CN107539982A - A kind of high-purity micro crystal graphite production system and its production technology - Google Patents
A kind of high-purity micro crystal graphite production system and its production technology Download PDFInfo
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- CN107539982A CN107539982A CN201711046993.6A CN201711046993A CN107539982A CN 107539982 A CN107539982 A CN 107539982A CN 201711046993 A CN201711046993 A CN 201711046993A CN 107539982 A CN107539982 A CN 107539982A
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Abstract
The present invention relates to micro crystal graphite purification technique field, disclose a kind of high-purity micro crystal graphite production system and its production technology, Feedstock treating workshop, the first Pickling-shop, ultrasonic response kettle and the second Pickling-shop that high-purity micro crystal graphite production system includes being sequentially connected according to micro crystal graphite purifying technique, the Feedstock treating workshop includes disintegrating machine, ball mill, flotation device and the centrifuge being sequentially connected, first Pickling-shop is identical with the second Pickling-shop, includes reactor, cleaning machine, centrifuge and the dryer being sequentially connected.High-purity micro crystal graphite of fixed carbon content energy more than 99.9% can be prepared in the high-purity micro crystal graphite production system of the present invention, and significantly reduces the usage amount of hydrofluoric acid, have the advantages of efficiency high, energy consumption are low, and refining effect is good.
Description
Technical field
The present invention relates to micro crystal graphite purification technique field, more particularly, to a kind of high-purity micro crystal graphite production system
And its production technology.
Background technology
Graphite is a kind of high energy crystal carbon material, because of its unique structure and conduction, heat conduction, lubrication, high temperature resistant, chemically
Can be stable the features such as, be widely used in metallurgy, machinery, environmental protection, chemical industry, fire resisting, new energy, nuclear energy, electronics, medicine, military project and
The fields such as Aero-Space.
Native graphite shaping geological conditions in China is good, widely distributed, aboundresources, quality are good, and reserves and yield all occupy generation
Boundary is the first, is one of the Dominant Mineral Resources in China.Native graphite can be divided into Scaly graphite and microcrystalline according to the difference of crystallization degree
The class of graphite two, wherein Chenzhou aphanitic graphite account for 74.7% or so of national gross reserves, and the aphanitic graphite quality is preferable,
Fixed carbon content is high.
But for a long time, people mostly pay attention to the exploitation and processing of Scaly graphite, ignore and occupy a greater part of reserves
The utilization of microcrystalline graphite, the problem of its deep process technology is horizontal and deep processing ability is relatively low, are not solved effectively for a long time
Certainly.At present mainly based on raw ore and rough-wrought product application, resource is not fully utilized, or even blindly exports, and causes ore deposit
Produce a large amount of losses and waste of resource.Therefore, the chemical purification research work of microcrystalline graphite, developing low-cost high-carbon stone are carried out
Black production technology, has important practical significance.
The purification of microcrystalline graphite at present mostly be use for reference Scaly graphite technology, common method of purification include floatation,
High temperature method, alkali acid system, hydrogen fluoride, chlorinating roasting etc., floatation are used for the preliminary purification of Scaly graphite, graphite products product
Position is not high, and the rate of recovery is very low, the method for the non-chemical purification graphite of alkali acid system, hydrogen fluoride, chlorinating roasting, wherein, alkali
Acid system purifies the shortcomings that graphite and is to need high-temperature calcination, and energy expenditure is big, and the reaction time length purified, and the method pair sets
Standby corrosion is more serious, and the graphite purity obtained by the method does not reach 99.9%, although high temperature method refining effect
Preferably, but its cost is too high, capital invested needed for industrialization is huge, and hydrogen fluoride purification graphite efficiency high, energy consumption are low, but hydrogen
The dosage of fluoric acid is huge and has severe toxicity and severe corrosive, causes production equipment and environmentally friendly cost higher, therefore, it is necessary to design one
Money new micro crystal graphite production system makes up drawbacks described above.
The content of the invention
The technical problems to be solved of the present invention are, fixed carbon content limited for prior art chemical purification effect
More than 99.9% is unable to reach, and high temperature method cost is too high, further to improve graphite purity and reducing the dosage of hydrofluoric acid,
A kind of high-purity micro crystal graphite production system is provided.
The present invention also provides a kind of production technology of high-purity micro crystal graphite production system.
