CN105152134B - A kind of method and device for preparing hydrogen fluoride - Google Patents
A kind of method and device for preparing hydrogen fluoride Download PDFInfo
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- CN105152134B CN105152134B CN201510605559.1A CN201510605559A CN105152134B CN 105152134 B CN105152134 B CN 105152134B CN 201510605559 A CN201510605559 A CN 201510605559A CN 105152134 B CN105152134 B CN 105152134B
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Abstract
The present invention relates to a kind of method and device for preparing hydrogen fluoride, belong to chemical technology field.Methods described step is：Vacuumize process first is carried out to whole reaction unit, then liquid feeding phase fluorination hydrogen is into reactor；Fluorine gas is added to the upper gaseous phase space of reactor, the pressure to reactor is 0.2~0.5MPa, the temperature for controlling reactor is 40~40 DEG C；Flow is added to reactor liquid Space for 0.1~10L/min hydrogen, after hydrogen is by gas distributor, is reacted with fluorine gas in liquid phase plane intersection, obtains the hydrogen fluoride.Described device is mainly made up of raw material gas inlet I, raw material gas inlet II, flow meter I, cooling liquid inlet, flow meter II, cooling liquid outlet, chuck, reactor, gas distributor, heat exchanger, vacuum system interface, flowmeter III and cryogenic memory.Device of the present invention, can realize the direct reaction of fluorine gas and hydrogen, safe operation, the fluorination hydrogen purity of preparation is high, and is adapted to large-scale production.
Description
Technical field
The present invention relates to a kind of method and device for preparing hydrogen fluoride, belong to chemical technology field.
Background technology
Hydrogen fluoride is a kind of chemicals of extensive application, and its main application fields is as follows：(1) as preparation containing fluorination
The raw material of compound, is to prepare villiaumite, containing fluorinated refrigerant, fluoro-containing plastic, fluorine-containing rubber, fluorine resin and fluorine-containing medicines or agriculture
The Fluorine source of the materials such as medicine；(2) as highly acid corrosive agent, for etching glass, acid-washed metal and etching semiconductor surface；
(3) as the catalyst for being alkylated reaction；(4) as analytical reagent；(5) as purge gas.
Industrial hydrogen fluoride is generated by fluorite and sulfuric acid heating response：
CaF2+H2SO4→2HF+CaSO4
Hydrogen fluoride is prepared using such a method, and production cost is low and HF that prepare can meet general industry application requirement.But
It is that the raw material used in this method contains more impurity, the impurity such as arsenic therein, sulfide, phosphoric acid passes through conventional purifying side
Method is extremely difficult except relatively low value is gone to, and causes the HF purity prepared low.In Application to Electronic Industry, the purity and cleanliness factor of hydrogen fluoride
Tremendous influence is suffered to the yield rate of integrated circuit, electrical property and reliability.Moreover, with electronics, information, communications industry
Fast development, electronics industry is to the purity of hydrogen fluoride and the requirement more and more higher of cleanliness factor.
The fluorination hydrogen purity directly synthesized using fluorine gas and hydrogen is higher, is suitable as electronic grade high-purity anhydrous hydrogen fluoride
Unstripped gas.Because fluorine gas and hydrogen reaction are violent, it will be exploded once contact, dangerous high, institute in this way one
Directly it is not carried out industrialized application.Control the speed that reaction is carried out and the key point that uniformity coefficient is this synthetic method.
The content of the invention
For defect present in prior art, an object of the present invention is to provide a kind of side for preparing hydrogen fluoride
Method, methods described can realize the direct reaction of fluorine gas and hydrogen, and prepared fluorination hydrogen purity is high, can meet electronics industry to fluorine
Change the requirement of hydrogen high-purity.
The second object of the present invention is to provide a kind of device for preparing hydrogen fluoride, described device safe operation, and is adapted to
The large-scale production of high-purity hydrogen fluoride.
The purpose of the present invention is achieved through the following technical solutions.
