CN105152134A - Method and device for preparing hydrogen fluoride - Google Patents
Method and device for preparing hydrogen fluoride Download PDFInfo
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- CN105152134A CN105152134A CN201510605559.1A CN201510605559A CN105152134A CN 105152134 A CN105152134 A CN 105152134A CN 201510605559 A CN201510605559 A CN 201510605559A CN 105152134 A CN105152134 A CN 105152134A
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Abstract
The invention relates to a method and device for preparing hydrogen fluoride, and belongs to the technical field of chemical engineering. The method includes the steps that a whole reaction device is vacuumized, and liquid-phase hydrogen fluoride is added into the reactor; fluorine gas is added into an upper gas-phase space of the reactor till the pressure of the reactor is 0.2-0.5 MPa, and the temperature of the reactor is controlled to range from -40 DEG C to 40 DEG C; hydrogen with the flow being 0.1-10L/min is added into a liquid-phase space of the reactor, the hydrogen reacts with the fluorine gas on the liquid-phase plane intersection after being introduced into a gas distributor, and hydrogen fluoride is obtained. The device is mainly composed of a raw material gas inlet I, a raw material gas inlet II, a flow meter I, a cooling liquid inlet, a flow meter II, a cooling liquid outlet, a jacket, the reactor, the gas distributor, a heat exchanger, a vacuum system port, a flow meter III and a low-temperature storage. By means of the device, the fluorine gas and the hydrogen can directly react with each other, operation is safe, the purity of the prepared hydrogen fluoride is high, and the device is suitable for large-scale production.
Description
Technical field
The present invention relates to one and prepare hydrofluoric method and device, belong to chemical technology field.
Background technology
Hydrogen fluoride is a kind of chemical of extensive application, its main application fields is as follows: (1), as the raw material preparing fluorochemicals, is prepare villiaumite, fluorine source containing fluorinated refrigerant, fluoro-containing plastic, fluorine-containing rubber, fluorine resin and the material such as fluorine-containing medicines or agricultural chemicals; (2) as strongly-acid etching reagent, for etching glass, acid-washed metal and etching semiconductor surface; (3) as the catalyzer carrying out alkylated reaction; (4) as analytical reagent; (5) as purge gas.
Industrial hydrogen fluoride is generated by fluorite and sulfuric acid reacting by heating:
CaF
2+H
2SO
4→2HF+CaSO
4
Utilize this kind of method to prepare hydrogen fluoride, production cost is low and HF that is preparation can meet general industry application requiring.But the method raw material used contains more impurity, the impurity such as arsenic wherein, sulfide, phosphoric acid are extremely difficult except going to lower value by conventional purification process, cause the HF purity prepared low.In Application to Electronic Industry, hydrofluoric purity and cleanliness factor have tremendous influence to the yield rate of unicircuit, electrical property and reliability.And along with the fast development of electronics, information, communications industry, the requirement of electronic industry to hydrofluoric purity and cleanliness factor is more and more higher.
The hydrogen fluoride purity adopting fluorine gas and hydrogen directly to synthesize is higher, is suitable as the unstripped gas of electronic grade high-purity anhydrous hydrogen fluoride.Because fluorine gas and hydrogen reaction are violent, just can blast once contact, dangerous high, institute never realizes industrialized application in this way.Control to react the key point of the speed of carrying out and degree of uniformity synthetic method for this reason.
Summary of the invention
For the defect existed in prior art, an object of the present invention is to provide one to prepare hydrofluoric method, described method can realize the direct reaction of fluorine gas and hydrogen, and prepared hydrogen fluoride purity is high, can meet electronic industry to the highly purified requirement of hydrogen fluoride.
Two of object of the present invention is to provide one to prepare hydrofluoric device, described device operational safety, and is applicable to the hydrofluoric large-scale production of high purity.
The object of the invention is to be achieved through the following technical solutions.
One prepares hydrofluoric method, and described method steps is as follows:
Step 1. first vacuumizes process to whole reaction unit, then adds liquid-phase fluorination hydrogen in reactor lower part; The volume of liquid-phase fluorination hydrogen is 20% ~ 80% of reactor volume;
Fluorine gas is added to the upper gaseous phase space of reactor by step 2., and to reactor, pressure is 0.2 ~ 0.5MPa;
The temperature that step 3. controls reactor is-40 ~ 40 DEG C, is the liquid Space that the hydrogen of 0.1 ~ 10L/min joins reactor lower part, reacts flow, obtain described hydrogen fluoride with fluorine gas at liquid phase plane intersection.
