CN208378429U - It is electrolysed HF and KHF2The system for generating fluorine gas purification graphite - Google Patents
It is electrolysed HF and KHF2The system for generating fluorine gas purification graphite Download PDFInfo
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- CN208378429U CN208378429U CN201820842296.5U CN201820842296U CN208378429U CN 208378429 U CN208378429 U CN 208378429U CN 201820842296 U CN201820842296 U CN 201820842296U CN 208378429 U CN208378429 U CN 208378429U
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Abstract
The utility model relates to be electrolysed HF and KHF2The system for generating fluorine gas purification graphite, including electrolysis cells I, electrolysis cells I include: electrolytic cell, and electrolyte bath adds HF and KHF2Mixture, intermediate to completely cut off gas intercommunication with diaphragm, the outside of electrolytic cell is provided with water-bath heater；Furnace body unit II, furnace body unit II includes: furnace body, the bottom of furnace body is disposed with furnace burdening, graphite products are placed at furnace core, the surrounding of graphite products is disposed with resistance material, insulation material is disposed on the outside of resistance material, the side of furnace body is provided with air inlet pipe a and air inlet pipe b for nitrogen and chlorine to be passed through to furnace core respectively, and the fluorine gas of generation is passed through the bottom of furnace core by link road a by electrolytic cell.The utility model generates fluorine gas using electrolysis and prior art is replaced to be passed through the step of freon is purified, guarantee to substantially reduce the adverse effect caused by environment in purification process while high-boiling-point impurity is removed again by increasing electrolysis section.
Description
Technical field:
The utility model relates to graphite preparation technical fields, more particularly to electrolysis HF and KHF2Fluorine gas is generated to mention
The system of pure graphite.
Background technique:
Existing technology status: existing purification graphite is all that gas heat purification, most metals halogenation are carried out in graphitization
The fusing point and boiling point of object are all relatively low, and especially some high-boiling-point impurities such as boron, vanadium, molybdenum, silicon etc. must pass through fluorination or chlorination
It can remove.When being graphitized purifying, generally reaches a timing in furnace core temperature and start to be passed through nitrogen, exclude the air in furnace core, so
After be passed through chlorine, freon and chlorine are passed through when reaching certain temperature to furnace core temperature again and is blown altogether, and then makes high-boiling-point impurity shape
It is discharged at boiling point is reduced after compound with gas.
But the freon that uses of the prior art can destroy ozone layer and lead to disruption of ecological balance, and need government using unit
Examine quota.
Utility model content:
The purpose of the utility model is to provide electrolysis HF and KHF2The system for generating fluorine gas purification graphite, by furnace body
Electrolytic cell is arranged in side, is passed into furnace body using the fluorine gas that electrolytic cell Inner electrolysis generates and is purified to graphite, and then solves
High-boiling-point impurity element is difficult to the problem of removing and causing the destruction to environment when being purified using freon in graphite.
It is electrolysed HF and KHF2The system that fluorine gas purifies graphite is generated, including electrolysis cells I, the electrolysis cells I include:
Electrolytic cell, the electrolyte bath add HF and KHF2Mixture, it is intermediate to completely cut off gas intercommunication, the electricity with diaphragm
The outside of solution slot is provided with water-bath heater；
Furnace body unit II, the furnace body unit II include:
Furnace body, the bottom of the furnace body are disposed with furnace burdening, and graphite products are placed at furnace core, the surrounding cloth of graphite products
It is equipped with resistance material, insulation material is disposed on the outside of resistance material, the side of the furnace body is provided with for respectively by nitrogen and chlorine
It is passed through the air inlet pipe a and air inlet pipe b of furnace core, the fluorine gas of generation is passed through the bottom of furnace core by link road a by the electrolytic cell.
As an improvement, online acidometer and hydrofluoric acid storage tank are provided at the top of the electrolytic cell, the online acidity
Hydrofluoric acid concentration in meter monitoring electrolytic cell, when concentration is too low, injects HF into electrolytic cell by hydrofluoric acid storage tank.
As another improvement, the side of the electrolytic cell is provided with hydrogen gas cleaner, and the hydrogen gas cleaner is for removing
The hydrogen fluoride carried secretly in the hydrogen that electrolytic cell emits；The side of the furnace body is provided with tail gas absorbing system, the tail gas
Absorption system is made of several sodium hydroxide solution absorbers, is used to remove the fluorine gas in the tail gas of graphitizing furnace discharge,
The tail gas absorbing system is provided on connecting tube b by being connected at the top of connecting tube b and furnace core for pumping gas in furnace core
To the air pump of tail gas absorbing system.
