CN102502601B - Continuously-expandable graphite production device - Google Patents
Continuously-expandable graphite production device Download PDFInfo
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- CN102502601B CN102502601B CN2011103314596A CN201110331459A CN102502601B CN 102502601 B CN102502601 B CN 102502601B CN 2011103314596 A CN2011103314596 A CN 2011103314596A CN 201110331459 A CN201110331459 A CN 201110331459A CN 102502601 B CN102502601 B CN 102502601B
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- relay tank
- communicated
- jet pipe
- belt vacuum
- black lead
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 27
- 229910002804 graphite Inorganic materials 0.000 title abstract description 27
- 239000010439 graphite Substances 0.000 title abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000002351 wastewater Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N HF Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000003929 acidic solution Substances 0.000 claims description 4
- 230000001105 regulatory Effects 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000000746 purification Methods 0.000 abstract description 5
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- 230000003247 decreasing Effects 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- 230000002035 prolonged Effects 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 238000011010 flushing procedure Methods 0.000 description 7
- 229910021382 natural graphite Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000015450 Tilia cordata Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000011218 segmentation Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L Iron(II) chloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 239000004698 Polyethylene (PE) Substances 0.000 description 1
- 210000003491 Skin Anatomy 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000001143 conditioned Effects 0.000 description 1
- 230000001808 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000001264 neutralization Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001590 oxidative Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- -1 poly ethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000630 rising Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
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Abstract
A continuously-expandable graphite production device comprises a reaction kettle. A blanking groove is disposed below the reaction kettle, and a jet pipe is arranged below the blanking groove. One end of the jet pipe is connected with an air compressor, the other end of the jet pipe is communicated with a first relay tank, and the blanking groove is communicated with the jet pipe through a siphon. A discharging port of the first relay tank is communicated with a feeding port of a first belt-type vacuum filtering dehydrating device. The continuously-expandable graphite production device adopts the special relay tank to immerse and wash reacted materials, thereby being easy to control concentration of acid liquor for immersion. The continuously-expandable graphite production device adopts the belt-type vacuum filtering dehydrating device to conduct sub-sectioned deacidification dehydration processing for the immersed materials, waste acid is recycled, waste water enters a sewage treatment pond, and the whole device is capable of achieving automatic and continuous production. In addition, in terms of follow-up purification work, a production line can be prolonged so that continuous production of graphite acidization and graphite purification can be achieved. The continuously-expandable graphite production device has the advantages of being controllable in concentration of reacted waste acid, controllable in reaction temperature and high in automation degree, greatly reducing water consumption for washing, decreasing emission and improving production efficiency.
Description
Technical field
The present invention relates to the Preparation of Expansible Graphite field, particularly a kind of continuous expansible black lead production equipment.
Background technology
Graphite is as a kind of non-metallic material, and having very widely in a plurality of fields, utilization, particularly its exclusive characteristic have the irreplaceable effect of other materials in fields such as sealing and heat conduction and heat radiations.
Natural graphite is carried out high temperature to expand and just must carry out the material intercalation processing to its sheet interlayer and obtain expansible black lead.Current now way is: to carrying out the acid ion intercalation processing between sky combustion graphite flake layer, acid ion is fully injected between the graphite flake layer in the environment of strong oxidizing property.Natural graphite behind the acid ion intercalation often is called acidifying graphite, just expansible black lead.The acid ion of expansible black lead (700 ~ 1200 ℃) sheet interlayer when high temperature can fiercely gasify, the bulging force that produces can draw back the interlamellar spacing of natural graphite, make fierce expansion of volume of expansible black lead, before all volumes after the expansion can reach and expand 100 ~ 350 times of acidifying graphite volume, have in addition can reach more than 500 times.Graphite quality after the expansion is bulk, and natural graphite is elongated to strip, because of its shape like worm, expanded graphite often is called as graphite worm.Can carry out post-production to expanded graphite, such as adopting roll compacting or compression molding to make various products, be widely used in fields such as sealing and heat conduction and heat radiation.
And prepare in the whole bag of tricks of expansible black lead carrying out acidification for natural stone, adopt the vitriol oil under strong well-oxygenated environment, allow sulfate ion (HSO
4 -) to insert the unilateral method of natural graphite the most extensive, and adopt this method cost the most economical, to the pollution level minimum that environment causes, the processing condition of this method are the most ripe simultaneously.