The volume preferably 10 ~ 2000L of reactor described in step 1.
Described in step 1, the volume of liquid-phase fluorination hydrogen is preferably 40% ~ 60% of reactor volume.
Pressure preferably 0.3 ~ 0.4MPa in reactor described in step 2.
The temperature of reactor described in step 3 preferably-20 ~ 20 DEG C.
The flow preferably 1 ~ 3L/min of hydrogen described in step 3.
Preferably, hydrogen described in step 3 is added to the liquid Space of reactor lower part, by reacting at liquid phase plane intersection with fluorine gas after gas distributor.
Preferably, when the pressure of question response device is 0.1 ~ 0.15MPa, stop adding hydrogen; In reactor, add fluorine gas, after being 0.5MPa to the pressure of reactor, continue to add hydrogen.
Preferably, when the hydrogen fluoride liquid phase volume produced is 10% ~ 20% of reactor volume, stop adding hydrogen; By volume be the liquid-phase fluorination hydrogen of 10% ~ 20% of reactor volume by pipeline and metered flow transfer in cryogenic memory.
One prepares hydrofluoric device of the present invention, and described device forms primarily of raw material gas inlet I 1, raw material gas inlet II 2, flow meter I 12, cooling liquid inlet 3, flow meter II 13, cooling liquid outlet 4, chuck 10, reactor 9, gas distributor 7, interchanger 6, vacuum system interface 5, under meter III 11 and cryogenic memory 8.
Wherein, the line end be connected with raw material gas inlet II 2 stretches into the liquid Space of reactor 9 bottom, and is connected with gas distributor 7; Raw material gas inlet II 2 pipeline is below provided with successively valve, flow meter I 12; The pipeline one end under meter III 11 place is connected with the liquid Space of reactor 9 bottom, and below gas distributor 7, the other end is connected with the top of cryogenic memory 8; Gas distributor 7 in the lower liquid phase space of reactor 9, and under the liquid level of liquid Space; The bottom of reactor 9 is in the inside of chuck 10; Thermometer in the outside of reactor 9 and chuck 10, and is positioned on the liquid level of reactor 9 liquid Space; Interchanger 6 is at the gas-phase space on reactor 9 top; The pipeline be connected with cooling liquid inlet 3 is respectively with the import of interchanger 6, be connected with the pipeline import of chuck 10 inside by reactor 9 outside; The outlet of interchanger 6, to be connected with the pipeline at cooling liquid outlet 4 place respectively with the tube outlet of chuck 10 inside by reactor 9 outside; Cooling liquid inlet 3 pipeline is below provided with flow meter II 13; The line end be connected with raw material gas inlet I 1 stretches into the upper gaseous phase space of reactor 9; Tensimeter in the outside of reactor 9, and is connected with the gas-phase space on reactor 9 top; The pipeline one end at vacuum system interface 5 place is connected with reactor 9, and the other end is connected with cryogenic memory 8.
Beneficial effect:
In method of the present invention, completely cut off hydrogen and fluorine gas by liquid-phase fluorination hydrogen, avoid the direct contact of the two; Make gas distribution even by gas distributor; And by the speed that the flow control controlling hydrogen is reacted, thus realize the direct reaction of fluorine gas and hydrogen, obtained highly purified hydrogen fluoride.
Device of the present invention, operational safety, is applicable to the hydrofluoric large-scale production of high purity.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention synthesizes hydrogen fluoride device.
In figure, 1-raw material gas inlet I, 2-raw material gas inlet II, 3-cooling liquid inlet, 4-cooling liquid outlet, 5-vacuum system interface, 6-interchanger, 7-gas distributor, 8-cryogenic memory, 9-reactor, 10-chuck, 11-under meter III, 12-flow meter I, 13-flow meter II.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail explanation.
In following examples:
Cooling fluid used is ethylene glycol.
As shown in Figure 1, prepare hydrofluoric device in embodiment to form primarily of raw material gas inlet I 1, raw material gas inlet II 2, flow meter I 12, cooling liquid inlet 3, flow meter II 13, cooling liquid outlet 4, chuck 10, reactor 9, gas distributor 7, interchanger 6, vacuum system interface 5, under meter III 11 and cryogenic memory 8.
