CN108483441A - Potassium hexafluoromanganate and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether - Google Patents
Potassium hexafluoromanganate and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether Download PDFInfo
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- CN108483441A CN108483441A CN201810555995.6A CN201810555995A CN108483441A CN 108483441 A CN108483441 A CN 108483441A CN 201810555995 A CN201810555995 A CN 201810555995A CN 108483441 A CN108483441 A CN 108483441A
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- reactor
- fluorine gas
- graphite
- furnace
- antimony pentafluoride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/20—Fluorine
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The present invention relates to potassium hexafluoromanganate and the antimony pentafluoride systems that heat production fluorine gas purifies graphite altogether, including fluorine gas reaction member I, fluorine gas reaction member I to include：Reactor and vacuum pump for being vacuumized to reactor, the outside of reactor are equipped with heater and furnace body unit II for being heated to reactor, and furnace body unit II includes：Furnace body, the bottom of furnace body is disposed with furnace burdening, graphite products are positioned at furnace core, graphite products surrounding 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 reactor reaction generates fluorine gas, and fluorine gas is passed through the impurity element in the bottom removal graphite products of furnace core.The present invention by the way that chemical reactor is arranged in the side of graphitizing furnace, using in reactor potassium hexafluoromanganate and antimony pentafluoride heat production fluorine gas purifies graphite in stove altogether, avoid the problem of being damaged to environment using freon.
Description
Technical field：
The present invention relates to graphite purification technical field, more particularly to potassium hexafluoromanganate and antimony pentafluoride heat productions altogether
The system that fluorine gas purifies graphite.
Background technology：
Existing technology status：Existing purification graphite is purified into promoting the circulation of qi heat in graphitization, most metals halogenation
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 chlorination and fluorination
It could remove.When being graphitized purifying, generally reaches a timing in furnace core temperature and starts to be passed through nitrogen, exclude the air in furnace core,
Chlorine is then passed to, freon and chlorine is passed through when reaching certain temperature to furnace core temperature again and blows altogether, and then make high-boiling-point impurity
Reduction boiling point is discharged with gas after forming compound.
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.
Invention content：
The purpose of the present invention is in view of the deficiencies of the prior art, provide potassium hexafluoromanganate and antimony pentafluoride heat production fluorine altogether
The system of the pure graphite of air lift utilizes the potassium hexafluoromanganate in reactor by the way that chemical reactor is arranged in the side of graphitizing furnace
Graphite in stove is purified with antimony pentafluoride total heat production fluorine gas, avoids and is asked what environment damaged using freon
Topic.
The technology solution of the present invention is as follows：
Potassium hexafluoromanganate and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, including fluorine gas reaction member I, the fluorine
Solid/liquid/gas reactions unit I includes：
The external installation of reactor and vacuum pump for being vacuumized to inside reactor, the reactor is useful
In the heater heated to reactor, and
Furnace body unit II, the furnace body unit II include：
The bottom of furnace body, the furnace body is disposed with furnace burdening, and graphite products are positioned 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 reactor reaction generates fluorine gas, and fluorine gas is passed through the bottom removal graphite of furnace core
Impurity element in product.
As an improvement, antimony pentafluoride is added in the reactor, the inner upper end of the reactor is additionally provided with feeder,
Potassium hexafluoromanganate is placed in the feeder, feeder control potassium hexafluoromanganate is added in reactor, and the reactor passes through
Air inlet pipe c is connected to furnace core.
As an improvement, being additionally provided with agitating device in the reactor, the agitating device is used for six in reactor
Fluorine potassium manganate and antimony pentafluoride mixture are stirred, the agitating device include be arranged the rotating member covered in reactor top,
Force piece drives the lower shaft a rotated and several agitating paddles in the ends shaft a is arranged.
As an improvement, being additionally provided at the outlet end of the feeder for controlling potassium hexafluoromanganate discharging in feeder
Control device, the control device include being fixed on the rotation seat of feeder side and being rotatably provided on rotation seat to turn
Axis b, the lower end of the shaft b are fixedly installed feeding plate, are done if being offered on described its circumferencial direction of feeding plate upper edge
Expect hole, belt is connected between the shaft b and shaft a, the shaft a rotations drive shaft b and feeding plate to turn by belt
It is dynamic to keep the discharge port of discharge hole and feeder intermittently connected.
