CN1040638C - High-temp chlorination refining process for natural graphite - Google Patents
High-temp chlorination refining process for natural graphite Download PDFInfo
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- CN1040638C CN1040638C CN94105051A CN94105051A CN1040638C CN 1040638 C CN1040638 C CN 1040638C CN 94105051 A CN94105051 A CN 94105051A CN 94105051 A CN94105051 A CN 94105051A CN 1040638 C CN1040638 C CN 1040638C
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Abstract
The present invention relates to a high-temperature chlorination purification technology of natural graphite, which is characterized in that the natural graphite is chlorinated in a reaction furnace at a high temperature under the action of a catalyst and a reducing agent in the mode that chlorine permeates through a bulk material layer of materials or in the mode that the chlorine is fluidized, and impurities of the natural graphite are simultaneously recovered as byproducts in the modes of chlorides in the purification process. The technology has the advantages of high purity of the purified product, high quality of the purified product, little energy consumption, low cost and simple operation. The technology is suitable for the purification of the natural graphite with all particle sizes and all mixed particle sizes, and the carbon content of the graphite is from 98% to 99%.
Description
The present invention relates to high-temp chlorination refining process for natural graphite and specific equipment thereof, belong to nonmetal purifying field.
When the natural graphite carbon content is 85-90%, be called medium-carbon graphite, its impurity is metallic iron, and aluminium and nonmetal silicon are brought up to 98-99% and even 99.9% with the carbon content of medium-carbon graphite, promptly are referred to as high-carbon graphite or high purity graphite.The employing acid-base method that the medium-carbon graphite method of purification has is with the molten medium-carbon graphite that soaks of hydrochloric acid, with heating or after heating means are not removed metallic impurity, reusable heat alkali lye or molten caustic soda are removed nonmetallic impurity, this processing method flow process complexity, and the graphite loss is big, the cost height, three-waste pollution is serious; Also useful acidic process, at first with HF or HF and Hcl in heating or not under the heating condition, leach metal and nonmetallic impurity, the same flow process complexity of this method, the graphite loss is big, the cost height, three-waste pollution is serious; Also have and adopt high-temperature chlorination that synthetic graphite piece and goods are purified, this method chlorination temperature is higher, reaches 2000 ℃, and the time is long, and current consumption is big, periodical operation, and can not handle for the natural graphite bulk cargo.
Purpose of the present invention is the shortcoming and deficiency in order to overcome above-mentioned prior art just, and provide a kind of under sealing condition, adopting the logical chlorine of infiltration and streaming mode to carry out high-temp chlorination in Reaktionsofen purifies, its impurity is chloride form and reclaims as paying product, thereby improves the purity of natural graphite.
The objective of the invention is to realize by following technical proposal:
High-temp chlorination refining process for natural graphite; be metal in the medium-carbon graphite and nonmetallic impurity to be removed with the pyrochemistry method; comprise stock grading; storing material; in Reaktionsofen, carry out high-temperature chlorination; remove impurity and obtain high-carbon or high purity graphite product; waste gas carries out purifying treatment; it is characterized in that under protection of inert gas, middle carbon natural graphite material being stored in the sealing feed bin; in Reaktionsofen, adopt chlorine and the infiltration of material bulk cargo layer or fluidization mode by carrying out high-temperature chlorination under catalyzer and/or the reductive agent effect; utilize negative pressure to reclaim major product again; according to the muriate condensing temperature difference of impurity, its impurity is chloride form reclaims simultaneously as paying product.
