from that of the original.
During maintenance, the metal balls 5112 can be replaced, so that the cleaning agent is convenient to maintain. The present invention may be more economical by replacing the metal balls 5112 as opposed to replacing the entire water vapor separator tube 511.
As a further improvement, the water outlet 516 is further connected to a water seal pipe 517, and the height H of the water seal pipe 517 is 0.3 to 0.5 meter. The too high height of the water seal pipe 517 influences the removal rate of aqueous vapor, the too low pressure of the water seal pipe 517 makes the pressure too little to make chemical gas discharge through the water seal mouth easily, cause pollution and extravagant. In one embodiment, the height of the water seal in the water seal tube 517 is 0.4 meter.
The cyclone separator 52 includes a cyclone separator body 520, a second air inlet 521 and a second air outlet 522 provided to the cyclone separator body 520, and a second drain pipe 523 provided to the bottom of the cyclone separator body 520. As a further improvement, the cyclone 52 is arranged on top of the steam-water separator 51, and the second drain line 523 extends along the outlet pipe 514 into the water reservoir 518 for liquid sealing.
The freeze dryer 53 includes a dryer body 530, a third air inlet 531 and a third air outlet 532 disposed on the dryer body 530, and a third drain pipeline 533 disposed at the bottom of the dryer body 530. As a further improvement, the freeze dryer 53 is disposed at an upper portion of the steam separator 51, and the third drain pipe 533 is communicated with the buffer chamber 519 through a water inlet 513 disposed at a top of the container 510. Since the third drain pipe 533 is communicated with the buffer chamber 519, the liquid droplets frozen by the freeze dryer 53 can be discharged into the buffer chamber 519, and flow from the buffer chamber 519 through the water-vapor separation pipe 511 to the water storage portion 518. The temperature of the liquid droplets frozen by the freeze dryer 53 is low, so that the low-temperature liquid enters the gas buffer chamber 519, and the liquid droplets in the chemical gas can be further condensed, so that the water removal efficiency of the gas-water separation device after water washing is improved. It will be appreciated that by completely removing the water, the effect of moisture on the adsorbent in the subsequent adsorption unit 60 can be greatly reduced.
The adsorption device 60 is mainly used for adsorbing carbon tetrafluoride gas in gas. Carbon tetrafluoride is one of the most difficult gases to separate from impurity gases in nitrogen trifluoride because carbon tetrafluoride has relatively similar properties to nitrogen trifluoride. The adsorption device 60 according to the embodiment of the present invention includes at least two stages of flat pressure adsorption tanks. The pressure of each stage of flat pressure adsorption tank is 1-3kPa. The flat pressure adsorption tank is filled with a special carbon tetrafluoride adsorbent, and is mainly used for special adsorption of carbon tetrafluoride. In one embodiment, the carbon tetrafluoride specific adsorbent is a carbon tetrafluoride specific adsorbent manufactured by Ningxia Huahui environmental protection technologies Co., ltd. In one embodiment, the method comprises 3 stages of flat-pressure adsorption tanks, wherein each flat-pressure adsorption tank has a length of about 4 meters and an inner diameter of about 0.2 meters, is filled with carbon tetrafluoride special-effect adsorbent, and can remove more than 99.95% of carbon tetrafluoride gas through the adsorption device 60.
The rectifying device 70 is used for removing other impurity gases, and the rectifying device 70 and its control are in the prior art, and will not be described here. Through the control, the nitrogen trifluoride gas with the purity of more than 99.999 percent can be obtained.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The high-purity nitrogen trifluoride preparation system is characterized by comprising an electrolytic tank device, a thermal cracking device, an oxidation-reduction tower, an alkaline washing device, a steam-water separation device, an adsorption device and a rectifying device which are connected in sequence; wherein, the electrolysis trough device includes:
the top of the closed electrolytic tank is provided with a first gas outlet, a second gas outlet, a feed inlet and heating pieces arranged around the electrolytic tank;
the cathode, the diaphragm and the anode are arranged in the electrolytic tank, wherein the diaphragm is used for isolating the cathode and the anode;
a negative pressure storage arranged at the second gas outlet;
the anode is a composite electrode formed by a carbon nano tube and a carbon electrode.
2. The high purity nitrogen trifluoride production system as claimed in claim 1, wherein said composite electrode is obtained by:
s10, dispersing pure carbon nano tube powder in an organic solvent;
s11, adding a binder, and continuously stirring and dispersing to form a mixed solution;
and S12, finally, coating the mixed solution on the surface of the carbon electrode, and drying to remove the redundant solvent to finally form the composite electrode.
3. The system for preparing high purity nitrogen trifluoride as claimed in claim 2 wherein said carbon nanotube powder is carbon nanotubes having a length of 100 microns to 1000 microns.
4. The high purity nitrogen trifluoride production system as claimed in claim 2 wherein said organic solvent is selected from NMP.
5. The high purity nitrogen trifluoride production system of claim 2 wherein said binder is PVDF.
6. The system for preparing high purity nitrogen trifluoride as claimed in claim 2, wherein the binder is about 10% -50% by weight of the carbon nanotubes.
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