CN103172060B - Continuous industrialized natural graphite purification equipment - Google Patents
Continuous industrialized natural graphite purification equipment Download PDFInfo
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- CN103172060B CN103172060B CN2013101280842A CN201310128084A CN103172060B CN 103172060 B CN103172060 B CN 103172060B CN 2013101280842 A CN2013101280842 A CN 2013101280842A CN 201310128084 A CN201310128084 A CN 201310128084A CN 103172060 B CN103172060 B CN 103172060B
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Abstract
The invention relates to continuous industrialized natural graphite purification equipment, and belongs to the technical field of graphite purification. According to the equipment, a furnace body is a closed long cylinder which is sectionally inclined downwards from high to low, and from the high end to the low end in the long cylinder, the long cylinder is divided into a feeding area, a feed buffer area, a low-temperature heating area, a middle-temperature heating area, a high-temperature heating area, a clinker buffer area and a cooling discharging area; an inert gas providing device is connected to the low-temperature heating area, the middle-temperature heating area and the high-temperature heating area of the closed long cylinder respectively; a byproduct recovery device and an inert gas curtain are arranged in the feed buffer area; and an inert gas curtain with the same structure is also arranged in the clinker buffer area. By using the continuous industrialized natural graphite purification equipment, high-purity microcrystal graphite powder of which the purity is 99%, 99.9% or 99.99% can be produced, atmospheric emissions are not generated, and the high-quality natural graphite is continuously purified at normal pressure, high temperature and low cost.
Description
Technical field
The present invention relates to the specific equipment that natural graphite is purified, particularly a kind of continuous industrial natural graphite purifying device.
Background technology
In recent years, to the increase of high purity graphite demand, graphite purification was subject to again many experts and scholars' attention, dropped into one after another experimental study due to both at home and abroad.When the natural graphite carbon content is 70-90%, be called medium-carbon graphite, its impurity is metallic iron, and aluminium and nonmetal silicon etc., bring up to 98-99% and even 99.9% with the carbon content of medium-carbon graphite, namely is referred to as high-carbon graphite or high purity graphite.Graphite purification, forefathers had done a lot of tests, and the condition that different times is different, obtain different results.According to investigating of contriver, as far back as the end of the eighties, just someone utilizes the chemical process purification processing, adopts strong acid HF or highly basic (NaOH)+hydrochloric acid (HCl) and the impurity of graphite to react, and generates soluble substance, then through washing, impurity is removed.This method, so-called wet chemical is purified.Take the graphite grade after this Methods For Purification also can reach 99% preferably the time, but while producing in a large number, because raw ore foreign matter content and composition are not quite similar, the ratio of acid, alkali is difficult to grasp, so after purifying, the discreteness of graphite grade is very large, on average get off and can only reach 94%-96%, the consumption of this method acid, alkali is large, and production cost is high, and per ton cost reaches 2700 yuan of-3000 yuan of left and right, under market condition at that time, can't sell at all.In today, the problem that the method is more serious be can working the mischief property environmental pollution, difficulty of governance is very large, also will consume a large amount of water resourcess simultaneously, does not obviously meet the requirement of Sustainable development.
According to investigating, the inventor thinks the mineral deposit that pyromagma invaded coal layer that the natural graphite of some areas of China is the earth's core due to its origin cause of formation forms, thus graphite crystal minimum≤1 μ m, claim micro crystal graphite.The impurity of this graphite separates very difficult with chemical process.Realize the industrial mass purification of this graphite, only have the pyroprocess of employing to realize.This is also many universities and colleges, the experts and scholars' of scientific research institutions common view.They also do not carry out the research of this respect in view of the restriction of scientific research condition, equipment, funds.
The ultimate principle of micro crystal graphite high temperature purification method is to utilize the resistant to elevated temperatures characteristics of graphite energy, and graphite is placed in special High Temperature Furnaces Heating Apparatus, and isolated air heating, to certain temperature, makes the impurity gasification in natural graphite and is evaporated away.Can know the analysis of graphite raw ore and experiment from us, this temperature will reach more than 2700 ℃.