As an improvement, the side of the furnace body is additionally provided with tail gas absorber, the tail gas absorber by escape pipe with
It is connected at the top of the furnace core of furnace body, the air pump for gas in furnace core to be pumped to tail gas absorber is provided on escape pipe；
The pressure gauge for monitoring furnace core internal pressure is additionally provided at the top of the furnace body.
As an improvement, the reactor head is provided with thermocouple, the thermocouple is used to monitor the heating temperature of heater
Degree.
As another improvement, the heater is set as resistance heater, and the resistance heater is by nickel chromium triangle or graphite material
Material is made, and the reactor is made of quartz or graphite material.
It should be noted that in mass ratio 2~3:1 ratio carries out feeding simultaneously to antimony pentafluoride and potassium hexafluoromanganate
It is added in reactor and is reacted, reaction temperature is at 490~500 DEG C, chemical equation 2K2MnF6+4SbF5→4KSbF6+
2MnF3+F2↑；
The spacing of multigroup graphite product as requested is arranged in graphitizing furnace, insulation material and resistance material are successively filled,
After shove charge, heating graphitizing furnace to furnace core temperature is passed through the air in nitrogen exclusion furnace core when being 1800~1900 DEG C, rise
Warm 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 lead to
Enter chlorine；Continue to heat graphitizing furnace when being warming up to 2300~2500 DEG C, the fluorine gas that generation is reacted in step b is passed through graphitization
In stove, fluorine gas forms fluoride with the impurity chemical combination in graphite product, reduces its boiling point, and by taking boron as an example, boiling point is more than 3500
DEG C, it is reacted with fluorine gas, 2B+3F2→2BF3, -127.1 DEG C of the boron fluoride boiling point of generation.
It is passed through molecular weight and boiling point parameter that chlorine and fluorine gas carry out pure treated the nuclear graphite materials metal chloride of core
It see the table below 1.
Table 1：The molecular weight and boiling point of typical metal chloride
Bibliography：
CRC Handbook of Chemistry and Physics, 75th ed., 1994
PlenumPress Handbook
Table 2：The molecular weight and boiling point of typical metal fluoride
Bibliography：
Merck Index, 11thEdition, 1989
CRC Handbook of Chemistry and Physics, 75th ed., 1994
By Tables 1 and 2 it is found that the present invention is under graphitization processing high temperature, it is passed through after chlorine and fluorine gas in nuclear graphite materials
Metal chloride and metal fluoride boiling point far below the high boron element in graphitization temperature, especially neutron absorption cross-section and
The fluoride boiling point of class boron element substantially reduces, and then can targetedly control the boron equivalent in nuclear graphite materials.
The beneficial effects of the present invention are：
1. it is chemically reacted in the present invention by being added in graphite purification technique, it is total using potassium hexafluoromanganate and antimony pentafluoride
Heat produces fluorine gas to replace the freon used in purification process in prior art, and fluorine is avoided while ensureing that purification effect is good
The problem of during the use of Leon to the adverse effect of environment.
2. being additionally provided with feeder in the inner upper end of reactor in the present invention, and potassium hexafluoromanganate is placed on charging
Device so that the problem of chemical reaction condition needs antimony pentafluoride to be in excessive state can be met, in addition by going out in feeder
Mouthful end setting control device and control device is set and agitating device linkage allows to stirring by adjusting agitating device
The feed rate of rate control potassium hexafluoromanganate, and then the rate for generating fluorine gas is controlled, when needing generation fluorine gas fast, accelerate to stir
It mixes, charging rate is also accelerated, and reacts in the case of expecting sufficient stirring again soon and also accelerates.
In conclusion the present invention optimizes with device structure, purified treatment effect is good, and environmental-protecting performance is high, at low cost etc. excellent
Point is particularly suitable for isostatic pressing formed graphite purification process technical field.