It should be noted that electrolytic cell is passed through the fluorine gas of furnace body, it is passed through the hydrogen and hydrofluoric acid storage tank of hydrogen gas cleaner
HF is injected into electrolytic cell, and uninterrupted is controlled by control valve.
In addition, the reaction equation in the utility model in electrolytic process is as follows:
Anode: 2F--2e-→F2↑
Cathode: 2HF2 -+2e-→H2↑+4F-。
It should be noted that replace freon to be purified using the fluorine gas generated in the utility model, for
Those skilled in the art it is contemplated that be passed into graphitizing furnace using air accumulator fluorine gas storage, then by the fluorine gas of air accumulator, but
This kind of mode firstly there are the problem of to be that fluorine gas vivaciously stores very much more difficult, can be very overcoming the cost of its storage
Height, even if the problem of overcoming cost again, with using, the pressure in tank can slowly decline the fluorine gas in air accumulator, with
The decline of pressure, the rate of gas supply can also decline, and are similar in life and use gas tank the same, use and will appear gas supply below not
The case where final firing can not burnt, air pump keep graphitizing furnace in negative pressure state it is certain in the case where, gassing rate deficiency is just difficult to
Guarantee the fluorine gas feed rate that graphite purification needs；
Assuming that the rate that cell reaction generates fluorine gas is V1, the rate that graphitizing furnace is passed through fluorine gas needs is V2, herein may be used
To guarantee that V1 is consistently greater than V2 by the process for artificially controlling cell reaction, negative pressure state one in graphitizing furnace is kept in air pump
In the case where fixed and V1 > V2, V1 suitably can be reduced by adjusting the valve on link road a, to guarantee in purification process
The rate stabilization that fluorine gas is passed through.
The utility model has the beneficial effects that:
(1) HF in electrolysis cell and KHF is utilized by setting electrolytic cell in the utility model2The mode of mixture produces
Fluorine gas is given birth to replace freon used in graphite purification process in the prior art, is passed into graphitizing furnace, makes in graphite
High-boiling-point impurity element compounds generate low boiling point fluoride and are discharged with gas, and which obviate freon in graphite production process
It is a large amount of to use, reduce the destruction to environment.
(2) rate that cell reaction generates fluorine gas in the utility model is assumed to be V1, and graphitizing furnace is passed through fluorine gas needs
Rate is V2, can guarantee that V1 is consistently greater than V2 by artificially controlling the process of cell reaction herein, to guarantee to purify
The rate holds steady that fluorine gas is passed through in journey.
(3) furthermore HF and KHF used in the utility model2Relative to freon, it is easier to obtain, and needs using i.e.
HF and KHF can be rapidly joined2It carries out electrolysis and generates fluorine gas, overcome interim in use, then freon, which needs to examine, transports week
The problem of turning, influencing production efficiency；And cell reaction is easy to control, and energization when needing to generate fluorine gas can stop when not needing
It is powered and stops fluorine gas supply at once, it is more convenient.
(4) and in the utility model the product for being electrolysed generation is relatively stable, will not pollute to graphite, use stabilization
Property it is good, the graphite quality produced is high.
In conclusion the utility model has process optimization, device structure is simple, graphite macromolecule impurity removal effect
Well, it the advantages that environmentally friendly, is particularly suitable in isostatic pressing formed graphite purifying process technology.
Detailed description of the invention:
The utility model is described further with reference to the accompanying drawing:
Fig. 1 is electrolysis HF and KHF2Generate the process flow chart of fluorine gas purification graphite；
Fig. 2 is electrolysis HF and KHF2Generate the system schematic of fluorine gas purification graphite.
Specific embodiment:
As described below is only the preferred embodiment of the utility model, is not defined to the scope of the utility model.