Wherein said rare gas element is N
2Or CO; Reaktionsofen carries out indirect heating with Sweet natural gas, coal gas or utilizes the resistance Reaktionsofen energising direct heating of graphite material bed of material resistance to produce high temperature; The high-temp chlorination temperature is 1100-1700 ℃; Catalyzer is Na
2CO
3, K
2CO
3, NH
4F, H
3BO
3, B
2O
3, KClO
4, also can use its consumption to be 5-10% by weight any two kinds of mixing of above-mentioned catalyzer; Reductive agent adopts solid reductant that refinery coke, high grade activated carbon, hard coal are arranged, and its consumption is 5-10%, and gaseous reducing agent has CO, phosgene, fluorine Lyons; When the logical chlorine of high-temp chlorination carried out with penetration mode, its chlorine was infiltrated by graphite bed of material top, and waste gas is discharged by material layer lower part; When carrying out in the fluidization mode, its chlorine is blasted by the graphite material layer lower part, and waste gas is discharged by bed of material top; It is iron trichloride, aluminum chloride and silicon tetrachloride that impurity chlorides is paid product, and it is 200-350 ℃ that its condensing temperature reclaims iron trichloride for first section, and second section is reclaimed aluminum chloride is 150-178 ℃, and the 3rd section is reclaimed silicon tetrachloride is 55-60 ℃; Penetration mode or fluidization mode high-temperature chlorination adopt tubular Reaktionsofen, and penetration mode also can adopt the resistance Reaktionsofen.
The used tubular Reaktionsofen of specific equipment of purifying technique of the present invention is by body of heater, the burning gas nozzle, reactor, feed-pipe, discharge nozzle, inlet pipe, vapor pipe, air distribution plate and filler are formed, body of heater is equipped with burning gas nozzle 5 on 37 two sides, tubular reactor 4 is housed in the body of heater 37, air distribution plate 1 and packing layer 3 are equipped with down in reactor 4 bottoms, the feed-pipe 11 that is connected with feed bin 12 is equipped with in reactor 4 tops, with rotoclone collector 14, filter the major product discharge nozzle 13 that collector 15 is connected with vacuum pump, the inlet pipe 10 that is connected with valve control system, a reactor bottom waste gas exhaust pipe 20 and a pair product withdrawing can 19,18,17 connect, and remainder of exhaust gas is handled by purification system.
Tubular Reaktionsofen inlet pipe 10 also can be installed in reactor 4 bottoms, and at packing layer 3 by adorning upper and lower air distribution plate 1,25, its waste gas exhaust pipe 20 is installed in reactor 4 tops and pays a product recovery system and be connected.
The resistance Reaktionsofen that purifying technique of the present invention is used, it is made up of body of heater, electrode bar, battery lead plate, air distribution plate, filler, air chamber, feed-pipe, inlet pipe, vapor pipe, discharge nozzle, cleaning eye, the inboard loading electrode rod 30 in body of heater 31 two ends, battery lead plate 32, upper and lower two air distribution plates 1,25 are equipped with in body of heater 31 bottoms, the centre is a packing layer 3, and a plurality of Cl are equipped with in the body of heater top
2Y-tube with CO inlet pipe 28,29 and feed-pipe 27 compositions, below air chamber 33 has cleaning eye 35 and vapor pipe 34, vapor pipe 34 is connected with a pair product withdrawing can, on body of heater 31 sidewalls discharge nozzle 36 is being housed above the last air distribution plate, is filtering collector 15 by rotoclone collector 14 and be connected with vacuum pump.
Wherein tubular Reaktionsofen is made of phosphoric acid salt, corundum material, and resistance furnace is made lining with graphite, phosphoric acid salt, corundum material, and filler adopts graphite or corundum material to be made as spheroidal and fills out product, and ball warp is 2-10mm.The cloth porosity of the air distribution plate of Reaktionsofen is 7-10%, and the aperture is 0.1-1.0mm.
Owing to take technique scheme, make the present invention compared with the prior art have following advantage and effect:
A) be reflected at tightness system and carry out, the chlorine consumption is little, and is easy to operate, pollutes fewly, can connect operation, but also intermittent action, the heat utilization efficiency height;
B) good product quality, the purification rate height, the graphite loss is few, and can comprehensively reclaim the impurity chlorides product;
C) applied widely, can require flexible adjusting process condition according to material properties with to product purity.
Description of drawings:
Fig. 1 penetration mode high-temp chlorination refining process schema;
Fig. 2 is a fluidised form mode high-temp chlorination refining process schema;
Fig. 3 is a resistance Reaktionsofen structural representation;
Fig. 4 is the A-A sectional view of Fig. 3.