A kind of method for preparing hydrogen fluoride, methods described step is as follows：
Step 1. first carries out vacuumize process to whole reaction unit, and then liquid feeding phase fluorination hydrogen is into reactor lower part；
The volume of liquid-phase fluorination hydrogen is the 20%~80% of reactor volume；
Fluorine gas is added to the upper gaseous phase space of reactor by step 2., and into reactor, pressure is 0.2~0.5MPa；
Step 3. controls the temperature of reactor to be -40~40 DEG C, and flow is added to instead for 0.1~10L/min hydrogen
The liquid Space of device bottom is answered, is reacted with fluorine gas in liquid phase plane intersection, obtains the hydrogen fluoride.
The volume of reactor described in step 1 preferably 10~2000L.
The volume of liquid-phase fluorination hydrogen described in step 1 is preferably the 40%~60% of reactor volume.
Pressure preferably 0.3~0.4MPa in reactor described in step 2.
Preferably -20~20 DEG C of the temperature of reactor described in step 3.
The flow of hydrogen described in step 3 preferably 1~3L/min.
Preferably, hydrogen described in step 3 is added to the liquid Space of reactor lower part, by existing after gas distributor with fluorine gas
Liquid phase plane intersection reacts.
Preferably, when the pressure of question response device is 0.1~0.15MPa, stop adding hydrogen；Add fluorine gas into reactor,
To reactor pressure be 0.5MPa after, continuously add hydrogen.
Preferably, when the hydrogen fluoride liquid phase volume of generation is the 10%~20% of reactor volume, stop adding hydrogen；
Volume is transferred to cryogenic memory for 10%~20% liquid-phase fluorination hydrogen of reactor volume by pipeline and metered flow
In.
A kind of device for preparing hydrogen fluoride of the present invention, described device is mainly by 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,
Heat exchanger 6, vacuum system interface 5, flowmeter III 11 and cryogenic memory 8 are constituted.
Wherein, the line end being connected with raw material gas inlet II 2 stretches into the liquid Space of the bottom of reactor 9, and and gas
Distributor 7 is connected；Valve, flow meter I 12 are sequentially provided with pipeline behind raw material gas inlet II 2；Where flowmeter III 11
Pipeline one end is connected with the liquid Space of the bottom of reactor 9, and below gas distributor 7, the other end and cryogenic memory 8
Top be connected；Gas distributor 7 is in the lower liquid phase space of reactor 9, and under the liquid level of liquid Space；Reactor 9
Bottom is in the inside of chuck 10；Thermometer is located at the liquid level of the liquid Space of reactor 9 in the outside of reactor 9 and chuck 10
On；Gas-phase space of the heat exchanger 6 on the top of reactor 9；The pipeline being connected with cooling liquid inlet 3 import respectively with heat exchanger 6,
It is connected by the outside of reactor 9 with the pipeline import inside chuck 10；The outlet of heat exchanger 6, pass through the outside of reactor 9 and chuck
Tube outlet inside 10 is connected with the pipeline where cooling liquid outlet 4 respectively；Pipeline behind cooling liquid inlet 3 is provided with stream
Gauge II 13；The line end being connected with raw material gas inlet I 1 stretches into the upper gaseous phase space of reactor 9；Pressure gauge is in reactor
9 outside, and be connected with the gas-phase space on the top of reactor 9；Pipeline one end and the phase of reactor 9 where vacuum system interface 5
Even, the other end is connected with cryogenic memory 8.
Beneficial effect：
In method of the present invention, hydrogen and fluorine gas are completely cut off by liquid-phase fluorination hydrogen, it is to avoid the direct contact of the two；It is logical
Crossing gas distributor makes gas be evenly distributed；And by control hydrogen flow control reaction speed so that realize fluorine gas and
The direct reaction of hydrogen, is made the hydrogen fluoride of high-purity.
Device of the present invention, safe operation is adapted to the large-scale production of high-purity hydrogen fluoride.
Brief description of the drawings
Fig. 1 is fluorinated the structural representation of hydrogen production device for present invention synthesis.
In figure, 1- raw material gas inlets I, 2- raw material gas inlets II, 3- cooling liquid inlets, 4- cooling liquid outlets, 5- vacuum system
System interface, 6- heat exchangers, 7- gas distributors, 8- cryogenic memories, 9- reactors, 10- chucks, 11- flowmeters III, 12- streams
Gauge I, 13- flow meter IIs.
Embodiment
Below in conjunction with the accompanying drawings with specific embodiment the present invention is described in further detail explanation.