In process of production, crystalline flake graphite and acid and oxygenant carry out in the reactor that band stirs, the reaction product of thickness adopts the flushing of high speed flowing water to enter flushing tank, high speed flow water generates siphonage is transported to flushing tank with reaction product, washing is to neutral in flushing tank, through centrifuge dehydration, drying obtains expansible black lead then.There is following defective in this technology: 1, owing to adopt the flushing of high speed flowing water, it is on the low side to wash residual acid concentration, and no recovery value pollutes environment; 2, temperature of charge is not easy control in the flushing process, causes unstable product quality; 3, will use a large amount of bath wateies, and waste water and cause huge environmental stress.
Summary of the invention
Technical problem to be solved by this invention provides a kind of continuous expansible black lead production equipment, be easy to control and soak acid strength, be convenient to carry out segmentation depickling dehydration to soaking product, waste acid recycling, waste water enters treatment tank, complete assembly can be realized automatization, serialization production, and can lengthen production line in follow-up purification operation, and realization graphite purifying, graphite acidifying are produced continuously.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of continuous expansible black lead production equipment, comprise reactor, and reactor has blanking groove, and the blanking groove below is provided with jet pipe;
Jet pipe one end is connected with air compressor machine, and the other end is communicated with first relay tank, and blanking groove is communicated with jet pipe by siphon pipe;
The first relay tank discharge port is communicated with the opening for feed of first belt vacuum filter.
The discharge port of described first belt vacuum filter is communicated with second relay tank, and the discharge port of second relay tank is communicated with the opening for feed of second belt vacuum filter.
Be provided with hydrofluoric acid solution in described second relay tank.
Described first relay tank and second relay tank also are provided with spiral coil cooling tube.
Material moisture after described first belt vacuum filter and second belt vacuum filter are handled is lower than 30%.
First belt vacuum filter and second belt vacuum filter are the Pyatyi treating processes, and the first step is the suction acidic solution, and level Four is drip washing in addition.
The air pressure that described air compressor machine produces is 0.3-1MPa.
A kind of continuous expansible black lead production equipment provided by the invention, adopt special relay tank washing by soaking reaction mass, thereby be easy to control and soak acid strength, adopt vacuum to take off filter and carry out segmentation depickling dehydration to soaking material, waste acid recycling, waste water enters treatment tank, and complete assembly can be realized automatization, serialization production, and can lengthen production line in follow-up purification operation, realization graphite purifying, graphite acidifying are produced continuously.Beneficial effect of the present invention is: the reaction acid-spending strength is controlled; Temperature of reaction is controlled; The bath water amount significantly reduces, and reduces discharging; The level of automation height has improved production efficiency.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples:
Fig. 1 is overall schematic of the present invention.
Embodiment
As shown in fig. 1, a kind of continuous expansible black lead production equipment comprises reactor 1, and reactor 1 has blanking groove 2, and blanking groove 2 belows are provided with jet pipe 3;
Jet pipe 3 one ends are connected with air compressor machine 5, and the other end is communicated with first relay tank 6, and blanking groove 2 is communicated with jet pipe 3 by siphon pipe 4;
First relay tank, 6 discharge ports are communicated with the opening for feed of first belt vacuum filter 8.Vacuum is taken off filter and is adopted the belt vacuum to take off filter.
The discharge port of described first belt vacuum filter 8 is communicated with second relay tank 9, and the discharge port of second relay tank 9 is communicated with the opening for feed of second belt vacuum filter 10.
Be provided with hydrofluoric acid solution in described second relay tank 9.Usually adopt the hydrofluoric acid solution of volumetric molar concentration 30-55% to handle.
Described first relay tank 6 and second relay tank 9 also are provided with spiral coil cooling tube 7.Spiral coil cooling tube 7 is used for logical water coolant or hot water, with the control temperature.
Material moisture after described first belt vacuum filter 8 and second belt vacuum filter 10 are handled is lower than 30%.
First belt vacuum filter 8 and second belt vacuum filter 10 are the Pyatyi treating processes, and the first step is the suction acidic solution, and level Four is drip washing in addition.
The air pressure that described air compressor machine 5 produces is 0.3-1MPa.