Wherein, the line end be connected with raw material gas inlet II 2 stretches into the liquid Space of reactor 9 bottom, and is connected with gas distributor 7; Raw material gas inlet II 2 pipeline is below provided with successively valve, flow meter I 12; The pipeline one end under meter III 11 place is connected with the liquid Space of reactor 9 bottom, and below gas distributor 7, the other end is connected with the top of cryogenic memory 8; Gas distributor 7 in the lower liquid phase space of reactor 9, and under the liquid level of liquid Space; The bottom of reactor 9 is in the inside of chuck 10; Thermometer in the outside of reactor 9 and chuck 10, and is positioned on the liquid level of reactor 9 liquid Space; Interchanger 6 is at the gas-phase space on reactor 9 top; The pipeline be connected with cooling liquid inlet 3 is respectively with the import of interchanger 6, be connected with the pipeline import of chuck 10 inside by reactor 9 outside; The outlet of interchanger 6, to be connected with the pipeline at cooling liquid outlet 4 place respectively with the tube outlet of chuck 10 inside by reactor 9 outside; Cooling liquid inlet 3 pipeline is below provided with flow meter II 13; The line end be connected with raw material gas inlet I 1 stretches into the upper gaseous phase space of reactor 9; Tensimeter in the outside of reactor 9, and is connected with the gas-phase space on reactor 9 top; The pipeline one end at vacuum system interface 5 place is connected with reactor 9, and the other end is connected with cryogenic memory 8.
Preparing hydrofluoric technical process is: first vacuumize process by vacuum system interface 5 to whole reaction unit; By raw material gas inlet I 1, liquid-phase fluorination hydrogen being added to volume is in reactor 9 bottom of 10 ~ 2000L, to 20% ~ 80% of reactor 9 volume; In reactor 9, pass into fluorine gas by raw material gas inlet I 1, the pressure to reactor 9 is 0.1 ~ 0.5MPa; Adjusted the coolant rate of cooling liquid inlet 3 by flow meter II 13, cooling fluid respectively through interchanger 6, be positioned at outside and chuck 10 inside of reactor 9 pipeline after flowed out by cooling liquid outlet 4, thus the temperature controlling reactor 9 is at-40 ~ 40 DEG C; By raw material gas inlet II 2 and flow meter I 12, add to reactor 9 hydrogen that inbound traffics are 0.1 ~ 10L/min, hydrogen, by after gas distributor 7, reacts at liquid phase plane intersection with fluorine gas, generates hydrogen fluoride; Along with the carrying out of reaction, the pressure of reactor 9 reduces gradually, when pressure is reduced to 0.1 ~ 0.15MPa, stops adding hydrogen; In reactor 9, add fluorine gas to the pressure of reactor 9 is, after 0.5MPa, continue to add hydrogen; When the hydrogen fluoride liquid phase volume produced is 10% ~ 20% of reactor 9 volume, stopping adding hydrogen, is that the liquid-phase fluorination hydrogen of 10% ~ 20% of reactor 9 volume is transferred in cryogenic memory 8 by under meter III 11 metered flow by volume.
Embodiment 1
After vacuumizing process by vacuum system interface 5 to whole reaction unit, by raw material gas inlet I 1, the liquid-phase fluorination hydrogen of 100L being added volume is in reactor 9 bottom of 200L; In reactor 9, passing into fluorine gas by raw material gas inlet I 1, is 0.5MPa to reactor 9 pressure; By the coolant rate of controlled cooling model liquid import 3, make the temperature of reactor 9 at-20 ~ 20 DEG C; By raw material gas inlet II 2, add to reactor 9 hydrogen that inbound traffics are 2L/min, hydrogen, by after gas distributor 7, reacts at liquid phase plane intersection with fluorine gas, generates hydrogen fluoride; Along with the carrying out of reaction, the pressure of reactor 9 reduces gradually, when pressure is reduced to 0.15MPa, stops adding hydrogen; In reactor 9, add fluorine gas, after being 0.5MPa to the pressure of reactor 9, continue to add hydrogen; When the hydrogen fluoride liquid phase volume produced is 20L, stops adding hydrogen, 20L liquid-phase fluorination hydrogen is transferred in cryogenic memory 8 by under meter III 11 metered flow.