Description of the drawings：
Following further describes the present invention with reference to the drawings：
Fig. 1 is that heat produces the apparatus structure schematic diagram that fluorine gas purifies graphite altogether for potassium hexafluoromanganate and antimony pentafluoride；
Fig. 2 is inside reactor structural schematic diagram；
Fig. 3 is the structural scheme of mechanism of agitating device and control device.
Specific implementation mode：
As described below is only presently preferred embodiments of the present invention, is not defined to the scope of the present invention.
Embodiment one
As shown in Figure 1, Figure 2 and Figure 3, potassium hexafluoromanganate and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, including
Fluorine gas reaction member I, the fluorine gas reaction member I include：
Reactor 1 and for the vacuum pump 2 to being vacuumized inside reactor 1, the external installation of the reactor 1
It is useful for the heater 3 heated to reactor 1, and
Furnace body unit II, the furnace body unit II include：
The bottom of furnace body 3, the furnace body 3 is disposed with furnace burdening 31, and graphite products are positioned at furnace core 32, graphite products
Surrounding is disposed with resistance material 33, and the outside of resistance material 33 is disposed with insulation material 34, and the side of the furnace body 3 is provided with for distinguishing
Nitrogen and chlorine are passed through to the air inlet pipe a4 and air inlet pipe b5 of furnace core 32, the reaction of the reactor 1 generates fluorine gas, and fluorine gas is passed through stove
Impurity element in the bottom removal graphite products of core 32.
By the way that chemical reaction is added in graphite purification technique, using potassium hexafluoromanganate and antimony pentafluoride altogether heat production fluorine gas come
Instead of the freon used in purification process in prior art, while ensureing that purification effect is good avoiding freon used
The problem of in journey to the adverse effect of environment.
Further, antimony pentafluoride is added in the reactor 1, the inner upper end of the reactor 1 is additionally provided with charging
Device 6, the feeder 6 is interior to place potassium hexafluoromanganate, and feeder 6 controls potassium hexafluoromanganate and is added in reactor 1, the reaction
Device 1 is connected to by air inlet pipe c7 with furnace core 32.
Further, agitating device 8 is additionally provided in the reactor 1, the agitating device 8 is used for in reactor 1
Potassium hexafluoromanganate and antimony pentafluoride mixture be stirred, which includes the rotation that is arranged on 1 head cover of reactor
Under the drive of force piece 81 the shaft a82 that rotates and several agitating paddles 83 in the ends shaft a82 are arranged in part 81.
Further, it is additionally provided at the outlet end of the feeder 6 and discharges for controlling potassium hexafluoromanganate in feeder 6
Control device 9, the control device 9 include be fixed on 6 side of feeder rotation seat 91 and be rotatably provided in rotation
The lower end of shaft b92, the shaft b92 on seat 91 are fixedly installed feeding plate 93, its circumference of 93 upper edge of the feeding plate
Several discharge holes 94 are offered on direction, and belt 10, the shaft a82 rotations are connected between the shaft b92 and shaft a82
Shaft b92 and the rotation of feeding plate 93 is driven to keep discharge hole 94 and the discharge port of feeder 6 intermittently connected by belt 10.
It should be noted that by being additionally provided with feeder 6 in the inner upper end of reactor 1 in the present embodiment, and by six
Fluorine potassium manganate is placed on feeder 6 so that the problem of chemical reaction condition needs antimony pentafluoride to be in excessive state can be met,
In addition by 6 outlet end of feeder be arranged control device 9 and be arranged control device 9 and agitating device 8 linkage allow to
Stir speed (S.S.) by adjusting agitating device 8 controls the feed rate of potassium hexafluoromanganate, and then controls the rate for generating fluorine gas, needs
Generate fluorine gas it is fast when, accelerate stirring, charging rate also accelerates, and expects to react in the case that sufficient stirring is again fast and also accelerate.
Further, 1 top of the reactor is provided with thermocouple 15, and the thermocouple 15 is for monitoring heater 3
Heating temperature.
Further, the heater 3 is set as resistance heater, and the resistance heater 3 is by nickel chromium triangle or graphite material
Material is made, and the reactor 1 is made of quartz or graphite material.