Adopt air-flow siphonage transfer of highly viscous acidifying graphite material among the present invention, acidifying graphite material soaks dilution through first relay tank 6, relay tank adopts the modified poly ethylene can, assembling spiral coil cooling tube 7 can feed cold water or hot water in jar, control flushing temperature, take off the filter washing through the belt vacuum after the material cooling, collect spent acid waste water and handle respectively, the expansible black lead after the washing or further carry out the back purification processes, or convection drying obtains the expansible black lead finished product.
In apparatus of the present invention, high pressure draft siphoning installation, relay tank, belt vacuum are taken off filter and are used the core that constitutes this device, and its function of the combination of these devices is supported mutually, thereby the automated job of realization acidifying graphite material has improved production efficiency.
Specifically, adopt device of the present invention to operate as follows:
1, crystalline flake graphite, sulfuric acid, oxygenant are measured stirring reaction in the proportioning reactor 1 by certain chemistry, the proportioning between the various materials is prior art;
2, after reaction was finished, upset reactor 1 was poured reacted sticky shape material into blanking groove 2, blanking groove 2 has certain tilt internal wall, material utilizes the gravity trickling, and at tip designs one siphon pipe 4 of blanking groove, siphon pipe 4 is connected with jet pipe 3 negative pressure end interfaces;
3, jet pipe 3 main pipe lines and mass transport pipe coupling are introduced first relay tank 6 with tail wind, and material is stirred cooling;
4, during blanking, start air compressor machine 5, blast reach 0.3-1MPa, the employing 0.3-0.5 MPa of optimization in the jet pipe 3.By the control blast, can adjust blanking velocity.Because material is vitriol oil mixture, material flows in first relay tank 6, first relay tank, 6 splendid attire washing water, vitriol oil mixture mixes with water will produce a large amount of heat, if blanking is too fast, temperature will raise, the rising temperature causes disadvantageous effect to expansible black lead quality stability, therefore, utilize the negative pressure adjustability, control temperature in first relay tank 6 thereby can control blanking velocity;
5, material flows into transfer lime in blanking groove 2 under little suction function and self gravitation effect that jet pipe 3 forms, and transfer lime has certain inclination, and material will utilize self gravitation to trickle naturally along smooth transfer lime, enter first relay tank 6.
6, design has stirring rake and spiral coil cooling tube 7 in first relay tank 6; spiral coil cooling tube 7 coils along first relay tank, 6 tank skins; introduce cooling circulating water in the spiral coil cooling tube; regulate the relay tank temperature on the one hand; in addition; relay tank is plastic cement products, introduces water coolant, is beneficial to protection first relay tank 6 tank wall materials.
7, material washs in first relay tank 6, adjusts first relay tank, 6 water yields, control acidity;
8, treat that temperature is down to 35 ± 5 ℃ in first relay tank 6, the baiting valve of first relay tank 6 opened that material flows to first belt vacuum filter 8 and carries out the depickling carrying out washing treatment according to certain flow;
9,8 fens Pyatyi washing process of first belt vacuum filter, one-level is mainly aspirated than concentrated acid water, and concentrated acid water carries out the purifying treatment reuse; Level Four is drip washing in addition, collects waste water and unifies to handle recycling;
10, the material moisture of handling through first belt vacuum filter 8 is controlled in 30%, and this mainly realizes by rotating speed and the vacuum tightness of controlling first belt vacuum filter 8.
11, after the material collection, can carry out next step operation, if the crystalline flake graphite raw material is high-carbon graphite, by truck 11 or directly enter the oven dry operation; If crystalline flake graphite is medium-carbon graphite, perhaps need to be further purified processing, material will enter second relay tank 9, add hydrofluoric acid treatment;
12, same design spiral coil cooling tube 7 in second relay tank 9 is introduced hot water or cold water, with the conditioned reaction temperature in the spiral coil cooling tube 7;
13, after reaction was finished, temperature was down to 35 ± 5 ℃ in second relay tank 9, and second relay tank, 9 baiting valves are opened, and material flows to second belt vacuum filter 10 and carries out the depickling carrying out washing treatment according to certain flow;
14,10 fens Pyatyi washing process of second belt vacuum filter, one-level is mainly aspirated than concentrated acid water, and concentrated acid water carries out the purifying treatment reuse; Level Four is drip washing in addition, collects waste water and unifies to handle recycling;
15, the material moisture of handling through second belt vacuum filter 10 is controlled in 30%, and this major control belt vacuum is taken off filter rotating speed and vacuum tightness.Material can carry out next step operation after collecting with truck 11.
