CN104495809A - Purification method of microcrystalline graphite - Google Patents
Purification method of microcrystalline graphite Download PDFInfo
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- CN104495809A CN104495809A CN201410727571.5A CN201410727571A CN104495809A CN 104495809 A CN104495809 A CN 104495809A CN 201410727571 A CN201410727571 A CN 201410727571A CN 104495809 A CN104495809 A CN 104495809A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000010439 graphite Substances 0.000 title claims abstract description 43
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000000746 purification Methods 0.000 title abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000003756 stirring Methods 0.000 claims abstract description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011259 mixed solution Substances 0.000 claims abstract description 35
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000001816 cooling Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 239000008139 complexing agent Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 30
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 24
- WQABCVAJNWAXTE-UHFFFAOYSA-N dimercaprol Chemical compound OCC(S)CS WQABCVAJNWAXTE-UHFFFAOYSA-N 0.000 claims description 24
- 239000013081 microcrystal Substances 0.000 claims description 16
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 12
- 230000018044 dehydration Effects 0.000 claims description 12
- 238000006297 dehydration reaction Methods 0.000 claims description 12
- 229960001051 dimercaprol Drugs 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003456 ion exchange resin Substances 0.000 claims description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002912 waste gas Substances 0.000 claims description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 239000011575 calcium Substances 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a purification method of microcrystalline graphite. The purification method of the microcrystalline graphite comprises the following steps: taking 450-500kg of graphite with carbon content of 70%-80%, sequentially adding sulfuric acid, hydrofluoric acid, nitric acid and hydrochloric acid, mixing and then adding 120-130L of pure water to dissolve, stirring, increasing the temperature of a reaction kettle to 86-90 DEG C and stirring to prepare a mixed solution A, putting the mixed solution A in a cooling tower, simultaneously injecting water and stirring to obtain a mixed solution B, putting the mixed solution B into a washer, simultaneously injecting water and washing, centrifugally dewatering until the content of water in the mixed solution B is 8%-10% to prepare a mixed solution C, putting the dewatered and mixed solution C into the reaction kettle, adding an oxidizing agent and a complexing agent, stirring to obtain a mixed solution D, feeding the mixed solution D to a drying device to dry at the temperature of 550-600 DEG C, wherein the content of water in the dried and mixed solution D is 0.05-0.09%, and the content of carbon in the dried and mixed solution D is 99.9993%-99.9996% to prepare the microcrystalline graphite. The purification method of the microcrystalline graphite is high in purity, simple in process and low in energy consumption.
Description
Technical field
The present invention relates to ceramic purification techniques field, more particularly, relate to a kind of micro crystal graphite purifying method.
Background technology
Graphite is a kind of high energy crystal carbon material, because of the feature such as the structure of its uniqueness and conduction, heat conduction, lubrication, high temperature resistant, stable chemical performance, make it in high performance material, have higher using value, be widely used in metallurgy, machinery, environmental protection, chemical industry, fire-resistant, the field such as electronics, medicine, military project and aerospace, become modern industry and height, the requisite non-metallic material of new, sharp technical development, the status in the national economic development is more and more important.
Along with the development of technology, common high-carbon graphite product can not meet the requirement of all trades and professions, therefore needs the purity improving graphite further.But the machining graphite state of the art of China is lower, product is main mainly with raw material and primary products, and the high impurity content of product makes its range of application limited.
Like this, domestic graphite products is cheap in international market price on the one hand, causes a large amount of graphite resource to outflow; High pure and ultra-fine graphite product then many dependence on import of domestic markets needs on the other hand, therefore, for high purity graphite, preparation technology studies, and has realistic meaning.
