CN207418305U - A kind of high-purity micro crystal graphite production system - Google Patents
A kind of high-purity micro crystal graphite production system Download PDFInfo
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- CN207418305U CN207418305U CN201721425348.0U CN201721425348U CN207418305U CN 207418305 U CN207418305 U CN 207418305U CN 201721425348 U CN201721425348 U CN 201721425348U CN 207418305 U CN207418305 U CN 207418305U
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Abstract
The utility model is related to micro crystal graphite purification technique fields, disclose a kind of high-purity micro crystal graphite production system, high-purity micro crystal graphite production system includes sequentially connected feedstock processing workshop, the first Pickling-shop, ultrasonic response kettle and the second Pickling-shop according to micro crystal graphite purifying technique, the feedstock processing workshop includes sequentially connected crusher, ball mill, flotation device and centrifuge, first Pickling-shop is identical with the second Pickling-shop, including sequentially connected reaction kettle, cleaning machine, centrifuge and dryer.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 utility model, and significantly reduces the usage amount of hydrofluoric acid, have the advantages of efficient, low energy consumption, and refining effect is good.
Description
Technical field
The utility model is related to micro crystal graphite purification technique fields, are produced more particularly, to a kind of high-purity micro crystal graphite
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 stablize 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 aerospace.
China's native graphite shaping geological conditions is good, widely distributed, resourceful, quality is 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
Two class of graphite, 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 problem of utilization of microcrystalline graphite, deep process technology is horizontal and deep processing ability is relatively low, is 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
The a large amount of of resource are produced to be lost in and waste.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 chiefly used in 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 purify graphite the shortcomings that be to need high-temperature calcination, energy expenditure is big, and purify reaction time it is long, the method pair is set
Standby corrosion is more serious, and is not achieved 99.9% by the graphite purity that the method obtains, although high temperature method refining effect is most
It is good, but its cost is excessively high, capital invested needed for industrialization is huge, hydrogen fluoride purification graphite is efficient, low energy consumption, but hydrogen fluorine
The dosage of acid is huge and has severe toxicity and severe corrosive, causes production equipment and environmentally friendly cost higher, therefore, it is necessary to design a
New micro crystal graphite production system makes up drawbacks described above.
The content of the invention
The technical problems to be solved of the utility model are, fixed carbon limited for prior art chemical purification effect
Content is unable to reach more than 99.9%, and high temperature method cost is excessively high, to further improve graphite purity and reducing the use of hydrofluoric acid
Amount, provides a kind of high-purity micro crystal graphite production system.
The utility model also provides a kind of production technology of high-purity micro crystal graphite production system.
The purpose of this utility model is achieved by the following technical programs：
A kind of high-purity micro crystal graphite production system is provided, is included according to micro crystal graphite purifying technique at sequentially connected raw material
Workshop, the first Pickling-shop, ultrasonic response kettle and the second Pickling-shop are managed, the feedstock processing workshop includes sequentially connected
Crusher, ball mill, flotation device and centrifuge, first Pickling-shop is identical with the second Pickling-shop structure, include according to
Reaction kettle, cleaning machine, centrifuge and the dryer of secondary connection.
Preferably, the crusher is jaw crusher.
Preferably, the crusher, 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 utility model 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 in crusher is crushed, is then fed into ball mill and carries out depth
Ore grinding obtains fineness as -0.074mm grades of materials by ore grinding, is the original that -0.074mm grades of material contents account for 90% to mog
Sample ore carries out flotation in flotation device, and after four selected once purging selection flows of one roughing, magnetic is carried out in centrifuge
Choosing is fixed carbon content as 90% micro crystal graphite；
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, is being reacted first with mixed acid
It is mixed in kettle, mixed acid is HF and H2SO4Mixed acid, wherein the concentration of HF be 7%, H2SO4Concentration for 30%, mixed acid with
Graphite liquid-solid ratio is 3.5:1, normal pressure acidleach, leached mud are carried out after stirring evenly under conditions of 80 DEG C of temperature, reaction time 3h
Washing to pH value is neutrality in cleaning machine, is filtered afterwards in centrifuge, temperature is dry 2 at 80 ~ 150 DEG C in dryer
~ 3h 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 in ultrasonic response kettle are mixed, mixed
Acid is HF and H2SO4Mixed acid, wherein the concentration of HF be 3%, H2SO4Concentration for 20%, mixed acid is 3 with graphite liquid-solid ratio:
1, it stirs evenly and is ultrasonically treated, time 15min obtains 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, it first will be micro-
Spar ink mixed acid solution, which is put into reaction kettle, 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 microlite
Ink.