Embodiment further describes the technology of the present invention below in conjunction with accompanying drawing:
High-temp chlorination refining process for natural graphite; as shown in Figure 1; comprise stock grading; storing material; in Reaktionsofen, carry out high-temperature chlorination; remove impurity and obtain high-carbon or high purity graphite product; waste gas carries out purifying treatment; it is characterized in that under protection of inert gas, middle carbon natural graphite material being stored in the sealing feed bin; in Reaktionsofen, adopt chlorine and the infiltration of material bulk cargo layer or fluidization mode by catalyzer with or the reductive agent effect under carry out high-temperature chlorination; utilize negative pressure to reclaim major product again; according to the muriate condensing temperature difference of impurity, its impurity is chloride form reclaims simultaneously as paying product.
Wherein seal feed bin and prevent that as rare gas element oxygen from entering the chlorination reaction stove with nitrogen or carbon monoxide; High-temp chlorination adopt Sweet natural gas or coal gas carry out Reaktionsofen between heat heating heat supply, perhaps utilize the resistance furnace energising direct heating heat supply of graphite bed of material resistance, according to material properties decision heating and logical chlorine mode; The high-temp chlorination temperature is 1100-1700 ℃, and temperature is high more, and purification purity is high more, time of chlorinating 1-4 hour; High-purity for obtaining (99.9%) graphite products needs 8 hours time expands; The catalyzer that chlorination reaction adopted is Na
2CO
3, K
2CO
3, H
4F, H
3BO
3, B
2O
3, KClO
4, also above-mentioned catalyzer can be mixed use for any two kinds, its consumption is 5-10%, this catalyzer is simple to operate, and reductive agent adopts solid reductant refinery coke to be arranged, high grade activated carbon, hard coal, granularity is 3-0.075mm, and its consumption is 5-10%, the back graphite of purifying, with sieve solid reductant is sifted out, gaseous reducing agent has CO, phosgene, fluorine Lyons, and ventilating mode mixes with chlorine or adds by turns all can.
When chlorine carried out chlorination with the layer material that loose with penetration mode, its chlorine was infiltrated by graphite material top, and waste gas is discharged by material layer lower part, and when carrying out in the fluidised form mode, its chlorine is blasted by the graphite material layer lower part, and waste gas is discharged by bed of material top.
It is iron trichloride, aluminum chloride and silicon tetrachloride that muriate is paid product, segmentation condensation waste gas and obtaining, first section is reclaimed 200-350 ℃ of iron(ic) chloride condensing temperature, second section is reclaimed aluminum chloride is 150-178 ℃, the 3rd section is reclaimed silicon tetrachloride is 55-60 ℃, and residue chlorine is with liming or water purifying treatment.
Chlorination reaction penetration mode or fluidised form mode adopt tubular Reaktionsofen, promptly use Sweet natural gas, the coal gas indirect heating, penetration mode also can adopt resistance Reaktionsofen electricity consumption (direct current or alternating-current) direct heating, Fig. 1 is a penetration mode high-temp chlorination refining process schema, Reaktionsofen is a tubular react furnace among the figure, by body of heater, the burning gas nozzle, reactor, feed-pipe, discharge nozzle, inlet pipe, vapor pipe, air distribution plate and filler are formed, body of heater is equipped with burning gas nozzle 5 on 37 two sides, tubular reactor 4 is housed in the body of heater, reactor bottom is equipped with down air distribution plate 1 and packing layer 3, the feed-pipe 11 that is connected with feed bin 12 is equipped with in the reactor top, with rotoclone collector 14, filter the major product discharge nozzle 13 that collector 15 is connected with vacuum pump, the inlet pipe 10 that is connected with valve control system, a reactor bottom waste gas exhaust pipe 20 and a pair product withdrawing can 19,18,17 connect, and remainder of exhaust gas is handled by purification system.，
It carries out high-temp chlorination with Sweet natural gas or coal gas indirect heating, the combustion gas of combustion gas from body of heater 37 sidewalls, nozzle 5 sprays into 6 burnings of Reaktionsofen combustion chamber, flue gas is discharged from flue 2, the intravital tubular reactor of Reaktionsofen 4 tops are equipped with feed-pipe 11 and are connected with sealing storehouse 12, feed bin is by upper and lower sealing damper 21,22 sealings, and by blow-off valve 23 control chargings, inlet pipe 10 is by air valve control system 7 and cl
2Inlet pipe 8 is connected with CO inlet pipe 9, discharge nozzle 13, and rotoclone collector 14 filters collector 15 and is connected with vacuum pump generation negative pressure pipe 24, obtains major product, and feed-pipe stretches in the furnace chamber, with the graphite bulk cargo sucking-off after purifying, fills N in the furnace chamber before the discharging
2Or CO gas, cleaning residue chlorine.Equally distributed hole is arranged on the reactor bottom air distribution plate 1, packing layer 3 is made up of multilayer spheroidal filler, aperture and sphere diameter are selected size according to raw meal particle size, waste gas exhaust pipe 20 is connected with iron trichloride withdrawing can 9 aluminum chloride withdrawing cans 18 silicon tetrachloride withdrawing cans 17, residue chlorine makes exhaust gas emission meet environmental standard with liming or water leaching tower 16 spray cleanings.