Embodiment 2
After vacuumizing process by vacuum system interface 5 to whole reaction unit, by raw material gas inlet I 1, the liquid-phase fluorination hydrogen of 8L being added volume is in reactor 9 bottom of 10L; In reactor 9, passing into fluorine gas by raw material gas inlet I 1, is 0.4MPa to reactor 9 pressure; By the coolant rate of controlled cooling model liquid import 3, make the temperature of reactor 9 at-40 ~ 40 DEG C; By raw material gas inlet II 2, add to reactor 9 hydrogen that inbound traffics are 0.1L/min, hydrogen, by after gas distributor 7, reacts at liquid phase plane intersection with fluorine gas, generates hydrogen fluoride; Along with the carrying out of reaction, the pressure of reactor 9 reduces gradually, when pressure is reduced to 0.1MPa, stops adding hydrogen; In reactor 9, add fluorine gas, after being 0.5MPa to the pressure of reactor 9, continue to add hydrogen; When the hydrogen fluoride liquid phase volume produced is 2L, stops adding hydrogen, 2L liquid-phase fluorination hydrogen is transferred in cryogenic memory 8 by under meter III 11 metered flow.
Embodiment 3
After vacuumizing process by vacuum system interface 5 to whole reaction unit, by raw material gas inlet I 1, the liquid-phase fluorination hydrogen of 400L being added volume is in reactor 9 bottom of 2000L; In reactor 9, passing into fluorine gas by raw material gas inlet I 1, is 0.2MPa to reactor 9 pressure; By the coolant rate of controlled cooling model liquid import 3, make the temperature of reactor 9 at-40 ~ 40 DEG C; By raw material gas inlet II 2, add to reactor 9 hydrogen that inbound traffics are 10L/min, hydrogen, by after gas distributor 7, reacts at liquid phase plane intersection with fluorine gas, generates hydrogen fluoride; Along with the carrying out of reaction, the pressure of reactor 9 reduces gradually, when pressure is reduced to 0.1MPa, stops adding hydrogen; In reactor 9, add fluorine gas, after being 0.5MPa to the pressure of reactor 9, continue to add hydrogen; When the hydrogen fluoride liquid phase volume produced is 300L, stops adding hydrogen, 300L liquid-phase fluorination hydrogen is transferred in cryogenic memory 8 by under meter III 11 metered flow.
These are only preferred embodiment of the present invention, be not intended to limit protection scope of the present invention.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement and improvement etc., be all included within protection scope of the present invention.
Claims (10)
1. prepare a hydrofluoric method, it is characterized in that: described method steps is as follows:
Step 1. first vacuumizes process to whole reaction unit, then adds liquid-phase fluorination hydrogen in reactor lower part; The volume of liquid-phase fluorination hydrogen is 20% ~ 80% of reactor volume;
Fluorine gas is added to the upper gaseous phase space of reactor by step 2., and to reactor, pressure is 0.2 ~ 0.5MPa;
The temperature that step 3. controls reactor is-40 ~ 40 DEG C, is the lower liquid phase space that the hydrogen of 0.1 ~ 10L/min joins reactor, reacts flow, obtain described hydrogen fluoride with fluorine gas at liquid phase plane intersection.
2. one according to claim 1 prepares hydrofluoric method, it is characterized in that: when the pressure of question response device is 0.1 ~ 0.15MPa, stops adding hydrogen; In reactor, add fluorine gas, after being 0.5MPa to the pressure of reactor, continue to add hydrogen.
3. one according to claim 1 prepares hydrofluoric method, it is characterized in that: when the hydrogen fluoride liquid phase volume produced is 10% ~ 20% of reactor volume, stops adding hydrogen; By volume be the liquid-phase fluorination hydrogen of 10% ~ 20% of reactor volume by pipeline and metered flow transfer in cryogenic memory.
4. one according to claim 1 prepares hydrofluoric method, it is characterized in that: the volume of described reactor is 10 ~ 2000L.
5. one according to claim 1 prepares hydrofluoric method, it is characterized in that: described in step 1, the volume of liquid-phase fluorination hydrogen is 40% ~ 60% of reactor volume.
6. one according to claim 1 prepares hydrofluoric method, it is characterized in that: the pressure of reactor described in step 2 is 0.3 ~ 0.4MPa.
7. one according to claim 1 prepares hydrofluoric method, it is characterized in that: the temperature of reactor described in step 3 is-20 ~ 20 DEG C.
8. one according to claim 1 prepares hydrofluoric method, it is characterized in that: the flow of hydrogen described in step 3 is 1 ~ 3L/min.