The purpose of the present invention is achieved by the following technical programs：
A kind of high-purity micro crystal graphite production system is provided, included according to micro crystal graphite purifying technique at the raw material that is sequentially connected
Workshop, the first Pickling-shop, ultrasonic response kettle and the second Pickling-shop are managed, the Feedstock treating workshop includes what is be sequentially connected
Disintegrating machine, ball mill, flotation device and centrifuge, first Pickling-shop is identical with the second Pickling-shop structure, include according to
Reactor, cleaning machine, centrifuge and the dryer of secondary connection.
Preferably, the disintegrating machine is jaw crusher.
Preferably, the disintegrating machine, ball mill, flotation device, centrifuge, the first Pickling-shop, ultrasonic response kettle, second
By transmitting band connection between Pickling-shop.
Preferably, second Pickling-shop is also associated with packing processes machine.
Preferably, by transmitting band connection between second Pickling-shop and packing processes machine.
The present invention also provides the production technology of high-purity micro crystal graphite production system, comprises the following steps：
S1. raw ore is handled：Shandong pool micro crystal graphite raw ore is crushed in disintegrating machine, is then fed into ball mill and carries out depth
Ore grinding, it is -0.074mm level materials to obtain fineness by ore grinding, is that -0.074mm level material contents account for 90% to mog
Primary sample carries out flotation in flotation device, after four selected once purging selection flows of one roughing, is carried out in centrifuge
Magnetic separation, it is 90% micro crystal graphite to be fixed carbon content；
The raw ore material performance of Shandong pool micro crystal graphite described in step S1 is as follows：Moisture 2.4%, volatile matter 2.99%, ash content
18.37% carbon content 78.64%；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 is sent into the first Pickling-shop, reacted first with mixed acid
Mixed in kettle, mixed acid is HF and H2SO4Mixed acid, wherein HF concentration is 7%, H2SO4Concentration be 30%, mixed acid
It is 3.5 with graphite liquid-solid ratio:1, normal pressure acidleach is carried out after stirring under conditions of 80 DEG C of temperature, reaction time 3h, is leached
It is neutrality that slag, which is washed in cleaning machine to pH value, is filtered afterwards in centrifuge, temperature is to be done at 80~150 DEG C in dryer
Dry 2~3h, it is fixed the micro crystal graphite that carbon content is 98.82%；
S22. it is ultrasonically treated：The obtained micro crystal graphites of step S21 and mixed acid are mixed in ultrasonic response kettle, mixed
Acid is HF and H2SO4Mixed acid, wherein HF concentration is 3%, H2SO4Concentration be 20%, mixed acid is with graphite liquid-solid ratio
3:1, stir and be ultrasonically treated, time 15min, obtain micro crystal graphite mixed acid solution；
S23. secondary pickling：Micro crystal graphite mixed acid solution obtained by step S22 is sent into the second Pickling-shop, first will be micro-
Spar ink mixed acid solution, which is put into reactor, to react, and reaction temperature is 90 DEG C, reaction time 3h, then passes sequentially through cleaning machine
Cleaned, centrifuge is filtered, dryer carries out drying drying, be fixed carbon content be 99.98% high-purity crystallite
Graphite.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention uses Shandong pool aphanitic graphite as raw material, and raw ore is tentatively located by Feedstock treating workshop first
Reason, is then purified using the two step acid-hatchings of young eggs to micro crystal graphite, and fixed carbon content can reach more than 99.9% high-purity crystallite
Graphite, the high-purity micro crystal graphite production system of the present invention significantly reduce the usage amount of hydrofluoric acid, have efficiency high, energy consumption low, carry
The advantages of pure effect is good.
The present invention is crushed and ground to crystallite stone mill raw ore in Feedstock treating workshop, coordinates the one roughing four of flotation
Secondary selected once purging selection flow, at utmost improving the purity of raw ore by physical method, (fixed carbon content is 90% microlite
If ink will also make its grade be further enhanced, floatation is all than relatively difficult to achieve in technology or economically)
Micro crystal graphite particle diameter is reduced simultaneously, increases the specific surface area of micro crystal graphite, is advantageous to reduce subsequent purification in follow-up acidleach purification
Energy consumption and cost.