Extraction process of the present invention adopts the tubular Reaktionsofen inlet pipe 10 of tubular type also can be installed in reactor bottom, and is shown in Figure 2, and at packing layer by adorning upper and lower air distribution plate 1,25, its waste gas exhaust pipe 20 is installed in the reactor top and is connected with a pair product recovery system.
Fig. 3,4 is the resistance furnace structure iron, be used for the logical chlorine purifying technique of penetration mode, electricity consumption direct heating high-temperature chlorination, electrode bar 30 is equipped with in inboard, body of heater 31 two ends, battery lead plate 32, bottom of furnace body are equipped with upper and lower gas distribution 1,25, the middle multilayer packing layer of making of corundum 3, a plurality of CO gas inlet pipe 29, Cl are equipped with in the body of heater top
2Gas inlet pipe 28 and feed-pipe 27 formed Y-tubes, and below air chamber 33 has cleaning eye 35 and waste gas exhaust pipe 4, on the sidewall of the furnace body discharge nozzle 36 is being housed above the last cloth gas, and discharge nozzle is connected by Fig. 1 mode respectively with waste pipe and gets final product.
Embodiment 1:
Test by the technical process of Fig. 1 that to adopt carbon content be 88% natural graphite, granularity+80,50 kilograms of weight add 2.5 kilograms of solid reductive agent refinery cokes, reaction boiler tube shaped reaction organ pipe footpath 40mm, high 2000mm, qi-emitting hole aperture 0.5mm, percentage of open area 10%, corundum ball packing layer, sphere diameter 66mm.
With 50 kilograms of natural graphites with go in the reactor during refinery coke mixes, after logical nitrogen is driven air out of, open the burning gas nozzle, heat up, when temperature of reaction reaches 600 ℃, lead to chlorine, carry out high-temperature chlorination, temperature 1100-1200 ℃, 2 hours time, reaction is removed the refinery coke reductive agent with sieve after finishing, major product natural graphite average purity is 98.49%, is up to 99.55%.
Embodiment 2:
Press Fig. 2 fluidization mode high-temp chlorination refining process schema, with above-mentioned test conditions same materials, adopt the refinery coke reductive agent, temperature of reaction 1200-1300 ℃, 2.5 hours time, chlorine is blown into by reactor bottom nozzle 26, is adding air distribution plate 25 on the packing layer, what major product recovery system, waste gas drainage conduit connected pays the product recovery system up, obtains product purity average out to 98.2%.
Embodiment 3:
Carry out high-temp chlorination by Fig. 1 flow process and purify, adopt resistance furnace, the high 500mm of stove, wide 200mm, long 1000mm, the carbon content of packing into is 30 kilograms in carbon natural graphite and catalyst n a in 88%
2 CO
32 kilograms, mix in the stove of packing into simultaneously, electrode connects direct current (also available alternating-current), is resistance with natural graphite bulk cargo layer, the heating of energising back, when temperature is raised to 600 ℃, begin logical chlorine, promptly penetration mode is pressed into, 1200 ℃ of control chlorination temperatures, 2 hours time, the content of graphite average out to 99.67%-99.77% after the purification.Maximum is 99.83-99.89%.