The silicate minerals of the impurity in graphite mainly potassium, sodium, magnesium, calcium, aluminium etc., the purifying technique of graphite, takes effective means to remove this part impurity exactly.At present, the method for domestic and international purification graphite mainly contains flotation process, alkali acid system, hydrogen fluoride, chlorinating roasting, pyroprocess etc.Wherein alkali acid system, hydrogen fluoride and chlorinating roasting belong to chemical purification, high temperature purification is owned by France in physical purification method, at present the resistant to elevated temperatures performance utilizing graphite is still to the method for purification that micro crystal graphite is taked, thus use high-temperature electric heat method to improve graphite purity, due to this complex process, need to build Large Electric Furnace, electric power resource waste is serious, need constantly to pass into rare gas element simultaneously, cause with high costs, be even more important a bit, be when graphite purity reaches 99.93%, reach capacity, the fixed carbon content of graphite cannot be made to continue to improve.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, provide a kind of micro crystal graphite purifying method, this method of purification purity is high, and technique is simple, and energy consumption is low.
Technical scheme of the present invention is:
A kind of micro crystal graphite purifying method, comprises the following steps:
Step 1, the graphite 450 ~ 500kg getting carbon content 70% ~ 80% put into reactor, adding weight percent is successively the sulfuric acid of 10% ~ 15%, hydrofluoric acid, the nitric acid of 0.2% ~ 0.32%, the hydrochloric acid of 20% ~ 24% of 20% ~ 25%, add 120 ~ 130L pure water after mixing to dissolve, stir;
Step 2, the temperature in reactor is risen to 86 ~ 90 DEG C, reaction 3 ~ 4h, once stir every 1h in reaction process, each churning time 4 ~ 6min, each stirring velocity is 400 ~ 500r/min, after reaction terminates, opens the exhaust relief valve on reactor, waste gas in reactor is discharged, obtained mixed liquor A;
Step 3, insert in cooling tower by mixed liquor A, inject the pure water that weight is mixed liquor A doubling dose in cooling tower, marginal not waterside is stirred, the temperature be stirred in cooling tower is only down to 12 ~ 18 DEG C, after completing cooling, open the baiting valve of cooling tower, obtain mixed liquid B;
Step 4, mixed liquid B is inserted washer after, the pure water that weight is mixed liquid B doubling dose is injected in washer, marginal not waterside is washed, washing speed is 200 ~ 300r/min, washing to the pH value of mixed liquid B be 6.4 ~ 6.9 to stop, after the washing speed of washer is adjusted to 800 ~ 1000r/min, carry out centrifuge dehydration, dewater to the water content of mixed liquid B be 8% ~ 10% only, obtained mixed solution C;
Step 5, again by dehydration after mixed solution C put into reactor, add oxygenant 20% ~ 25% and complexing agent 30% ~ 40%, then add pure water 80 ~ 100L, stir 30 ~ 40min, stirring velocity 400 ~ 500r/min, obtain mixed solution D;
Step 6, to be delivered on drying plant by mixed solution D and dry, bake out temperature is 550 ~ 600 DEG C, and the water content after oven dry is 0.05 ~ 0.09%, and carbon content is 99.9993% ~ 99.9996%, obtained product.
Further, in step 1, stirring velocity is 200 ~ 300r/min, and churning time is 20 ~ 30min.
Further, described pure water be through ion exchange resin treatment cross not containing Ca
2+, Mg
2+, CL
-, Si
2+the water of foreign ion.
Further, in steps of 5, sulfuric acid, concentration that described oxygenant is 92% ~ 93% by concentration be 94 ~ 95% nitric acid, concentration be 20% ~ 30% hydrochloric acid and concentration be that 42% ~ 50% hydrofluoric acid forms, the weight ratio of each material is sulfuric acid 31% ~ 40%: nitric acid 2% ~ 4%: hydrochloric acid 33% ~ 35%: hydrofluoric acid 25% ~ 33%;
Further, in steps of 5, described complexing agent is the composition of ethylenediamine tetraacetic acid (EDTA), Neutral ammonium fluoride and dimercaprol dimercaptopropanol, and the weight ratio of each material is ethylenediamine tetraacetic acid (EDTA) 31% ~ 34%: Neutral ammonium fluoride 32% ~ 35%: dimercaprol dimercaptopropanol 30% ~ 36%.
The invention has the beneficial effects as follows: micro crystal graphite purifying method purity provided by the invention is high, technique is simple, and energy consumption is low.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, to understand the present invention better.