The inventor once attempted with high temperature purification method purification natural graphite, as on 08 03rd, 2005, the inventor is in Chinese utility model notification number CN2714538Y, " a kind of continuous industrial natural graphite purifying device " proposed, its structure comprises that mainly storehouse, feed(raw material)inlet, body of heater and outlet storehouse, body of heater are a totally enclosed long cylindrical shell, from an end of cylindrical shell start to the other end be divided into successively intake zone, low-temperature heat district, warm heating zone and heat district, material discharge region cools; This equipment is connected with rare gas element circulation device and vacuum extractor on cylindrical shell, although can under the hot conditions more than 2700 ℃, be purified to natural graphite in principle continuously.But find while implementing to have following problem: 1) system will be worked under isolated air negative pressure condition, makes the sealing of body of heater cylindrical shell require high, and feed(raw material)inlet, outlet sealing structure on body of heater have particular requirement.Sealing difficulty is large, also will have simultaneously complicated vacuum apparatus to guarantee; 2) spiral propeller of high-purity graphite carbon pipe easily damages in hot environment, causes and can't work fast; 3) because system needs non-stop run, the entrance storehouse of raw material and outlet storehouse are to be in heating zone, directly communicating of opening-wide state, cause a large amount of device that is evacuated of rare gas element in heating zone to be taken away, rare gas element consumption is large, cause the high temperature oxidation of refractory materials in heating zone, production cost is higher simultaneously.
Summary of the invention
Technical problem to be solved by this invention is: in view of the foregoing defects the prior art has, redesign a kind of continuous industrial natural graphite purifying device., to overcome above-mentioned deficiency, can produce high-purity microlite ink powder of 99%, 99.9%, 99.99%; There is no atmospheric emission, under atmospheric pressure state, realize that serialization is low-cost, the high temperature purification natural graphite.
The technical scheme of technical solution problem of the present invention is such: a kind of continuous industrial natural graphite purifying device, comprise that storehouse, feed(raw material)inlet, body of heater and outlet storehouse, body of heater are the long cylindrical shell of sealing that tilts of segmentation downwards from high to low, this long cylindrical shell interior from high-end start to low side be divided into successively intake zone, charging buffer zone, low-temperature heat district, warm heating zone, heat district, grog buffer zone and the material discharge region that cools; Be connected with the rare gas element generator on the basic, normal, high temperature heating zone of the long cylindrical shell of above-mentioned sealing; Described intake zone is the cylindrical shell that one section most significant end has end socket, and the perisporium of cylindrical shell is a three-decker that is comprised of housing skin, high-temperature insulation filled insulation interlayer, high-purity graphite carbon inner tube layer, and the top of cylindrical shell is provided with the storehouse, feed(raw material)inlet; The cylindrical shell that described basic, normal, high temperature heating zone is respectively more than one section is composed in series successively, come top low-temperature heat district and tap into the material buffer zone, one section last heat district connects the grog buffer zone, every section heating zone forms by housing skin, liquid cooling tube layer, high-temperature insulation filled insulation interlayer, high purity graphite carbon tube furnace thorax internal layer, is laid with heating installation around high purity graphite carbon tube furnace thorax; The present invention also is provided with by-product plant on the outer field corresponding position of charging buffer zone housing, described by-product plant is connected to form by inert gas cooler, pipeline, aspirator pump and switching valve; The described material discharge region that cools is also to be composed in series successively with upper shell by two sections, and every section cooling area or cooling material discharge region form by double hull, internal layer high-purity graphite carbon pipe, lays liquid cooling tube in the double hull interlayer; Except laying liquid cooling tube, also be laid with coil tube type or diaphragm type vaporizer in the double hull interlayer of first paragraph cooling area, the interior filling refrigerant of vaporizer also passes through the outer refrigeration compressor of pipe and body of heater and is connected; The final stage material discharge region that cools is connected with a totally-enclosed high purity graphite outlet storehouse; The liquid cooling tube of the pipeline of above-mentioned basic, normal, high temperature heating zone liquid cooling tube layer and the material discharge region double hull interlayer that cools is one another in series identical, by feed liquor house steward, time liquid house steward and liquid circulating pump, is connected to the outer cooling tower of body of heater; The present invention is respectively arranging an identical inert gas curtain device of structure above the transverse section of above-mentioned charging buffer zone graphite carbon inner tube layer with above the transverse section of grog buffer zone graphite carbon inner tube layer; Described inert gas curtain device is by fire-resistant impeller, backboard, and drive-motor and flow deflector form; Flow deflector semi-surrounding fire-resistant impeller, the top of flow deflector and graphite carbon inner tube layer surface forms gas returning port, flow deflector form below the air outlet of the shape that is rectangle with backboard, it is long parallel and mouthful hold down to the transverse section with the graphite carbon inner tube layer; Drive-motor is positioned at outside body of heater, connects the fire-resistant impeller of body of heater graphite carbon inner tube layer by main shaft.