9. one according to claim 1 prepares hydrofluoric method, it is characterized in that: hydrogen described in step 3 is added to the liquid Space of reactor lower part, by reacting at liquid phase plane intersection with fluorine gas after gas distributor.
10. prepare a hydrofluoric device as claimed in claim 1, it is characterized in that: described device forms primarily of raw material gas inlet I (1), raw material gas inlet II (2), flow meter I (12), cooling liquid inlet (3), flow meter II (13), cooling liquid outlet (4), chuck (10), reactor (9), gas distributor (7), interchanger (6), vacuum system interface (5), under meter III (11) and cryogenic memory (8);
Wherein, the line end be connected with raw material gas inlet II (2) stretches into the liquid Space of reactor (9) bottom, and is connected with gas distributor (7); Raw material gas inlet II (2) pipeline is below provided with successively valve, flow meter I (12); The pipeline one end under meter III (11) place is connected with the liquid Space of reactor 9 bottom, and below gas distributor (7), the other end is connected with the top of cryogenic memory (8); Gas distributor (7) in the lower liquid phase space of reactor (9), and under the liquid level of liquid Space; The bottom of reactor (9) is in the inside of chuck (10); Thermometer in the outside of reactor (9) and chuck (10), and is positioned on the liquid level of reactor (9) liquid Space; Interchanger (6) is at the gas-phase space on reactor (9) top; The pipeline be connected with cooling liquid inlet (3) is connected with the import of interchanger (6), pipeline import that is outside by reactor (9) and chuck (10) inside respectively; The outlet of interchanger (6), tube outlet that is outside by reactor (9) and chuck (10) inside are connected with the pipeline at cooling liquid outlet (4) place respectively; Cooling liquid inlet (3) pipeline is below provided with flow meter II (13); The line end be connected with raw material gas inlet I (1) stretches into the upper gaseous phase space of reactor (9); Tensimeter in the outside of reactor (9), and is connected with the gas-phase space on reactor (9) top; The pipeline one end at vacuum system interface (5) place is connected with reactor (9), and the other end is connected with cryogenic memory (8).
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|---|---|---|---|
| CN201510605559.1A CN105152134B (en) | 2015-09-22 | 2015-09-22 | A kind of method and device for preparing hydrogen fluoride |
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| CN201510605559.1A CN105152134B (en) | 2015-09-22 | 2015-09-22 | A kind of method and device for preparing hydrogen fluoride |
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| CN105152134B CN105152134B (en) | 2017-10-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115445536A (en) * | 2022-09-20 | 2022-12-09 | 北京理工大学 | Novel experiment method and experiment device for reaction of hydrogen and fluorine gas |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6346227B1 (en) * | 1999-02-12 | 2002-02-12 | Bayer Aktiengesellschaft | Process for preparing pure hydrofluoric acid |
| JP2007112683A (en) * | 2005-10-21 | 2007-05-10 | Morita Kagaku Kogyo Kk | Method of producing hydrogen fluoride using recovered calcium fluoride |
| CN201031140Y (en) * | 2007-01-08 | 2008-03-05 | 战玉柏 | Device for producing ultra-clear and high-purity |
| CN102923664A (en) * | 2012-11-27 | 2013-02-13 | 福州大学 | Method for producing hydrogen fluoride by virtue of gas-solid-liquid associative reaction method |
-
2015
- 2015-09-22 CN CN201510605559.1A patent/CN105152134B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6346227B1 (en) * | 1999-02-12 | 2002-02-12 | Bayer Aktiengesellschaft | Process for preparing pure hydrofluoric acid |
| JP2007112683A (en) * | 2005-10-21 | 2007-05-10 | Morita Kagaku Kogyo Kk | Method of producing hydrogen fluoride using recovered calcium fluoride |
| CN201031140Y (en) * | 2007-01-08 | 2008-03-05 | 战玉柏 | Device for producing ultra-clear and high-purity |
| CN102923664A (en) * | 2012-11-27 | 2013-02-13 | 福州大学 | Method for producing hydrogen fluoride by virtue of gas-solid-liquid associative reaction method |
Non-Patent Citations (1)
| Title |
|---|
| 王占前等: "氟化氢生产技术进展", 《化工生产与技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115445536A (en) * | 2022-09-20 | 2022-12-09 | 北京理工大学 | Novel experiment method and experiment device for reaction of hydrogen and fluorine gas |
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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Patentee after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Patentee before: PERIC SPECIAL GASES Co.,Ltd. |
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