In following examples：
Coolant used is ethylene glycol.
As shown in figure 1, the device that hydrogen fluoride is prepared in embodiment is main by raw material gas inlet I 1, raw material gas inlet II 2, stream
Gauge I 12, cooling liquid inlet 3, flow meter II 13, cooling liquid outlet 4, chuck 10, reactor 9, gas distributor 7, heat exchanger
6th, vacuum system interface 5, flowmeter III 11 and cryogenic memory 8 are constituted.
Wherein, the line end being connected with raw material gas inlet II 2 stretches into the liquid Space of the bottom of reactor 9, and and gas
Distributor 7 is connected；Valve, flow meter I 12 are sequentially provided with pipeline behind raw material gas inlet II 2；Where flowmeter III 11
Pipeline one end is connected with the liquid Space of the bottom of reactor 9, and below gas distributor 7, the other end and cryogenic memory 8
Top be connected；Gas distributor 7 is in the lower liquid phase space of reactor 9, and under the liquid level of liquid Space；Reactor 9
Bottom is in the inside of chuck 10；Thermometer is located at the liquid level of the liquid Space of reactor 9 in the outside of reactor 9 and chuck 10
On；Gas-phase space of the heat exchanger 6 on the top of reactor 9；The pipeline being connected with cooling liquid inlet 3 import respectively with heat exchanger 6,
It is connected by the outside of reactor 9 with the pipeline import inside chuck 10；The outlet of heat exchanger 6, pass through the outside of reactor 9 and chuck
Tube outlet inside 10 is connected with the pipeline where cooling liquid outlet 4 respectively；Pipeline behind cooling liquid inlet 3 is provided with stream
Gauge II 13；The line end being connected with raw material gas inlet I 1 stretches into the upper gaseous phase space of reactor 9；Pressure gauge is in reactor
9 outside, and be connected with the gas-phase space on the top of reactor 9；Pipeline one end and the phase of reactor 9 where vacuum system interface 5
Even, the other end is connected with cryogenic memory 8.
The technological process for preparing hydrogen fluoride is：The whole reaction unit of 5 pairs of vacuum system interface is first passed through to carry out vacuumizing place
Reason；Liquid-phase fluorination hydrogen is added to by raw material gas inlet I 1 in the bottom of reactor 9 that volume is 10~2000L, to the body of reactor 9
Long-pending 20%~80%；Fluorine gas is passed through into reactor 9 by raw material gas inlet I 1, to reactor 9 pressure for 0.1~
0.5MPa；The coolant rate of cooling liquid inlet 3 is adjusted by flow meter II 13, coolant is respectively through heat exchanger 6, positioned at anti-
Flowed out after answering the pipeline inside the outside of device 9 and chuck 10 by cooling liquid outlet 4, so as to control the temperature of reactor 9-40~40
℃；By raw material gas inlet II 2 and flow meter I 12, the hydrogen that flow is 0.1~10L/min is added to reactor 9, hydrogen leads to
Cross after gas distributor 7, reacted with fluorine gas in liquid phase plane intersection, generate hydrogen fluoride；With the progress of reaction, reactor 9
Pressure be gradually reduced, when pressure is reduced to 0.1~0.15MPa, stop add hydrogen；Into reactor 9 plus fluorine gas is to anti-
The pressure of device 9 is answered after 0.5MPa, to continuously add hydrogen；When the hydrogen fluoride liquid phase volume of generation is the 10% of the volume of reactor 9
When~20%, stop adding hydrogen, volume is passed through into flowmeter III for 10%~20% liquid-phase fluorination hydrogen of the volume of reactor 9
11 metered flows are transferred in cryogenic memory 8.