The present invention adds ultrasonic response kettle on the basis of traditional Pickling-shop, carries out secondary pickling purification processes, its
Middle first time is significantly reduced using the impurity volume in graphite after acid-hatching of young eggs purification, and metamorphosis is larger, but still with granulated
Formula is present, and reason is that impurity particle ecto-entad gradually dissolves as reaction is carried out, and reaction difficulty gradually increases, and this
A little precipitations are covered in undissolved impurity particle surface, hinder the further progress of reaction, now continue the concentration of increase acid
Effect and unobvious, in addition, these precipitations are difficult in itself to be removed in the washing and filtering stage, the present invention adds ultrasonic response
Kettle so that the micro crystal graphite after acidleach purification is additionally separated with impurity, the mechanical crushing effect in ultrasonic procedure
Micro crystal graphite particle can be crushed with cavitation, make to be wrapped in the partial impurities in aggregate and participate in reaction, accelerate miscellaneous
Matter and the reaction rate of acid, therefore, second of acidleach purification only need minimal amount of acid to can obtain high-purity micro crystal graphite, significantly
Reduce purification energy consumption and cost.
Brief description of the drawings
The high-purity micro crystal graphite production system equipment block diagrams of Fig. 1.
The high-purity micro crystal graphite production system process charts of Fig. 2.
Fig. 3 the first Pickling-shop structural representations.
Fig. 4 flotation flowsheet figures.
Embodiment
With reference to embodiment, the present invention is further illustrated.Wherein, being given for example only property of accompanying drawing illustrates,
What is represented is only schematic diagram, rather than pictorial diagram, it is impossible to is interpreted as the limitation to this patent；In order to which the reality of the present invention is better described
Example is applied, some parts of accompanying drawing have omission, zoomed in or out, and do not represent the size of actual product；To those skilled in the art
For, some known features and its explanation may be omitted and will be understood by accompanying drawing.
Embodiment 1
As shown in figure 1, the present embodiment provides a kind of high-purity micro crystal graphite production system, including it is suitable according to micro crystal graphite purification
Feedstock treating workshop, the first Pickling-shop 5, ultrasonic response kettle 6, the second Pickling-shop 7 and the packing processes that sequence is sequentially connected
Machine 8, wherein Feedstock treating workshop include disintegrating machine 1, ball mill 2, flotation device 3 and the centrifuge 4 being sequentially connected.
As shown in Fig. 2 micro crystal graphite raw ore is crushed by disintegrating machine in the present embodiment, the micro crystal graphite after crushing is former
Ore deposit is admitted to ball mill 2 and carries out ball milling operation, and after ball milling operation, micro crystal graphite is admitted to flotation device 3 and carries out flotation, after flotation
Micro crystal graphite can be admitted to centrifuge 4 and carry out centrifugal treating, the process of centrifugal treating is magnetic separation process in the present embodiment, magnetic
After choosing, microcrystalline graphite material, which can be admitted in the first Pickling-shop 5, carries out first of acidleach purification processes, after the completion of be re-fed into
It is ultrasonically treated in ultrasonic response kettle 6, completes to be ultrasonically treated, is fed again into the second Pickling-shop 7 and carries out second acidleach
Purification processes, finally give high-purity micro crystal graphite and complete packaging and storage in packing processes machine 8.
The present embodiment production capacity balanced arrangement is as shown in table 1.
Table 1
As known from Table 1, the present embodiment is cooperated using existing equipment, it is possible to achieve high production capacity, low cost, and into
Product rate is high, and after especially first of pickling is by supersound process, the yield rate of second pickling has reached 99.7%.
Disintegrating machine 1, ball mill 2, flotation device 3, centrifuge 4, the first Pickling-shop 5, ultrasonic response kettle in the present embodiment
6th, by transmitting band connection between the second Pickling-shop 7, packing processes machine 8.Wherein, disintegrating machine 1 uses jaw crusher, and first
The Pickling-shop 7 of Pickling-shop 5 and second is identical, as shown in figure 3, the reactor 51, clear that the first Pickling-shop 5 includes being sequentially connected
Washing machine 52, centrifuge 53 and dryer 55, microcrystalline graphite material complete acid reaction in reactor 51, afterwards in cleaning machine 52
With pure water to neutrality, filtered by centrifuge 53, then carry out drying and processing in dryer 55, complete drying.
The present embodiment can be placed above-mentioned all parts in multiple workshops or computer room according to actual conditions, for saving reality
Border floor space, and some parts are unsuitable for putting together, but when carrying out high-purity micro crystal graphite processing, it is still desirable to
The micro crystal graphite that one equipment is treated is sent into a leave from office equipment, and therefore, each equipment of the present embodiment is according to purifying technique
It is sequentially connected to be considered as.