Embodiment one
As shown in Figure 1, electrolysis HF and KHF2The technique for generating fluorine gas purification graphite, comprises the following production steps that
One, electrolysis section: by HF and KHF21:3 carries out being mixed to form electrolyte in molar ratio, is put into electrolytic cell, wherein
The concentration of HF is maintained at 38%~40%, and fluorine gas electrolytic cell is all made of the Hastelloy of heat-and corrosion-resistant or similar material,
Electrolysis electrode is installed on electrolytic cell both sides respectively, and anode is nickel plate, and cathode is stainless steel plate；By water-bath heater to electrolytic cell into
Row heating, heating temperature make the HF and KHF of electrolyte bath at 80 DEG C~95 DEG C2Reach molten condition, opens power supply to electrolysis
Liquid carries out electrolysis and generates fluorine gas；
Reaction equation in electrolytic process is as follows:
Anode: 2F--2e-→F2↑
Cathode: 2HF2 -+2e-→H2↑+4F-；
Two, graphitization/purification part: the spacing of multiple groups graphite product as requested is arranged in graphitizing furnace, successively
Insulation material and resistance material are inserted, after shove charge, heating graphitizing furnace to furnace core temperature is passed through nitrogen when being 1800~1900 DEG C
The air in furnace core is excluded, heating rate is 10~30 DEG C/min；Continue to heat graphitizing furnace when being warming up to 1900~2000 DEG C,
Stopping is passed through chlorine, switchs to be passed through chlorine；Continue to heat graphitizing furnace when being warming up to 2300~2500 DEG C, will be electrolysed in step 1
The fluorine gas of generation is passed through in graphitizing furnace, keeps micro-vacuum state during being passed through fluorine gas and being purified in graphitizing furnace,
Chlorine and fluorine gas are diffused in product by graphitizing furnace bottom, and wherein chlorine supplies gas unit consumption as 20~25kg/m3, fluorine gas supplies gas list
Consumption is 15-20kg/m3；Wherein the impurity element chemical combination in fluorine gas and sample, which generates fluoride, reduces its boiling point；By taking boron as an example,
Boiling point is greater than 3500 DEG C, reacts with fluorine gas, 2B+3F2→2BF3, -127.1 DEG C of the boron fluoride boiling point of generation.
It further, further include vent gas treatment part, the mixed gas generated in step 2 is passed into tail gas absorbing system
It is discharged after the middle removal by fluorine gas therein；It further include hydrogen purification part, the hydrogen of generation is electrolysed in step 1, and to enter hydrogen net
It is discharged after changing the hydrogen fluoride that device removal is wherein carried secretly, wherein tail gas absorbing system is by several sodium hydroxide solution absorber groups
At fluorine gas reacts removal, equation 2F with sodium hydroxide2+4NaOH→NaF+2H2O+O2, the molten people of the fluoride of gasification is water-soluble
In liquid, after absorption system, after tail gas reaches discharge standard, it is discharged into air.
Further, further include feed supplement part, in step 1 during electrolysis, pass through the monitoring electrolysis of online acidometer
Hydrofluoric acid concentration in slot when concentration is too low, injects hydrofluoric acid by hydrofluoric acid storage tank in electrolytic cell.
It is noted that, by the way that electrolytic cell is arranged, utilizing HF in electrolysis cell and KHF in the present embodiment2Mixing
The mode of object generates fluorine gas to replace freon used in graphite purification process in the prior art, is passed into graphitizing furnace,
The high-boiling-point impurity element compounds in graphite are made to generate low boiling point fluoride and be discharged with gas, which obviate graphite production processes
A large amount of uses of middle freon, reduce the destruction to environment；
In addition, HF and KHF used in the present embodiment2Relative to freon, it is easier to obtain, and needs use fast
HF and KHF is added in speed2It carries out electrolysis and generates fluorine gas, overcome interim in use, freon needs to examine then transport turnover, shadow
The problem of ringing production efficiency；And cell reaction is easy to control, and energization when needing to generate fluorine gas can stop energization horse when not needing
Upper stopping fluorine gas supply, it is more convenient；
And the product that generation is electrolysed in the present embodiment is relatively stable, will not pollute to graphite, and stability in use is good,
The graphite quality produced is high.