It should be noted that in mass ratio 2~3:1 ratio carries out feeding simultaneously to antimony pentafluoride and potassium hexafluoromanganate
It is added in reactor and is reacted, reaction temperature is at 490~500 DEG C, chemical equation 2K2MnF6+4SbF5→4KSbF6+
2MnF3+F2↑；
The spacing of multigroup graphite product as requested is arranged in graphitizing furnace, insulation material and resistance material are successively filled,
After shove charge, heating graphitizing furnace to furnace core temperature is passed through the air in nitrogen exclusion furnace core when being 1800~1900 DEG C, rise
Warm 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 lead to
Enter chlorine；Continue to heat graphitizing furnace when being warming up to 2300~2500 DEG C, the fluorine gas that generation is reacted in step b is passed through graphitization
In stove, fluorine gas forms fluoride with the impurity chemical combination in graphite product, reduces its boiling point, and by taking boron as an example, boiling point is more than 3500
DEG C, it is reacted with fluorine gas, 2B+3F2→2BF3, -127.1 DEG C of the boron fluoride boiling point of generation.
Embodiment two
As shown in Fig. 2, as an improvement, the side of the furnace body 3 is additionally provided with tail gas absorber 11, the tail gas absorber
11 are connected to by escape pipe 12 with 32 top of furnace core of furnace body 3, are provided on escape pipe 12 for pumping gas in furnace core 32
To the air pump 13 of tail gas absorber 11；
The top of the furnace body 3 is additionally provided with the pressure gauge 14 for monitoring 32 internal pressure of furnace core.
It should be noted that tail gas absorber 11 is made of several sodium hydroxide solution absorbers, fluorine gas and hydroxide
Sodium reaction removal, equation 2F2+4NaOH→NaF+2H2O+O2, in the molten people's aqueous solution of sodium fluoride of gasification, in the present embodiment
It is directly discharged to pollute environment in the air by the way that the exhaust gas that tail gas absorber avoids graphitization, purifying generates is arranged.
Above in association with described in attached drawing being only the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, it is noted that for those skilled in the art, without departing from the structure of the invention, can also make various
Modification and improvement, these should also be considered as protection scope of the present invention, all not interfere with effect and practicability that the present invention is implemented.
Claims (7)
1. potassium hexafluoromanganate and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, it is characterised in that：React single including fluorine gas
Member I, the fluorine gas reaction member I include：
Reactor (1) and the vacuum pump (2) for being used to vacuumize reactor (1) inside, the outside of the reactor (1)
Heater (16) for being heated to reactor (1) is installed, and
Furnace body unit II, the furnace body unit II include：
The bottom of furnace body (3), the furnace body (3) is disposed with furnace burdening (31), and graphite products are positioned at furnace core (32), graphite production
The surrounding of product is disposed with resistance material (33), and insulation material (34) is disposed on the outside of resistance material (33), and the side of the furnace body (3) is set
It is equipped with the air inlet pipe a (4) and air inlet pipe b (5) for nitrogen and chlorine to be passed through to furnace core (32) respectively, the reactor (1) is anti-
Fluorine gas should be generated, fluorine gas is passed through the impurity element in the bottom removal graphite products of furnace core (32).
2. potassium hexafluoromanganate as described in claim 1 and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, feature exist
In：Antimony pentafluoride is added in the reactor (1), the inner upper end of the reactor (1) is additionally provided with feeder (6), described
Potassium hexafluoromanganate is placed in feeder (6), feeder (6) control potassium hexafluoromanganate is added in reactor (1), the reactor
(1) it is connected to furnace core (32) by air inlet pipe c (7).