Embodiment 1
Carried out by 5 pairs of whole reaction units of vacuum system interface after vacuumize process, will by raw material gas inlet I 1
100L liquid-phase fluorination hydrogen adds volume in the 200L bottom of reactor 9；It is passed through by raw material gas inlet I 1 into reactor 9
Fluorine gas, is 0.5MPa to the pressure of reactor 9；By controlling the coolant rate of cooling liquid inlet 3, make the temperature of reactor 9-
20~20 DEG C；By raw material gas inlet II 2, the hydrogen that flow is 2L/min is added to reactor 9, hydrogen passes through gas distributor
After 7, reacted with fluorine gas in liquid phase plane intersection, generate hydrogen fluoride；With the progress of reaction, the pressure of reactor 9 gradually subtracts
It is small, when pressure is reduced to 0.15MPa, stop adding hydrogen；Add fluorine gas into reactor 9, the pressure to reactor 9 is
After 0.5MPa, hydrogen is continuously added；When the hydrogen fluoride liquid phase volume of generation is 20L, stop adding hydrogen, by 20L liquid phase fluorines
Change hydrogen to be transferred in cryogenic memory 8 by the metered flow of flowmeter III 11.
Embodiment 2
Carried out by the whole reaction units of 5 pairs of vacuum system interface after vacuumize processs, by raw material gas inlet I 1 by 8L
Liquid-phase fluorination hydrogen add volume for 10L the bottom of reactor 9 in；Fluorine gas is passed through into reactor 9 by raw material gas inlet I 1,
It is 0.4MPa to the pressure of reactor 9；By controlling the coolant rate of cooling liquid inlet 3, make the temperature of reactor 9-40~
40℃；By raw material gas inlet II 2, the hydrogen that flow is 0.1L/min is added to reactor 9, hydrogen passes through gas distributor 7
Afterwards, reacted with fluorine gas in liquid phase plane intersection, generate hydrogen fluoride；With the progress of reaction, the pressure of reactor 9 gradually subtracts
It is small, when pressure is reduced to 0.1MPa, stop adding hydrogen；Add fluorine gas into reactor 9, the pressure to reactor 9 is
After 0.5MPa, hydrogen is continuously added；When the hydrogen fluoride liquid phase volume of generation is 2L, stop adding hydrogen, by 2L liquid-phase fluorinations
Hydrogen is transferred in cryogenic memory 8 by the metered flow of flowmeter III 11.
Embodiment 3
Carried out by 5 pairs of whole reaction units of vacuum system interface after vacuumize process, will by raw material gas inlet I 1
400L liquid-phase fluorination hydrogen adds volume in the 2000L bottom of reactor 9；Led to by raw material gas inlet I 1 into reactor 9
Enter fluorine gas, be 0.2MPa to the pressure of reactor 9；By controlling the coolant rate of cooling liquid inlet 3, make the temperature of reactor 9
At -40~40 DEG C；By raw material gas inlet II 2, the hydrogen that flow is 10L/min is added to reactor 9, hydrogen passes through gas point
After cloth device 7, reacted with fluorine gas in liquid phase plane intersection, generate hydrogen fluoride；With the progress of reaction, the pressure of reactor 9 by
It is decrescence small, when pressure is reduced to 0.1MPa, stop adding hydrogen；Add fluorine gas into reactor 9, the pressure to reactor 9 is
After 0.5MPa, hydrogen is continuously added；When the hydrogen fluoride liquid phase volume of generation is 300L, stop adding hydrogen, by 300L liquid phases
Hydrogen fluoride is transferred in cryogenic memory 8 by the metered flow of flowmeter III 11.
Presently preferred embodiments of the present invention is these are only, is not intended to limit the scope of the present invention.It is all in this hair
Within bright spirit and principle, any modification, equivalent substitution and improvement for being made etc. are all contained in protection scope of the present invention
Within.
Claims (9)
1. a kind of method for preparing hydrogen fluoride, it is characterised in that：Methods described step is as follows：
Step 1. first carries out vacuumize process to whole reaction unit, and then liquid feeding phase fluorination hydrogen is into reactor lower part；Liquid phase
The volume of hydrogen fluoride is the 20%~80% of reactor volume；
Fluorine gas is added to the upper gaseous phase space of reactor by step 2., and into reactor, pressure is 0.2~0.5MPa；
Step 3. controls the temperature of reactor to be -40~40 DEG C, and flow is added into reactor for 0.1~10L/min hydrogen
Lower liquid phase space, hydrogen obtains the fluorine by being reacted after gas distributor with fluorine gas in liquid phase plane intersection
Change hydrogen.
2. a kind of method for preparing hydrogen fluoride according to claim 1, it is characterised in that：The pressure of question response device is 0.1
During~0.15MPa, stop adding hydrogen；Into reactor plus fluorine gas, to reactor pressure be 0.5MPa after, continuously add hydrogen
Gas.