Claims (7)
1. a continuous expansible black lead production equipment comprises reactor (1), it is characterized in that: reactor (1) has blanking groove (2), and blanking groove (2) below is provided with jet pipe (3);
Jet pipe (3) one ends are connected with the air compressor machine (5) that is used for control blast, adjusting blanking velocity, and the other end is communicated with first relay tank (6), and blanking groove (2) is communicated with jet pipe (3) by siphon pipe (4);
Described first relay tank (6) also is provided with for the spiral coil cooling tube (7) of regulating temperature;
First relay tank (6) discharge port is communicated with the opening for feed that the first belt vacuum is taken off filter (8),
First belt vacuum filter (8) is the Pyatyi treating processes, and the first step is the suction acidic solution, and concentrated acid water carries out the purifying treatment reuse; Level Four is drip washing in addition, collects waste water and unifies to handle recycling;
Material moisture after first belt vacuum filter (8) is handled is lower than 30%.
2. a kind of continuous expansible black lead production equipment according to claim 1, it is characterized in that: the discharge port of described first belt vacuum filter (8) is communicated with second relay tank (9), and the discharge port of second relay tank (9) is communicated with the opening for feed of second belt vacuum filter (10).
3. a kind of continuous expansible black lead production equipment according to claim 2 is characterized in that: be provided with hydrofluoric acid solution in described second relay tank (9).
4. according to claim 2 or 3 described a kind of continuous expansible black lead production equipments, it is characterized in that: described second relay tank (9) also is provided with spiral coil cooling tube (7).
5. a kind of continuous expansible black lead production equipment according to claim 4 is characterized in that: the material moisture after described second belt vacuum filter (10) is handled is lower than 30%.
6. a kind of continuous expansible black lead production equipment according to claim 5 is characterized in that: second belt vacuum filter (10) is the Pyatyi treating processes, and the first step is the suction acidic solution, and level Four is drip washing in addition.
7. a kind of continuous expansible black lead production equipment according to claim 1 is characterized in that: the air pressure that described air compressor machine (5) produces is 0.3-1MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103314596A CN102502601B (en) | 2011-10-27 | 2011-10-27 | Continuously-expandable graphite production device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103314596A CN102502601B (en) | 2011-10-27 | 2011-10-27 | Continuously-expandable graphite production device |
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| Publication Number | Publication Date |
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| CN102502601A CN102502601A (en) | 2012-06-20 |
| CN102502601B true CN102502601B (en) | 2013-07-17 |
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| CN2011103314596A Active CN102502601B (en) | 2011-10-27 | 2011-10-27 | Continuously-expandable graphite production device |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108203092A (en) * | 2018-02-06 | 2018-06-26 | 青岛晶莹石墨有限公司 | Graphite powder impurity removal process and sewage treatment process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201276423Y (en) * | 2008-10-17 | 2009-07-22 | 任崇桂 | Microwave continuous graphite swelling apparatus |
| CN202279696U (en) * | 2011-10-27 | 2012-06-20 | 中科恒达石墨股份有限公司 | Continuous expansible graphite production device |
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2011
- 2011-10-27 CN CN2011103314596A patent/CN102502601B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201276423Y (en) * | 2008-10-17 | 2009-07-22 | 任崇桂 | Microwave continuous graphite swelling apparatus |
| CN202279696U (en) * | 2011-10-27 | 2012-06-20 | 中科恒达石墨股份有限公司 | Continuous expansible graphite production device |
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| CN102502601A (en) | 2012-06-20 |
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Effective date of registration: 20170110 Address after: 443100 Hubei city of Yichang Province Branch Road, Yiling District of Yiling Economic Development Zone No. 1 Patentee after: Hubei liantou Hengda graphite Co. Ltd. Address before: 443100 East Lake Road, Yiling District, Hubei, No. four, No. Patentee before: China Sciences Hengda Graphite Co., Ltd. |