Compared with prior art, the beneficial effects of the utility model are：
The utility model uses Shandong pool aphanitic graphite as raw material, raw ore is carried out by feedstock processing workshop first preliminary
Processing, then purifies micro crystal graphite using the two step acid-hatchings of young eggs, and fixed carbon content can reach more than 99.9% high-purity crystallite
Graphite, the high-purity micro crystal graphite production system of the utility model significantly reduce the usage amount of hydrofluoric acid, have efficient, energy consumption
It is low, the advantages of refining effect is good.
The utility model is crushed and ground to crystallite stone mill raw ore in feedstock processing workshop, coordinates the once thick of flotation
Four selected once purging selection flows are selected, the purity of raw ore is utmostly improved 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
's）Micro crystal graphite grain size is reduced simultaneously, increases the specific surface area of micro crystal graphite, is conducive to reduce subsequently carrying in follow-up acidleach purification
Pure energy consumption and cost.
The utility model adds in ultrasonic response kettle on the basis of traditional Pickling-shop, carries out at secondary pickling purification
Reason, wherein being significantly reduced for the first time using the impurity volume after acid-hatching of young eggs purification in graphite, metamorphosis is larger, but still with
Particle shape formula exists, and reason is to carry out with reaction, and impurity particle ecto-entad gradually dissolves, and reaction difficulty gradually increases, and
And these precipitations are covered in undissolved impurity particle surface, hinder the further progress of reaction, continue to increase acid at this time
Concentration effect is not obvious, in addition, these precipitations are difficult in itself to be removed in the washed filter stage, the utility model adds in ultrasound
Ripple reaction kettle so that the micro crystal graphite after acidleach purification is additionally separated with impurity, the mechanical powder in ultrasonic procedure
Broken effect and cavitation can crush micro crystal graphite particle, make to be wrapped in the in vivo partial impurities participation reaction of set, add
Fast reaction rate of the impurity with acid, therefore, second of acidleach purification only needs minimal amount of acid to can obtain high-purity microlite
Ink significantly reduces purification energy consumption and cost.
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 flow charts of Fig. 2.
Fig. 3 the first Pickling-shop structure diagrams.
Fig. 4 flotation flowsheet figures.
Specific embodiment
The utility model is further described With reference to embodiment.Wherein, being given for example only property of attached drawing
Illustrate, expression is only schematic diagram rather than pictorial diagram, it is impossible to be interpreted as the limitation to this patent；In order to which this reality is better described
With new embodiment, some components of attached drawing have omission, zoom in or out, and do not represent the size of actual product；To ability
For field technique personnel, some known features and its explanation may be omitted and will be understood by attached drawing.
Embodiment 1
As shown in Figure 1, the present embodiment provides a kind of high-purity micro crystal graphite production system, it is suitable including being purified according to micro crystal graphite
The sequentially connected feedstock processing workshop of sequence, the first Pickling-shop 5, ultrasonic response kettle 6, the second Pickling-shop 7 and packing processes
Machine 8, wherein feedstock processing workshop include sequentially connected crusher 1, ball mill 2, flotation device 3 and centrifuge 4.
As shown in Fig. 2, micro crystal graphite raw ore is crushed by crusher in the present embodiment, broken micro crystal graphite 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, is re-fed into after finishing
It is ultrasonically treated in ultrasonic response kettle 6, completes to be ultrasonically treated, be fed again into the second Pickling-shop 7 and carry out second acidleach
Purification processes finally obtain 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, can realize 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%.
Crusher 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, crusher 1 use jaw crusher, first
5 and second Pickling-shop 7 of Pickling-shop is identical, as shown in figure 3, the first Pickling-shop 5 includes sequentially connected reaction kettle 51, clear
Washing machine 52, centrifuge 53 and dryer 55, microcrystalline graphite material completes acid reaction in reaction kettle 51, afterwards in cleaning machine 52
It with pure water to neutrality, is filtered by centrifuge 53, then carries 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 components are unsuitable for putting together, but when carrying out high-purity micro crystal graphite processing, it is still desirable to
The processed micro crystal graphite of one equipment is sent into a leave from office equipment, 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 in crusher 1 is crushed, is then fed into ball mill 2 and carries out deeply
Ore grinding is spent, fineness is obtained as -0.074mm grades of materials by ore grinding, 90% is accounted for for -0.074mm grades of material contents to mog
Primary sample flotation device 3 carry out flotation, flotation flowsheet as shown in figure 4, using four selected once purging selection flows of one roughing it
Afterwards, magnetic separation is carried out in centrifuge 4, is fixed carbon content as 90% micro crystal graphite；
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, is being reacted first with mixed acid
It is mixed in kettle 51, mixed acid is HF and H2SO4Mixed acid, wherein the concentration of HF be 7%, H2SO4Concentration for 30%, mixed acid
It is 3.5 with graphite liquid-solid ratio:1, normal pressure acidleach is carried out after stirring evenly under conditions of 80 DEG C of temperature, reaction time 3h, is leached
It is neutrality that slag, which is washed in cleaning machine 52 to pH value, afterwards filtering, dry in dryer 54, actual temp in centrifuge 53
For dry 2 ~ 3h at 80 ~ 150 DEG C, the micro crystal graphite that carbon content is 98.82% is fixed；
S22. it is ultrasonically treated：The obtained micro crystal graphites of step S21 and mixed acid in ultrasonic response kettle 6 are mixed, mixed
It is HF and H to close acid2SO4Mixed acid, wherein the concentration of HF be 3%, H2SO4Concentration for 20%, mixed acid is with graphite liquid-solid ratio
3:1, it stirs evenly and is ultrasonically treated, time 15min obtains 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 reaction kettle, 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, is fixed high-purity crystallite that carbon content is 99.98%
Graphite, final packaging storage.