Principle of work of the present invention is: the natural graphite powder raw material through grinding and processing enters from the entrance storehouse, relies on Graphite Powder 99 deadweight and good sliding, natural flow in the long cylindrical shell of sealing that tilts; Enter low-temperature heat district, middle temperature heating zone and the heat district that is full of rare gas element through intake zone, charging buffer zone; Natural graphite powder under the isolated air conservation condition of the rare gas element in heat district, is heated to the high temperature more than 2700 ℃, makes the impurity in natural graphite gasify and be volatilized away, becomes the pure graphite of high temperature; The pure graphite of high temperature stirs through grog buffer zone inert gas, further makes residual impurity gasification volatilization in the pure graphite of high temperature, the pure graphite of high temperature enter the material discharge region that cools force cooling after, derive from totally-enclosed high purity graphite outlet storehouse.Thereby realize under atmospheric pressure state, serialization is low-cost, the function of high temperature purification natural graphite, has solved the technical problem of continuous industrial batch purifying graphite.The foreign gas that gasifies from natural graphite in heating zone, under the aspirator pump effect in by-product plant, along the graphite carbon pipe that tilts from bottom to top, rise to arrive in by-product plant is recovered foreign gas.The rare gas element in above-mentioned heat district is supplied with by the rare gas element generator, and relies on charging buffer zone inert gas curtain device and grog buffer zone inert gas curtain device to form the shutoff of " dynamically ".The furnace shell of basic, normal, high temperature heating zone, grog buffer zone and the material discharge region that cools of the long cylindrical shell of above-mentioned sealing is cooling is to adopt circulating cooling.
Compared with the prior art, innovative point of the present invention is:
1. utilize the deadweight of natural graphite powder and lubricate natural flow characteristic in the long cylindrical shell of sealing that tilts, realized that dexterously furnace charge advances automatically, omitted spiral propeller; Thereby overcome spiral propeller easy damage problem in hot environment of prior art;
2. the present invention arranges the charging buffer zone at intake zone, the grog buffer zone is set before the material discharge region that cools, not only solved the homogeneity question of furnace charge natural flow, also utilize two buffer zones to form the twice inert gas curtain, the escape consumption problem that has stopped heat district rare gas element, can allow again Graphite Powder 99 pass through smoothly, realize constant-pressure and high-temperature purification graphite; Thereby really realized the function that serialization is produced; In addition,, owing to being provided with the inert gas curtain device, can also blow furnace charge by adjusting the air strength of twice inert gas curtain, produce and realized stirring the beyond thought technique effect of furnace charge;
3. the present invention can produce high-purity microlite ink powder of 99%, 99.9%, 99.99%; There is no the air pollution emission thing, there is no the underground pollution discharge yet.Level of automation of the present invention is higher, belongs to domestic initiation.The present invention cools back debit's face at impurity and has used by-product plant, has overcome and has produced the pollution of discharge to environment, has novelty;
4. the present invention is through implementing check, and the performance index that reach are as follows;
Industrial scale of the present invention is for the high-purity microlite ink powder of daily output greater than 30 tons, and annual output approaches and reaches ten thousand tons.Production cost 99% be 2700 yuan/tons; 99.9% be 3100 yuan/tons; 99.99% be 3500 yuan/tons.
Description of drawings
Fig. 1 is structural representation of the present invention.
In accompanying drawing: 1 storehouse, feed(raw material)inlet; 2 bodies of heater and outlet storehouse; 3 intake zones; 4 charging buffer zones; 5 low-temperature heat districts; Warm heating zone in 6; 7 heat districts; 8 grog buffer zones; 9 material discharge regions that cool; 10 rare gas element generators; 11 heating installations; 12 by-product plants; 13 vaporizers; 14 refrigeration compressors; 15 feed liquor house stewards; 16 times liquid house stewards; 17 liquid circulating pumps; 18 cooling towers; 19 inert gas curtain devices.
Embodiment
Be below with reference to accompanying drawing some specific descriptions to embodiment of the present invention, but must know, this embodiment can not be used for being construed as limiting the invention.
