CN105347338B - A kind of method of use light metal halogen high temperature purification native graphite - Google Patents
A kind of method of use light metal halogen high temperature purification native graphite Download PDFInfo
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- CN105347338B CN105347338B CN201510888684.8A CN201510888684A CN105347338B CN 105347338 B CN105347338 B CN 105347338B CN 201510888684 A CN201510888684 A CN 201510888684A CN 105347338 B CN105347338 B CN 105347338B
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Abstract
The invention discloses a kind of method of use light metal halogen high temperature purification native graphite, the method comprises the following steps：Natural graphite powder and light metal halogen are mixed, is stirred, be fitted into pyrographite purification furnace；Pyrographite is purified into stove evacuation；Protective gas is filled with pyrographite purification furnace；Pyrographite purification furnace is heated up, heating rate is 4~20 DEG C/min, temperature rises to 1600~3000 DEG C, 20~120min of soaking time；After insulation, pyrographite purification furnace temperature is down to room temperature, the graphite powder for being purified.The method of present invention light metal halogen high temperature purification native graphite substantially increases the purification purity of graphite, the purification purity of graphite is up to 90.0~99.99%, while the problems such as solving high temperature and be passed through equipment and process complications, equipment corrosion that reacting gas method of purification brings and purify uneven.
Description
Technical field
The present invention relates to graphite chemical technology field, one kind light metal halogen high temperature purification native graphite is more particularly to
Method.
Background technology
Graphite and its product are the basic former materials of modern high temperature, high pressure, high-speed industrial and modern biotechnology, information, the energy
Material, is also the critical material and multifunctional environment friendly material of modern high technology industry, even more nuclear energy, Aero-Space, national defense and military
Field (such as the neutron moderator in nuclear reactor, the stealth material in photoelectronic warfare, attack enemy's power system graphite bomb
Deng) indispensable strategic material.Graphite raw material is processed into graphite material, it must technically be purified first, then
It is processed in granularity, pattern or performance further according to the field applied.The height of graphite purification quality decides graphite material
The use characteristic and combination property of material, graphite purity are higher, and application value is higher.
Graphite purification method mainly has floatation, alkali acid system, hydrogen fluoride, chlorinating roasting and high temperature method, its high temperature
Method is the essential method for obtaining ultra-pure graphite.However, high temperature method exist Technological adaptability it is not strong the shortcomings of, it is relatively low for purity
Graphite raw material, purity lifting it is limited so that ratio for input and output is smaller, the uncontested advantage compared with other method.In this regard, in height
Reacting gas is introduced in warm purification process can effectively improve the Technological adaptability of high temperature purification method, have the excellent of chemical purification concurrently
Point, so as to improve graphite purity and ratio for input and output.However, reacting gas is passed through in high temperature purification stove increased equipment and work
The complexity of skill, and reacting gas may react corrosion to stove inner assembly, have detrimental effect to equipment.In addition, being deposited for substrate
The graphite purification material put, the purification material for being deposited in surface is maximum with reacting gas contact surface, and refining effect is optimal, and in being deposited in
The purification material in portion is smaller with reacting gas contact surface, and refining effect is also accordingly reduced, therefore to the refining effect of this method
Uniformity produces certain influence.
Reacting gas high temperature being passed through in the method for purification of reacting gas is substituted with solid impurity reactant, can be effective
Solve the problems, such as equipment that reacting gas brings and process complications, equipment corrosion and purify uneven.Light metal halogen exists
The gaseous state halogen ion produced under high temperature can generate volatile halide with the impurity reaction of difficult volatilization in graphite, therefore can conduct
A kind of effective solid-state purification auxiliary material is participated in the middle of pyrographite purification.
The content of the invention
(1) technical problem to be solved
The technical problem to be solved in the present invention is exactly to improve graphite purification purity, reduces production cost, and solve graphite carrying
Pure uneven and equipment corrosion problem.
(2) technical scheme
In order to solve the above-mentioned technical problem, the invention provides a kind of side of use light metal halogen high temperature purification native graphite
Method, the method comprises the following steps：
Step one：Natural graphite powder and light metal halogen are mixed, is stirred, be fitted into pyrographite purification furnace；
Step 2：Pyrographite is purified into stove evacuation, pressure to 100Pa and following；
Step 3：Protective gas, pressure to 100~1000Pa of superatmospheric are filled with pyrographite purification furnace；
Step 4：Pyrographite purification furnace is warming up to 1600~3000 DEG C, heating rate is 4~20 DEG C/min, insulation
20~120min；
Step 5：After insulation, pyrographite purification furnace is down to room temperature, rate of temperature fall is 4~20 DEG C/min, is purified
Graphite powder.