Claims (14)
1; high-temp chlorination refining process for natural graphite; comprise stock grading; storing material; in Reaktionsofen, carry out high-temperature chlorination; remove impurity and obtain high-carbon or high purity graphite product; waste gas carries out purifying treatment; it is characterized in that under protection of inert gas, middle carbon natural graphite material being stored in the sealing feed bin; in Reaktionsofen, adopt chlorine and the infiltration of material bulk cargo layer or fluidization mode by carrying out high-temperature chlorination under catalyzer and/or the reductive agent effect; utilize negative pressure to reclaim major product again; according to the muriate condensing temperature difference of impurity, its impurity is chloride form reclaims simultaneously as paying product.
2, purifying technique according to claim 1 is characterized in that rare gas element is N
2Or CO.
3, purifying technique according to claim 1 is characterized in that Reaktionsofen carries out indirect heating with Sweet natural gas, coal gas or utilizes the resistance Reaktionsofen energising direct heating of graphite material bed of material resistance to produce high temperature.
4, purifying technique according to claim 1 is characterized in that the high-temp chlorination temperature is 1100-1700 ℃.
5, purifying technique according to claim 1 is characterized in that catalyzer is Na
2CO
3, K
2CO
3, NH
4F, H
3BO
3, B
2O
3, KClO
4, also above-mentioned catalyzer can be mixed use for any two kinds, its consumption is 5-10%.
6, purifying technique according to claim 1 is characterized in that reductive agent adopts the curing reductive agent that refinery coke, high grade activated carbon, hard coal are arranged, and its consumption is 5-10%, and gaseous reducing agent has CO, phosgene, fluorine Lyons.
7, purifying technique according to claim 1, when it is characterized in that the logical chlorine of high-temp chlorination carries out with penetration mode, its chlorine is infiltrated by graphite bed of material top, and waste gas is discharged by material layer lower part; When carrying out in the fluidization mode, its chlorine is blasted by the graphite material layer lower part, and waste gas is discharged by bed of material top.
8, purifying technique according to claim 1, it is characterized in that it is iron trichloride, aluminum chloride and silicon tetrachloride that impurity chlorides is paid product, it is 200-350 ℃ that its condensing temperature reclaims iron trichloride for first section, second section is reclaimed aluminum chloride is 150-178 ℃, and the 3rd section is reclaimed silicon tetrachloride is 55-60 ℃.
9, purifying technique according to claim 1 is characterized in that penetration mode or fluidization mode high-temperature chlorination adopt tubular Reaktionsofen, and penetration mode also can adopt the resistance Reaktionsofen.
10, the Reaktionsofen that purifying technique according to claim 1 adopted, it is characterized in that this Reaktionsofen is tubular Reaktionsofen, this stove is by body of heater, the burning gas nozzle, reactor, feed-pipe, discharge nozzle, inlet pipe, vapor pipe, air distribution plate and filler are formed, body of heater (37) is equipped with burning gas nozzle (5) on the two side, tubular reactor (4) is housed in the body of heater (37), air distribution plate (1) and packing layer (3) are equipped with down in reactor (4) bottom, the feed-pipe (11) that is connected with feed bin (12) is equipped with in reactor (4) top, with rotoclone collector (14), filter the major product discharge nozzle (13) that collector (15) is connected with vacuum pump, the inlet pipe that is connected with valve control system (10), reactor (a 4) bottom waste gas exhaust pipe (20) and a pair product withdrawing can (19,18,17) connect, remainder of exhaust gas is handled by purification system.
11, Reaktionsofen according to claim 10, it is characterized in that this Reaktionsofen is tubular Reaktionsofen, the inlet pipe of Reaktionsofen (10) also can be installed in reactor bottom, and at packing layer by adorning upper and lower air distribution plate (1,25), its waste gas exhaust pipe (20) is installed in the reactor top and is connected with a pair product recovery system.