Accompanying drawing 1 has been described 30 tons of continuous industrial natural graphite purifying devices of a kind of daily output, comprises storehouse, feed(raw material)inlet 1, body of heater and outlet storehouse 2; Body of heater is the long cylindrical shell of sealing that tilts of segmentation downwards from high to low, this long cylindrical shell interior from high-end start to low side be divided into successively intake zone 3, charging buffer zone 4, low-temperature heat district 5, warm heating zone 6, heat district 7, grog buffer zone 8 and the material discharge region 9 that cools; , in order to make the impurity in micro crystal graphite melt, gasify and be volatilized away, be connected with rare gas element generator 10 on the basic, normal, high temperature heating zone 7 of the long cylindrical shell of above-mentioned sealing under the condition of isolated air; Described intake zone 3 is the cylindrical shell that one section most significant end has end socket, and the perisporium of cylindrical shell is a three-decker that is comprised of housing skin, high-temperature insulation filled insulation interlayer, high-purity graphite carbon inner tube layer, and the top of cylindrical shell is provided with storehouse, feed(raw material)inlet 1; In order to make natural graphite reach high-temperature digestion condition more than 2700 ℃, of the present inventionly add the way that the thermal recovery subregion heats up piecemeal, the cylindrical shell that described basic, normal, high temperature heating zone is respectively more than one section is composed in series successively, come top low-temperature heat district 5 and tap into material buffer zone 4, one section last heat district 7 connects grog buffer zone 8, every section heating zone forms by housing skin, liquid cooling tube layer, high-temperature insulation filled insulation interlayer, high purity graphite carbon tube furnace thorax internal layer, is laid with heating installation 11 around high purity graphite carbon tube furnace thorax; In order to overcome the impurity vaporizing, discharging thing contaminate environment in natural graphite, the present invention also is provided with by-product plant 12 on the charging buffer zone 4 outer field corresponding positions of housing, described by-product plant 12 is connected to form by inert gas cooler, pipeline, aspirator pump and switching valve; The described material discharge region 9 that cools is also to be composed in series successively with upper shell by two sections, and every section cooling area or cooling material discharge region form by double hull, internal layer high-purity graphite carbon pipe, lays liquid cooling tube in the double hull interlayer; In order to strengthen cooling performance, except laying liquid cooling tube, also be laid with coil tube type or diaphragm type vaporizer 13 in the double hull interlayer of first paragraph cooling area, the interior filling refrigerant of vaporizer 13 also is connected by the outer refrigeration compressor 14 of pipe and body of heater; The final stage material discharge region 9 that cools is connected with a totally-enclosed high purity graphite outlet storehouse 2; The liquid cooling tube of the pipeline of above-mentioned basic, normal, high temperature heating zone liquid cooling tube layer and the material discharge region 9 double hull interlayers that cool is one another in series identical, by feed liquor house steward 15, time liquid house steward 16 and liquid circulating pump 17, is connected to the outer cooling tower 18 of body of heater; For reduce rare gas element in heating zone from storehouse, feed(raw material)inlet 1, the opening part in body of heater and outlet storehouse 2 escapes and consumes; The present invention is respectively arranging an identical inert gas curtain device 19 of structure above the transverse section of above-mentioned charging buffer zone 4 graphite carbon inner tube layers with above the transverse section of grog buffer zone 8 graphite carbon inner tube layers; Described inert gas curtain device 19 is by fire-resistant impeller, backboard, and drive-motor and flow deflector form; Flow deflector semi-surrounding fire-resistant impeller, the top of flow deflector and graphite carbon inner tube layer surface forms gas returning port, flow deflector form below the air outlet of the shape that is rectangle with backboard, it is long parallel and mouthful hold down to the transverse section with the graphite carbon inner tube layer; Drive-motor is positioned at outside body of heater, connects the fire-resistant impeller of body of heater graphite carbon inner tube layer by main shaft.