Preferably, described native graphite powder purity is 60~95%, and particle diameter is 1~300 μm；Described light metal halogen
Purity for analysis it is pure and more than.
Preferably, the chemical formula of described light metal halogen is MeX, and wherein Me is metal Na, K, and X is halogen Cl, F, Br.
Preferably, described light metal halogen is sodium chloride nacl, sodium fluoride NaF, sodium bromide NaBr, potassium chloride (KCl), fluorine
Change one or more in potassium KF, KBr KBr.
Preferably, natural graphite powder and the weight ratio of light metal halogen mixing are 100：0.1~5.5.
Preferably, described stirring is mechanical agitation, and rotating speed is 5~25 turns/min.
Preferably, the interior chamber size of described graphite purifying furnace is
Preferably, described protective gas is nitrogen or argon gas, and the purity of the nitrogen or argon gas is more than 99.9%.
Preferably, the described flow for being filled with protective gas is 100~4000L/h；Keep graphite purification furnace chamber size
It is 1m with the ratio of shield gas flow rate3：2~10m3/h。
Present invention also offers the graphite obtained by the method with light metal halogen high temperature purification native graphite, the graphite
Purity is 90.0~99.99%.
(3) beneficial effect
The present invention is mixed in providing a kind of new graphite raw material with the method for light metal halogen high temperature purification native graphite
Enter the high temperature native graphite purifying technique of solid purification, compensate for problem that current single purifying technique is individually present, do not have
Extension process cycle, purification purity, the purification purity of graphite that can be reduced production cost, substantially increase graphite are up to 90.0
~99.99%, at the same solve high temperature be passed through equipment that reacting gas method of purification brings and process complications, equipment corrosion and
The problems such as purifying uneven.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the scanning electron microscope diagram of the inventive method purification gained graphite.
Specific embodiment
Embodiments of the present invention are described in further detail with reference to the accompanying drawings and examples.Following examples are used for
The present invention is illustrated, but can not be used for limiting the scope of the present invention.
Embodiment 1：
By natural graphite powder that purity is 76.4% (average grain diameter is 50 μm) with sodium chloride by 100:0.5 weight is than mixing
Stir, agitator speed is 12 turns/min, and batch mixing is loaded into graphite purifying furnace (furnace chamber size)。
After purification furnace is evacuated into 100Pa negative pressure, test Pressure Rise Rate is 10Pa/h.To big flow argon gas is passed through in stove, (purity is
99.999%) 200L/h, is adjusted to argon flow amount after pressure-fired, and is started to warm up, rate of temperature rise is 8 DEG C/min, is warming up to 2200
After DEG C, 60min is kept, subsequent near room temperature, detemperature rate is 8 DEG C/min.Graphite powder purity is promoted to 96.33% after purification.
Embodiment 2：
By natural graphite powder that purity is 76.4% (average grain diameter is 50 μm) with potassium chloride by 100:1.0 weight are than mixing
Stir, agitator speed is 20 turns/min.Batch mixing is loaded into graphite purifying furnace (furnace chamber size), take out
After vacuum to 100Pa negative pressure, test Pressure Rise Rate is 10Pa/h.To big flow argon gas (purity is 99.999%) is passed through in stove, extremely
Argon flow amount is adjusted to 250L/h after pressure-fired, and starts to warm up, and rate of temperature rise is 6 DEG C/min, after being warming up to 2400 DEG C, keeps
80min, is subsequently reduced to room temperature, and detemperature rate is 6 DEG C/min.Graphite powder purity is promoted to 98.92% after purification.Graphite powder after purification
Scanning electron microscope (SEM) photograph see accompanying drawing 1.
Embodiment 3：
By natural graphite powder that purity is 88.2% (particle diameter is 10~100 μm) with sodium chloride by 100:1.5 weight are than mixed
Conjunction stirs, and agitator speed is 22 turns/min.Batch mixing is loaded into graphite purifying furnace (furnace chamber size),
After being evacuated to 100Pa negative pressure, test Pressure Rise Rate is 10Pa/h.To being passed through big flow argon gas (purity is 99.999%) in stove,
Argon flow amount is adjusted to 280L/h after to pressure-fired, and starts to warm up, and rate of temperature rise is 8 DEG C/min, after being warming up to 2600 DEG C, keeps
100min, is subsequently reduced to room temperature, and detemperature rate is 8 DEG C/min.Graphite powder purity is promoted to 99.92% after purification.