12, Reaktionsofen according to claim 10, it is characterized in that this Reaktionsofen is the resistance Reaktionsofen, this Reaktionsofen is made up of body of heater, electrode bar, battery lead plate, air distribution plate, filler, air chamber, feed-pipe, inlet pipe, vapor pipe, discharge nozzle, cleaning eye, the inboard loading electrode rod (30) in body of heater (31) two ends, battery lead plate (32), upper and lower two air distribution plates (1,25) are equipped with in body of heater (31) bottom, the centre is packing layer (3), and a plurality of Cl are equipped with in the body of heater top
2With the Y-tube of CO inlet pipe (28,29) with feed-pipe (27) composition, below air chamber (33) has cleaning eye (35) and vapor pipe (34), vapor pipe (34) is connected with a pair product withdrawing can, on body of heater (31) sidewall of last air distribution plate (25) top, discharge nozzle (36) is housed, filters collector (15) by rotoclone collector (14) and be connected with vacuum pump.
13, according to claim 10,11,12 described Reaktionsofens, it is characterized in that tubular Reaktionsofen phosphoric acid salt, corundum material making, resistance furnace is made lining with graphite, phosphoric acid salt, corundum material, and filler adopts graphite or corundum material to be made as the spheroidal filler, and sphere diameter is 2-10mm.
14, according to claim 10,11,12 described Reaktionsofens, the cloth porosity that it is characterized in that the air distribution plate of Reaktionsofen is 7-10%, and the aperture is 0.1-1.0mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94105051A CN1040638C (en) | 1994-05-13 | 1994-05-13 | High-temp chlorination refining process for natural graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94105051A CN1040638C (en) | 1994-05-13 | 1994-05-13 | High-temp chlorination refining process for natural graphite |
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| Publication Number | Publication Date |
|---|---|
| CN1094695A CN1094695A (en) | 1994-11-09 |
| CN1040638C true CN1040638C (en) | 1998-11-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94105051A Expired - Fee Related CN1040638C (en) | 1994-05-13 | 1994-05-13 | High-temp chlorination refining process for natural graphite |
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Cited By (1)
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|---|---|---|---|---|
| WO2019134029A1 (en) * | 2018-01-05 | 2019-07-11 | Northern Graphite Corporation | System and method for producing high purity particulate graphite |
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| JP3764157B2 (en) * | 2003-10-10 | 2006-04-05 | 東洋炭素株式会社 | High-purity carbon-based material and ceramic film-coated high-purity carbon-based material |
| CN105460926B (en) * | 2015-12-30 | 2018-06-19 | 株洲弗拉德科技有限公司 | A kind of native graphite is without boat purifying process |
| CN106943966B (en) * | 2017-04-05 | 2020-03-17 | 攀钢集团研究院有限公司 | Experimental reaction system for preparing titanium dioxide by titanium tetrachloride gas phase oxidation |
| CN109502572A (en) * | 2018-12-29 | 2019-03-22 | 苏州第元素纳米技术有限公司 | Carbon nanotube method of purification |
| CN109553089A (en) * | 2018-12-29 | 2019-04-02 | 赛福纳米科技(徐州)有限公司 | Multi-purpose material heat treatment apparatus |
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| CN115140729A (en) * | 2022-07-18 | 2022-10-04 | 株洲弗拉德科技有限公司 | Preparation method of high-purity carbon material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052463A (en) * | 1990-11-30 | 1991-06-26 | 中国科学院西安光学精密机械研究所 | Graphite purification method |
| JPH1188413A (en) * | 1997-09-08 | 1999-03-30 | Hitachi Inf Syst Ltd | Electronic mail distributing system and storage medium used for the same |
-
1994
- 1994-05-13 CN CN94105051A patent/CN1040638C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052463A (en) * | 1990-11-30 | 1991-06-26 | 中国科学院西安光学精密机械研究所 | Graphite purification method |
| JPH1188413A (en) * | 1997-09-08 | 1999-03-30 | Hitachi Inf Syst Ltd | Electronic mail distributing system and storage medium used for the same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019134029A1 (en) * | 2018-01-05 | 2019-07-11 | Northern Graphite Corporation | System and method for producing high purity particulate graphite |
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| CN1094695A (en) | 1994-11-09 |
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