Claims (2)
1. a continuous industrial natural graphite purifying device, comprise storehouse, feed(raw material)inlet (1), body of heater and outlet storehouse (2); It is characterized in that: body of heater is the long cylindrical shell of sealing that tilts of segmentation downwards from high to low, this long cylindrical shell interior from high-end start to low side be divided into successively intake zone (3), charging buffer zone (4), low-temperature heat district (5), warm heating zone (6), heat district (7), grog buffer zone (8) and the material discharge region that cools (9); Be connected with rare gas element generator (10) on the basic, normal, high temperature heating zone (5,6,7) of the long cylindrical shell of above-mentioned sealing; Described intake zone (3) is the cylindrical shell that one section most significant end has end socket, and the perisporium of cylindrical shell is a three-decker that is comprised of housing skin, high-temperature insulation filled insulation interlayer, high-purity graphite carbon inner tube layer, and the top of cylindrical shell is provided with storehouse, feed(raw material)inlet (1); The cylindrical shell that described basic, normal, high temperature heating zone (5,6,7) is respectively more than one section is composed in series successively, come top low-temperature heat district (5) and tap into material buffer zone (4), the final stage in heat district (7) connects grog buffer zone (8), every section heating zone forms by housing skin, liquid cooling tube layer, high-temperature insulation filled insulation interlayer, high purity graphite carbon tube furnace thorax internal layer, is laid with heating installation (11) around high purity graphite carbon tube furnace thorax; Also be provided with by-product plant (12) on the outer field corresponding position of charging buffer zone (4) housing, described by-product plant (12) is connected to form by inert gas cooler, pipeline, aspirator pump and switching valve; The described material discharge region that cools (9) is also to be composed in series successively with upper shell by two sections, and every section of the material discharge region that cools (9) forms by double hull, internal layer high-purity graphite carbon pipe, lays liquid cooling tube in the double hull interlayer; Cool in the double hull interlayer of first paragraph of material discharge region (9) except laying liquid cooling tube, also be laid with coil tube type or diaphragm type vaporizer (13), interior the filling refrigerant of vaporizer (13) also is connected by the refrigeration compressor (14) outside pipe and body of heater; The final stage of material discharge region (9) of cooling is connected with a totally-enclosed high purity graphite outlet storehouse (2); The liquid cooling tube of the pipeline of above-mentioned basic, normal, high temperature heating zone (5,6,7) liquid cooling tube layer and material discharge region (9) the double hull interlayer that cools is one another in series and communicates, and by feed liquor house steward (15), time liquid house steward (16) and liquid circulating pump (17), is connected to the outer cooling tower (18) of body of heater; In the top, transverse section of above-mentioned charging buffer zone (4) graphite carbon inner tube layer and the top, transverse section of grog buffer zone (8) graphite carbon inner tube layer, an inert gas curtain device (19) that structure is identical is set respectively.
2. continuous industrial natural graphite purifying device according to claim 1, it is characterized in that: described inert gas curtain device (19) is by fire-resistant impeller, backboard, and drive-motor and flow deflector form; Flow deflector semi-surrounding fire-resistant impeller, the top of flow deflector and graphite carbon inner tube layer surface forms gas returning port, flow deflector form below the air outlet of the shape that is rectangle with backboard, it is long parallel and mouthful hold down to the transverse section with the graphite carbon inner tube layer; Drive-motor is positioned at outside body of heater, connects the fire-resistant impeller of body of heater graphite carbon inner tube layer by main shaft.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101280842A CN103172060B (en) | 2013-04-15 | 2013-04-15 | Continuous industrialized natural graphite purification equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101280842A CN103172060B (en) | 2013-04-15 | 2013-04-15 | Continuous industrialized natural graphite purification equipment |
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| Publication Number | Publication Date |
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| CN103172060A CN103172060A (en) | 2013-06-26 |
| CN103172060B true CN103172060B (en) | 2013-11-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2013101280842A Expired - Fee Related CN103172060B (en) | 2013-04-15 | 2013-04-15 | Continuous industrialized natural graphite purification equipment |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104627991A (en) * | 2013-11-14 | 2015-05-20 | 王修海 | Special fusion furnace for graphite purification through alkali-acid method |
| CN111228834B (en) * | 2020-02-17 | 2021-09-28 | 北京航空航天大学 | High-vacuum continuous graphite purification device and application thereof |
| CN112546659B (en) * | 2020-12-08 | 2022-02-15 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2690373Y (en) * | 2004-04-26 | 2005-04-06 | 朱兴发 | Vacuum high temperatare continuous micro crystal graphite purifting producing device |
| CN2714538Y (en) * | 2004-04-30 | 2005-08-03 | 郴州精工石墨有限公司 | Continuous industrial natural graphite purifying device |
| CN1310833C (en) * | 2004-11-15 | 2007-04-18 | 镇江焦化煤气集团有限公司 | Continuous production and apparatus for high-purity graphite carbon material |
| CN102923699B (en) * | 2012-11-26 | 2015-07-01 | 鹤岗市华信科技有限公司 | Continuous pyrographite purifying device |
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