The present embodiment also provides the production technology of high-purity micro crystal graphite production system, comprises the following steps：
S1. raw ore is handled：Shandong pool micro crystal graphite raw ore is crushed in disintegrating machine 1, is then fed into ball mill 2 and carries out deeply
Ore grinding is spent, it is -0.074mm level materials to obtain fineness by ore grinding, is that -0.074mm level material contents account for 90% to mog
Primary sample flotation device 3 carry out flotation, flotation flowsheet is as shown in figure 4, using four selected once purging selection flows of one roughing
Afterwards, magnetic separation is carried out in centrifuge 4, it is 90% micro crystal graphite to be fixed carbon content；
The raw ore material performance of Shandong pool micro crystal graphite described in step S1 is as follows：Moisture 2.4%, volatile matter 2.99%, ash content
18.37% carbon content 78.64%；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 is sent into the first Pickling-shop 5, reacted first with mixed acid
Mixed in kettle 51, mixed acid is HF and H2SO4Mixed acid, wherein HF concentration is 7%, H2SO4Concentration be 30%, mixing
Acid is 3.5 with graphite liquid-solid ratio:1, normal pressure acidleach, leaching are carried out after stirring under conditions of 80 DEG C of temperature, reaction time 3h
Washing to the pH value in cleaning machine 52 of slagging tap is neutrality, afterwards filtering, dry in dryer 54, specific temperature in centrifuge 53
Spend the micro crystal graphite for dry 2~3h at 80~150 DEG C, being fixed that carbon content is 98.82%；
S22. it is ultrasonically treated：The obtained micro crystal graphites of step S21 and mixed acid are mixed in ultrasonic response kettle 6, mixed
It is HF and H to close acid2SO4Mixed acid, wherein HF concentration is 3%, H2SO4Concentration be 20%, mixed acid and graphite liquid-solid ratio
For 3:1, stir and be ultrasonically treated, time 15min, obtain micro crystal graphite mixed acid solution；
S23. secondary pickling：Micro crystal graphite mixed acid solution obtained by step S22 is sent into the second Pickling-shop 7, first will
Micro crystal graphite mixed acid solution, which is put into reactor, to react, and reaction temperature is 90 DEG C, reaction time 3h, then passes sequentially through cleaning
Machine is cleaned, centrifuge is filtered, dryer carries out drying drying, be fixed carbon content be 99.98% it is high-purity micro-
Spar ink, final packaging storage.
The present embodiment uses Shandong pool aphanitic graphite as raw material, and raw ore is tentatively located by Feedstock treating workshop first
Reason, is then purified using the two step acid-hatchings of young eggs to micro crystal graphite, and fixed carbon content can reach more than 99.9% high-purity crystallite
Graphite, the usage amount of hydrofluoric acid is significantly reduced, there is the advantages of efficiency high, energy consumption are low, and refining effect is good.
The present embodiment is crushed and ground to crystallite stone mill raw ore in Feedstock treating workshop, coordinates the one roughing of flotation
Four selected once purging selection flows, at utmost improving the purity of raw ore by physical method, (fixed carbon content is 90% crystallite
If graphite will also make its grade be further enhanced, floatation is all than relatively difficult to achieve in technology or economically
) while reduce micro crystal graphite particle diameter, increase the specific surface area of micro crystal graphite, be advantageous to reduce subsequently carrying in follow-up acidleach purification
Pure energy consumption and cost.
The present embodiment adds ultrasonic response kettle on the basis of traditional Pickling-shop, carries out secondary pickling purification processes,
Wherein being significantly reduced for the first time using the impurity volume in graphite after acid-hatching of young eggs purification, metamorphosis is larger, but still with particle
Form is present, and reason is that impurity particle ecto-entad gradually dissolves as reaction is carried out, and reaction difficulty gradually increases, and
These precipitations are covered in undissolved impurity particle surface, hinder the further progress of reaction, now continue the dense of increase acid
Effect and unobvious are spent, in addition, these precipitations are difficult in itself to be removed in the washing and filtering stage, it is anti-that the present embodiment adds ultrasonic wave
Answer kettle so that the micro crystal graphite after acidleach purification is additionally separated with impurity, and the mechanical crushing in ultrasonic procedure is made
Micro crystal graphite particle can be crushed with cavitation, make to be wrapped in the partial impurities in aggregate and participate in reaction, accelerate
The reaction rate of impurity and acid, therefore, second of acidleach purification only need minimal amount of acid to can obtain high-purity micro crystal graphite, show
Work reduces purification energy consumption and cost.
Obviously, above-described embodiment is only intended to clearly illustrate technical scheme example, and is not
Restriction to embodiments of the present invention.For those of ordinary skill in the field, on the basis of the above description also
It can make other changes in different forms.Any modification for being made within the spirit and principles of the invention, etc.