Embodiment two
It is electrolysed the method that HF and KHF2 generates fluorine gas purification graphite, is comprised the following production steps that
One, electrolysis section: by HF and KHF21:3 carries out being mixed to form electrolyte in molar ratio, is put into electrolytic cell, wherein
The concentration of HF is maintained at 38%~40%, and fluorine gas electrolytic cell is all made of the Hastelloy of heat-and corrosion-resistant or similar material,
Electrolysis electrode is installed on electrolytic cell both sides respectively, and anode is nickel plate, and cathode is stainless steel plate；
Two, graphitization/purification part: the spacing of multiple groups graphite product as requested is arranged in graphitizing furnace, successively
Insulation material and resistance material are inserted, after shove charge, heating graphitizing furnace to furnace core temperature is passed through nitrogen when being 1800~1900 DEG C
The air in furnace core is excluded, heating rate is 10~30 DEG C/min；Continue to heat graphitizing furnace when being warming up to 1900~2000 DEG C,
Stopping is passed through chlorine, switchs to be passed through chlorine；Continue to heat graphitizing furnace when being warming up to 2300~2500 DEG C, the electrolysis to step 1
Slot is heated by water-bath heater, and heating temperature makes the HF and KHF of electrolyte bath at 80 DEG C~95 DEG C2Reach melting
State opens power supply and carries out electrolysis generation fluorine gas to electrolyte；
Reaction equation in electrolytic process is as follows:
Anode: 2F--2e-→F2↑
Cathode: 2HF2 -+2e-→H2↑+4F-；,
The fluorine gas of generation is passed through in graphitizing furnace, keeps micro- negative in graphitizing furnace during being passed through fluorine gas and being purified
Pressure condition, chlorine and fluorine gas are diffused in product by graphitizing furnace bottom, and wherein chlorine supplies gas unit consumption as 20~25kg/m3, fluorine
Pneumatic transmission gas unit consumption is 15-20kg/m3；Wherein the impurity element chemical combination in fluorine gas and sample, which generates fluoride, reduces its boiling point；With
For boron, boiling point is greater than 3500 DEG C, reacts with fluorine gas, 2B+3F2→2BF2, -127.1 DEG C of the boron fluoride boiling point of generation.
It further, further include vent gas treatment part, the mixed gas generated in step 2 is passed into tail gas absorbing system
It is discharged after the middle removal by fluorine gas therein；It further include hydrogen purification part, the hydrogen of generation is electrolysed in step 1, and to enter hydrogen net
It is discharged after changing the hydrogen fluoride that device removal is wherein carried secretly, wherein tail gas absorbing system is by several sodium hydroxide solution absorber groups
At fluorine gas reacts removal, equation 2F with sodium hydroxide2+4NaOH→NaF+2H2O+O2, the molten people of the fluoride of gasification is water-soluble
In liquid, after absorption system, after tail gas reaches discharge standard, it is discharged into air.
Further, further include feed supplement part, in step 1 during electrolysis, pass through the monitoring electrolysis of online acidometer
Hydrofluoric acid concentration in slot when concentration is too low, injects hydrofluoric acid by hydrofluoric acid storage tank in electrolytic cell.
Embodiment three
As shown in Fig. 2, electrolysis HF and KHF2The system for generating fluorine gas purification graphite, including electrolysis cells I, the electrolysis are single
First I includes:
Electrolytic cell 1 adds HF and KHF inside the electrolytic cell 12Mixture, centre completely cut off gas intercommunication, institute with diaphragm 2
The outside for stating electrolytic cell 1 is provided with water-bath heater 3；
Furnace body unit II, the furnace body unit II include:
Furnace body 4, the bottom of the furnace body 4 are disposed with furnace burdening 41, and graphite products are placed at furnace core 42, graphite products
Surrounding is disposed with resistance material 43, and the outside of resistance material 43 is disposed with insulation material 44, and the side of the furnace body 4 is provided with for distinguishing
Nitrogen and chlorine are passed through to the air inlet pipe a5 and air inlet pipe b6 of furnace core 42, the electrolytic cell 1 passes through link road a7 for the fluorine of generation
Gas is passed through the bottom of furnace core 42.
Further, the top of the electrolytic cell 1 is provided with online acidometer 8 and hydrofluoric acid storage tank 9, the online acid
Hydrofluoric acid concentration in 8 monitoring electrolytic cell 1 of degree meter, when concentration is too low, injects HF into electrolytic cell 1 by hydrofluoric acid storage tank 9.
Further, the side of the electrolytic cell 1 is provided with hydrogen gas cleaner 10, and the hydrogen gas cleaner 10 is for clear
The hydrogen fluoride carried secretly in the hydrogen emitted except electrolytic cell 1；The side of the furnace body 4 is provided with tail gas absorbing system 11, institute
It states tail gas absorbing system 11 to be made of several sodium hydroxide solution absorbers, in the tail gas for being used to remove graphitizing furnace discharge
Fluorine gas, the tail gas absorbing system 11 is provided on connecting tube b12 and is used for by being connected at the top of connecting tube b12 and furnace core 42
Gas in furnace core 42 is pumped to the air pump 13 of tail gas absorbing system 11.