Embodiment 4：
By natural graphite powder that purity is 88.2% (particle diameter is 10~100 μm) with sodium fluoride by 100:1.5 weight are than mixed
Conjunction stirs, and agitator speed is 25 turns/min.Batch mixing is loaded into graphite purifying furnace (furnace chamber size),
After being evacuated to 100Pa negative pressure, test Pressure Rise Rate is 10Pa/h.To being passed through big flow argon gas (purity is 99.999%) in stove,
Argon flow amount is adjusted to 250L/h after to pressure-fired, and starts to warm up, and rate of temperature rise is 8 DEG C/min, after being warming up to 2400 DEG C, keeps
100min, is subsequently reduced to room temperature, and detemperature rate is 8 DEG C/min.Graphite powder purity is promoted to 99.24% after purification.
Comparative example 1：
Purification condition with embodiment 1 is identical, but sodium chloride is not mixed into graphite powder, without stirring for.Graphite powder after purification
Purity is promoted to 89.4%.
By comparative example 1 and comparative example 1, single high-temperature physics method of purification is carried to native graphite purity
Rising has certain effect, but purity lifting is limited, and the purity of the graphite obtained using light metal halogen high temperature purification method is obtained
Lifting higher.
Embodiment of above is merely to illustrate the present invention, rather than limitation of the present invention.Although with reference to embodiment to this hair
It is bright to be described in detail, it will be understood by those within the art that, technical scheme is carried out various combinations,
Modification or equivalent, without departure from the spirit and scope of technical solution of the present invention, all should cover will in right of the invention
Ask in the middle of scope.
Claims (1)
1. a kind of method of use light metal halogen high temperature purification native graphite, it is characterised in that the method comprises the following steps：
Step one：Natural graphite powder and light metal halogen are mixed, is stirred, be fitted into pyrographite purification furnace；
Step 2：Pyrographite is purified into stove evacuation, pressure to 100Pa and following；
Step 3：Protective gas, pressure to 100~1000Pa of superatmospheric are filled with pyrographite purification furnace；
Step 4：Pyrographite purification furnace is warming up to 1600~3000 DEG C, heating rate is 4~20 DEG C/min, insulation 20~
120min；
Step 5：After insulation, pyrographite purification furnace is down to room temperature, rate of temperature fall is 4~20 DEG C/min, the stone for being purified
Ink powder；
Described native graphite powder purity is 60~95%, and particle diameter is 1~300 μm；Described light metal halogen purity is analysis
It is pure and more than；
Described light metal halogen is sodium chloride nacl, sodium fluoride NaF, sodium bromide NaBr, potassium chloride (KCl), potassium fluoride KF, bromination
One or more in potassium KBr；
Natural graphite powder and the weight ratio of light metal halogen mixing are 100：0.1~5.5；
Described stirring is mechanical agitation, and rotating speed is 5~25 turns/min；
The interior chamber size of described graphite purifying furnace is
Described protective gas is nitrogen or argon gas, and the purity of the nitrogen or argon gas is more than 99.9%；
The described flow for being filled with protective gas is 100~4000L/h；Keep graphite purification furnace chamber size and protective gas stream
The ratio of amount is 1m3：2~10m3/h。
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| CN107473214A (en) * | 2017-08-30 | 2017-12-15 | 河南理工大学 | A kind of graphite essence purifying technique |
| CN108529615A (en) * | 2018-06-01 | 2018-09-14 | 中钢集团新型材料（浙江）有限公司 | A kind of addition fluoride salt is the graphite purification method of impregnating agent |
| CN108545736A (en) * | 2018-06-01 | 2018-09-18 | 中钢集团新型材料（浙江）有限公司 | A kind of graphite purification method for adding fluoride salt into being formulated |
| CN113830765A (en) * | 2021-09-29 | 2021-12-24 | 大同新成新材料股份有限公司 | Resistance material for purifying isostatic pressing graphite product and purification process thereof |
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| CN101462716A (en) * | 2008-05-05 | 2009-06-24 | 陈怀军 | Preparation technique for purifying graphite by high temperature method |
| CN102001649B (en) * | 2010-11-25 | 2012-07-25 | 洛阳市冠奇工贸有限责任公司 | Purification method for high-purity natural graphite |
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Address after: 410199 No. 1271, liangtang East Road, Xingsha industrial base (Changlong Street), Changsha area, China (Hunan) pilot Free Trade Zone, Changsha, Hunan Province Patentee after: Hunan Dingli Technology Co.,Ltd. Address before: 410199 No. 1271, liangtang East Road, Xingsha industrial base (Changlong Street), Changsha area, China (Hunan) pilot Free Trade Zone, Changsha, Hunan Province Patentee before: ADVANCED CORPORATION FOR MATERIALS & EQUIPMENTS Co.,Ltd. |