The present embodiment uses Shandong pool aphanitic graphite as raw material, and raw ore is tentatively located by feedstock processing workshop first
Reason, then purifies micro crystal graphite using the two step acid-hatchings of young eggs, and fixed carbon content can reach more than 99.9% high-purity microlite
Ink significantly reduces the usage amount of hydrofluoric acid, has the advantages of efficient, low energy consumption, and refining effect is good.
The present embodiment is crushed and ground to crystallite stone mill raw ore in feedstock processing workshop, coordinates the one roughing of flotation
Four selected once purging selection flows utmostly improve 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 grain size is reduced simultaneously, increases the specific surface area of micro crystal graphite, is conducive to reduce subsequent purification in follow-up acidleach purification
Energy consumption and cost.
The present embodiment adds in 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 exists, and reason is to carry out with reaction, and impurity particle ecto-entad gradually dissolves, and reaction difficulty gradually increases, and
These precipitations are covered in undissolved impurity particle surface, hinder the further progress of reaction, continue to increase the dense of acid at this time
Degree effect is not obvious, in addition, these precipitations are difficult in itself to be removed in the washed filter stage, it is anti-that the present embodiment adds in 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 in vivo partial impurities participation reaction of set, 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 the technical solution of the utility model example, and simultaneously
Non- is the restriction to the embodiment of the utility model.For those of ordinary skill in the art, in above description
On the basis of can also make other variations or changes in different ways.Made within the spirit and principle of the utility model
All any modification, equivalent and improvement etc., should be included within the protection of the utility model claims.
Claims (5)
1. a kind of high-purity micro crystal graphite production system, which is characterized in that include according to micro crystal graphite purifying technique sequentially connected
Feedstock processing workshop, the first Pickling-shop, ultrasonic response kettle and the second Pickling-shop, the feedstock processing workshop are included successively
Crusher, ball mill, flotation device and the centrifuge of connection, first Pickling-shop is identical with the second Pickling-shop structure,
Including sequentially connected reaction kettle, cleaning machine, centrifuge and dryer.
2. high-purity micro crystal graphite production system according to claim 1, which is characterized in that the crusher is jaw crushing
Machine.
3. high-purity micro crystal graphite production system according to claim 1, which is characterized in that the crusher, 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, which is characterized 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, which is characterized in that second Pickling-shop and packaging
By transmitting band connection between processor.
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| CN201721425348.0U CN207418305U (en) | 2017-10-31 | 2017-10-31 | A kind of high-purity micro crystal graphite production system |
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| CN201721425348.0U CN207418305U (en) | 2017-10-31 | 2017-10-31 | A kind of high-purity micro crystal graphite production system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110600737A (en) * | 2019-09-30 | 2019-12-20 | 广东凯金新能源科技股份有限公司 | Preparation method of graphite negative electrode material |
| CN117819541A (en) * | 2024-03-04 | 2024-04-05 | 矿冶科技集团有限公司 | Method for purifying graphite by high-temperature drying-free raw materials and simple acid-base method |
-
2017
- 2017-10-31 CN CN201721425348.0U patent/CN207418305U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110600737A (en) * | 2019-09-30 | 2019-12-20 | 广东凯金新能源科技股份有限公司 | Preparation method of graphite negative electrode material |
| CN117819541A (en) * | 2024-03-04 | 2024-04-05 | 矿冶科技集团有限公司 | Method for purifying graphite by high-temperature drying-free raw materials and simple acid-base method |
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Granted publication date: 20180529 Termination date: 20201031 |