With replacement and improvement etc., should be included within the protection of the claims in the present invention.
Claims (6)
1. a kind of high-purity micro crystal graphite production system, it is characterised in that include what is be sequentially connected according to micro crystal graphite purifying technique
Feedstock treating workshop, the first Pickling-shop, ultrasonic response kettle and the second Pickling-shop, the Feedstock treating workshop are included successively
Disintegrating machine, ball mill, flotation device and the centrifuge of connection, first Pickling-shop is identical with the second Pickling-shop structure,
Including reactor, cleaning machine, centrifuge and the dryer being sequentially connected.
2. high-purity micro crystal graphite production system according to claim 1, it is characterised in that the disintegrating machine is jaw crushing
Machine.
3. high-purity micro crystal graphite production system according to claim 1, it is characterised in that the disintegrating machine, ball mill, flotation
By transmitting band connection between machine, centrifuge, the first Pickling-shop, ultrasonic response kettle, the second Pickling-shop.
4. high-purity micro crystal graphite production system according to claim 1, it is characterised in that second Pickling-shop is also connected with
There is packing processes machine.
5. high-purity micro crystal graphite production system according to claim 4, it is characterised in that second Pickling-shop and packaging
By transmitting band connection between processor.
6. the production technology of high-purity micro crystal graphite production system according to Claims 1 to 5 any one, it is characterised in that
Comprise the following steps：
S1. raw ore is handled：Shandong pool micro crystal graphite raw ore is crushed in disintegrating machine, is then fed into progress depth mill in ball mill
Ore deposit, it is -0.074mm level materials to obtain fineness by ore grinding, is the raw ore that -0.074mm level material contents account for 90% to mog
Sample carries out flotation in flotation device, and after four selected once purging selection flows of one roughing, magnetic separation is carried out in centrifuge,
It is 90% micro crystal graphite to be fixed carbon content；
The raw ore material performance of Shandong pool micro crystal graphite described in step S1 is as follows：Moisture 2.4%, volatile matter 2.99%, ash content 18.37%
Carbon content 78.64%；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 is sent into the first Pickling-shop, first with mixed acid in a kettle
Mixing, mixed acid is HF and H2SO4Mixed acid, wherein HF concentration is 7%, H2SO4Concentration be 30%, mixed acid and graphite
Liquid-solid ratio is 3.5:1, normal pressure acidleach is carried out after stirring under conditions of 80 DEG C of temperature, reaction time 3h, leached mud is clear
In washing machine washing to pH value for neutrality, afterwards in centrifuge filtering, in dryer temperature be 80 ~ 150 DEG C at dry 2 ~ 3h,
It is fixed the micro crystal graphite that carbon content is 98.82%；
S22. it is ultrasonically treated：The obtained micro crystal graphites of step S21 and mixed acid are mixed in ultrasonic response kettle, mixed acid is
HF and H2SO4Mixed acid, wherein HF concentration is 3%, H2SO4Concentration be 20%, mixed acid and graphite liquid-solid ratio are 3:1, stir
Mix and be uniformly ultrasonically treated, time 15min, obtain micro crystal graphite mixed acid solution；
S23. secondary pickling：Micro crystal graphite mixed acid solution obtained by step S22 is sent into the second Pickling-shop, first by microlite
Black mixed acid solution, which is put into reactor, to react, and reaction temperature is 90 DEG C, reaction time 3h, then passes sequentially through cleaning machine progress
Cleaning, centrifuge is filtered, dryer carries out drying drying, is fixed high-purity micro crystal graphite that carbon content is 99.98%.
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| CN110171825A (en) * | 2019-07-10 | 2019-08-27 | 青岛洛唯新材料有限公司 | A kind of high purity graphite purifying technique |
| CN113716559A (en) * | 2021-09-03 | 2021-11-30 | 黑龙江省宝泉岭农垦溢祥石墨有限公司 | Strong acid method scale graphite purification process and device |
| CN114538430A (en) * | 2020-11-26 | 2022-05-27 | 鸡西市贝特瑞石墨产业园有限公司 | Method for purifying graphite, lithium ion battery cathode, lithium ion battery and electric equipment |
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| CN114538430A (en) * | 2020-11-26 | 2022-05-27 | 鸡西市贝特瑞石墨产业园有限公司 | Method for purifying graphite, lithium ion battery cathode, lithium ion battery and electric equipment |
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