It is above only preferred embodiments of the present invention in conjunction with described in attached drawing, but the utility model is not limited to
State embodiment, it is noted that for those skilled in the art, under the premise of not departing from the utility model structure,
Various changes and improvements can be also made, these also should be considered as the protection scope of the utility model, and it is practical new all to will not influence this
The effect and practicability that type is implemented.
Claims (3)
1. being electrolysed HF and KHF2The system for generating fluorine gas purification graphite, it is characterised in that: including electrolysis cells I, the electrolysis cells
I includes:
Electrolytic cell (1), the electrolytic cell (1) is internal to add HF and KHF2Mixture, intermediate diaphragm (2) completely cut off gas intercommunication, institute
The outside for stating electrolytic cell (1) is provided with water-bath heater (3)；
Furnace body unit II, the furnace body unit II include:
The bottom of furnace body (4), the furnace body (4) is disposed with furnace burdening (41), and graphite products are placed at furnace core (42), and graphite produces
The surrounding of product is disposed with resistance material (43), is disposed on the outside of resistance material (43) insulation material (44), and the side of the furnace body (4) is set
It is equipped with the air inlet pipe a (5) and air inlet pipe b (6) for nitrogen and chlorine to be passed through to furnace core (42) respectively, the electrolytic cell (1) is logical
Cross the bottom that the fluorine gas of generation is passed through furnace core (42) by link road a (7).
2. electrolysis HF and KHF as described in claim 12The system for generating fluorine gas purification graphite, it is characterised in that: the electrolysis
Online acidometer (8) and hydrofluoric acid storage tank (9) are provided at the top of slot (1), the online acidometer (8) monitors electrolytic cell
(1) interior hydrofluoric acid concentration when concentration is too low, injects HF into electrolytic cell (1) by hydrofluoric acid storage tank (9).
3. electrolysis HF and KHF as described in claim 12The system for generating fluorine gas purification graphite, it is characterised in that: the electrolysis
The side of slot (1) is provided with hydrogen gas cleaner (10), and the hydrogen gas cleaner (10) is for removing what electrolytic cell (1) emitted
The hydrogen fluoride carried secretly in hydrogen；The side of the furnace body (4) is provided with tail gas absorbing system (11), the tail gas absorbing system
(11) it is made of several sodium hydroxide solution absorbers, is used to remove the fluorine gas in the tail gas of graphitizing furnace discharge, it is described
Tail gas absorbing system (11) is provided on connecting tube b (12) by being connected at the top of connecting tube b (12) and furnace core (42) for inciting somebody to action
Furnace core (42) interior gas pumps to the air pump (13) of tail gas absorbing system (11).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201820842296.5U CN208378429U (en) | 2018-06-01 | 2018-06-01 | It is electrolysed HF and KHF2The system for generating fluorine gas purification graphite |
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| CN201820842296.5U CN208378429U (en) | 2018-06-01 | 2018-06-01 | It is electrolysed HF and KHF2The system for generating fluorine gas purification graphite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516544A (en) * | 2018-06-01 | 2018-09-11 | 中钢集团新型材料（浙江）有限公司 | It is electrolysed HF and KHF2Generate the method and system of fluorine gas purification graphite |
| CN112239205A (en) * | 2019-07-17 | 2021-01-19 | 侯梦斌 | Graphite purification equipment and technology for intervening sodium chloride electrolysis |
-
2018
- 2018-06-01 CN CN201820842296.5U patent/CN208378429U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516544A (en) * | 2018-06-01 | 2018-09-11 | 中钢集团新型材料（浙江）有限公司 | It is electrolysed HF and KHF2Generate the method and system of fluorine gas purification graphite |
| CN112239205A (en) * | 2019-07-17 | 2021-01-19 | 侯梦斌 | Graphite purification equipment and technology for intervening sodium chloride electrolysis |
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Address after: 313100 9 Zhonggang Avenue, Chicheng Town, Changxing County, Huzhou City, Zhejiang Province Patentee after: Sinosteel new materials Co.,Ltd. Address before: 313100 9 Zhonggang Avenue, Chicheng Town, Changxing County, Huzhou City, Zhejiang Province Patentee before: SINOSTEEL CORPORATION NEW MATERIAL (ZHEJIANG) Co.,Ltd. |
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Address after: 313100 9 Zhonggang Avenue, Chicheng Town, Huzhou City, Zhejiang Province Patentee after: Symantec Advanced Materials Co.,Ltd. Address before: 313100 9 Zhonggang Avenue, Chicheng Town, Changxing County, Huzhou City, Zhejiang Province Patentee before: Sinosteel new materials Co.,Ltd. |