3. potassium hexafluoromanganate as described in claim 1 and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, feature exist
In：Agitating device (8) is additionally provided in the reactor (1), the agitating device (8) is used for the hexafluoro in reactor (1)
Potassium manganate and antimony pentafluoride mixture are stirred, which includes the rotating member being arranged on reactor (1) head cover
(81), it drives the lower shaft a (82) rotated in force piece (81) and several agitating paddles in shaft a (82) end is set
(83)。
4. potassium hexafluoromanganate as claimed in claim 3 and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, feature exist
In：The control device for controlling the interior potassium hexafluoromanganate discharging of feeder (6) is additionally provided at the outlet end of the feeder (6)
(9), the control device (9) includes being fixed on the rotation seat (91) of feeder (6) side and being rotatably provided in rotation seat
(91) the shaft b (92) on, the lower end of the shaft b (92) are fixedly installed feeding plate (93), on the feeding plate (93)
Several discharge holes (94) are offered along its circumferencial direction, and belt is connected between the shaft b (92) and shaft a (82)
(10), the shaft a (82) rotation by belt (10) drive shaft b (92) and feeding plate (93) rotation make discharge hole (94) and
The discharge port of feeder (6) is intermittently connected.
5. potassium hexafluoromanganate as described in claim 1 and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, feature exist
In：The side of the furnace body (3) is additionally provided with tail gas absorber (11), the tail gas absorber (11) by escape pipe (12) with
It is connected at the top of the furnace core (32) of furnace body (3), is provided on escape pipe (12) and is inhaled for furnace core (32) interior gas to be pumped to tail gas
Receive the air pump (13) of device (11)；
The pressure gauge (14) for monitoring furnace core (32) internal pressure is additionally provided at the top of the furnace body (3).
6. potassium hexafluoromanganate as described in claim 1 and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, feature exist
In：Thermocouple (15) is provided at the top of the reactor (1), the thermocouple (15) is used to monitor the heating temperature of heater (16)
Degree.
7. potassium hexafluoromanganate as described in claim 1 and the antimony pentafluoride system that heat production fluorine gas purifies graphite altogether, feature exist
In：The heater (16) is set as resistance heater, and the heater (16) is made of nickel chromium triangle or graphite material, the reaction
Device (1) is made of quartz or graphite material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810555995.6A CN108483441B (en) | 2018-06-01 | 2018-06-01 | System for potassium hexafluoromanganate and antimony pentafluoride generate fluorine gas purification graphite by concurrent heating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810555995.6A CN108483441B (en) | 2018-06-01 | 2018-06-01 | System for potassium hexafluoromanganate and antimony pentafluoride generate fluorine gas purification graphite by concurrent heating |
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| Publication Number | Publication Date |
|---|---|
| CN108483441A true CN108483441A (en) | 2018-09-04 |
| CN108483441B CN108483441B (en) | 2020-04-07 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101927981A (en) * | 2010-08-17 | 2010-12-29 | 北京矿冶研究总院 | Preparation method of graphite fluoride |
| CN102126721A (en) * | 2011-04-27 | 2011-07-20 | 深圳市贝特瑞新能源材料股份有限公司 | Purification and graphitization method of graphite material |
| CN107879340A (en) * | 2017-12-11 | 2018-04-06 | 湖南顶立科技有限公司 | A kind of graphite purification system |
| CN208829273U (en) * | 2018-06-01 | 2019-05-07 | 中钢集团新型材料（浙江）有限公司 | The system that potassium hexafluoromanganate and antimony pentafluoride heat together produce fluorine gas purification graphite |
-
2018
- 2018-06-01 CN CN201810555995.6A patent/CN108483441B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101927981A (en) * | 2010-08-17 | 2010-12-29 | 北京矿冶研究总院 | Preparation method of graphite fluoride |
| CN102126721A (en) * | 2011-04-27 | 2011-07-20 | 深圳市贝特瑞新能源材料股份有限公司 | Purification and graphitization method of graphite material |
| CN107879340A (en) * | 2017-12-11 | 2018-04-06 | 湖南顶立科技有限公司 | A kind of graphite purification system |
| CN208829273U (en) * | 2018-06-01 | 2019-05-07 | 中钢集团新型材料（浙江）有限公司 | The system that potassium hexafluoromanganate and antimony pentafluoride heat together produce fluorine gas purification graphite |
Non-Patent Citations (1)
| Title |
|---|
| CHRISTE, KARL O.: "Chemical synthesis of elemental fluorine", 《INORGANIC CHEMICAL》 * |
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