3. a kind of method for preparing hydrogen fluoride according to claim 1, it is characterised in that：When the hydrogen fluoride liquid phase body of generation
When product is the 10%~20% of reactor volume, stop adding hydrogen；By 10%~20% liquid that volume is reactor volume
Phase fluorination hydrogen is transferred in cryogenic memory by pipeline and metered flow.
4. a kind of method for preparing hydrogen fluoride according to claim 1, it is characterised in that：The volume of the reactor is 10
~2000L.
5. a kind of method for preparing hydrogen fluoride according to claim 1, it is characterised in that：Liquid-phase fluorination hydrogen described in step 1
Volume be reactor volume 40%~60%.
6. a kind of method for preparing hydrogen fluoride according to claim 1, it is characterised in that：The pressure of reactor described in step 2
Power is 0.3~0.4MPa.
7. a kind of method for preparing hydrogen fluoride according to claim 1, it is characterised in that：The temperature of reactor described in step 3
Spend for -20~20 DEG C.
8. a kind of method for preparing hydrogen fluoride according to claim 1, it is characterised in that：The flow of hydrogen described in step 3
For 1~3L/min.
9. a kind of device that hydrogen fluoride is prepared using the method for preparing hydrogen fluoride as claimed in claim 1, it is characterised in that：Institute
State device main by 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), heat exchanger (6), vacuum system interface
(5), flowmeter III (11) and cryogenic memory (8) composition；
Wherein, the line end being connected with raw material gas inlet II (2) stretches into the liquid Space of reactor (9) bottom, and and gas
Distributor (7) is connected；Valve, flow meter I (12) are sequentially provided with pipeline behind raw material gas inlet II (2)；Flowmeter III
(11) pipeline one end where is connected with the liquid Space of the bottom of reactor 9, and below gas distributor (7), the other end
It is connected with the top of cryogenic memory (8)；Gas distributor (7) is in the lower liquid phase space of reactor (9), and in liquid Space
Liquid level under；Inside of the bottom of reactor (9) in chuck (10)；Thermometer in the outside of reactor (9) and chuck (10), and
On the liquid level of reactor (9) liquid Space；Gas-phase space of the heat exchanger (6) on reactor (9) top；With cooling liquid inlet
(3) import respectively with heat exchanger (6) of connected pipeline, pass through that reactor (9) is outside and chuck (10) inside pipeline import
It is connected；The outlet of heat exchanger (6), by reactor (9) is outside and chuck (10) inside tube outlet go out respectively with coolant
Pipeline where mouth (4) is connected；Pipeline behind cooling liquid inlet (3) is provided with flow meter II (13)；With raw material gas inlet I
(1) connected line end stretches into the upper gaseous phase space of reactor (9)；Pressure gauge in the outside of reactor (9), and with reaction
The gas-phase space on device (9) top is connected；Pipeline one end where vacuum system interface (5) is connected with reactor (9), the other end with
Cryogenic memory (8) is connected.
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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 true CN105152134B (en) | 2017-10-13 |
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| 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6346227B1 (en) * | 1999-02-12 | 2002-02-12 | Bayer Aktiengesellschaft | Process for preparing pure hydrofluoric acid |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4652948B2 (en) * | 2005-10-21 | 2011-03-16 | 森田化学工業株式会社 | Method for producing hydrogen fluoride using recovered calcium fluoride |
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2015
- 2015-09-22 CN CN201510605559.1A patent/CN105152134B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6346227B1 (en) * | 1999-02-12 | 2002-02-12 | Bayer Aktiengesellschaft | Process for preparing pure hydrofluoric acid |
| 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 |
|---|
| 氟化氢生产技术进展;王占前等;《化工生产与技术》;20091231;第16卷(第6期);第1-5页 * |
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Effective date of registration: 20190703 Address after: 057550 No. 1 Weiwu Road, Chemical Industry Agglomeration Area, Feixiang County, Handan City, Hebei Province Patentee after: CSIC (Handan) Perry Special Gas Co. Ltd Address before: 056027 17 Exhibition Road, Handan, Hebei Patentee before: No.718 Inst., China Shipping Heavy Industry Group Co. |
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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. |