Embodiment 1
A kind of micro crystal graphite purifying method, comprises the following steps:
Step 1, the graphite 500kg getting carbon content 70% put into reactor, and adding weight percent is successively the sulfuric acid of 10%, hydrofluoric acid, the nitric acid of 0.32%, the hydrochloric acid of 24% of 25%, add 130L pure water and dissolve, stir after mixing;
Step 2, the temperature in reactor is risen to 86 DEG C, reaction 3h, once stirs every 1h in reaction process, each churning time 4min, each stirring velocity is 400r/min, after reaction terminates, open the exhaust relief valve on reactor, the waste gas in reactor is discharged, obtained mixed liquor A;
Step 3, insert in cooling tower by mixed liquor A, inject the pure water that weight is mixed liquor A doubling dose in cooling tower, marginal not waterside is stirred, and the temperature be stirred in cooling tower is only down to 18 DEG C, after completing cooling, opens the baiting valve of cooling tower, obtains mixed liquid B;
Step 4, mixed liquid B is inserted washer after, the pure water that weight is mixed liquid B doubling dose is injected in washer, marginal not waterside is washed, washing speed is 200r/min, washing to the pH value of mixed liquid B be 6.4 to stop, after the washing speed of washer is adjusted to 1000r/min, carry out centrifuge dehydration, dewater to the water content of mixed liquid B be 10% only, obtained mixed solution C;
Step 5, again by dehydration after mixed solution C put into reactor, add oxygenant 20% and complexing agent 40%, then add pure water 100L, stir 40min, stirring velocity 400r/min, obtain mixed solution D;
Step 6, to be delivered on drying plant by mixed solution D and dry, bake out temperature is 600 DEG C, and the water content after oven dry is 0.09%, and carbon content is 99.9996%, obtained product.
In the present invention, in step 1, stirring velocity is 300r/min, and churning time is 30min.
In the present invention, described pure water be through ion exchange resin treatment cross not containing Ca
2+, Mg
2+, CL
-, Si
2+the water of foreign ion.
In the present invention, in steps of 5, sulfuric acid, concentration that described oxygenant is 92% by concentration be 95% nitric acid, concentration be 20% hydrochloric acid and concentration be that 50% hydrofluoric acid forms, the weight ratio of each material is sulfuric acid 31%: nitric acid 4%: hydrochloric acid 33%: hydrofluoric acid 33%;
In the present invention, in steps of 5, described complexing agent is the composition of ethylenediamine tetraacetic acid (EDTA), Neutral ammonium fluoride and dimercaprol dimercaptopropanol, and the weight ratio of each material is ethylenediamine tetraacetic acid (EDTA) 34%: Neutral ammonium fluoride 32%: dimercaprol dimercaptopropanol 36%.
Embodiment 2
A kind of micro crystal graphite purifying method, comprises the following steps:
Step 1, the graphite 450kg getting carbon content 80% put into reactor, and adding weight percent is successively the sulfuric acid of 15%, hydrofluoric acid, the nitric acid of 0.2%, the hydrochloric acid of 20% of 20%, add 120L pure water and dissolve, stir after mixing;
Step 2, the temperature in reactor is risen to 90 DEG C, reaction 4h, once stirs every 1h in reaction process, each churning time 6min, each stirring velocity is 500r/min, after reaction terminates, open the exhaust relief valve on reactor, the waste gas in reactor is discharged, obtained mixed liquor A;
Step 3, insert in cooling tower by mixed liquor A, inject the pure water that weight is mixed liquor A doubling dose in cooling tower, marginal not waterside is stirred, and the temperature be stirred in cooling tower is only down to 12 DEG C, after completing cooling, opens the baiting valve of cooling tower, obtains mixed liquid B;
Step 4, mixed liquid B is inserted washer after, the pure water that weight is mixed liquid B doubling dose is injected in washer, marginal not waterside is washed, washing speed is 300r/min, washing to the pH value of mixed liquid B be 6.9 to stop, after the washing speed of washer is adjusted to 800r/min, carry out centrifuge dehydration, dewater to the water content of mixed liquid B be 8% only, obtained mixed solution C;
Step 5, again by dehydration after mixed solution C put into reactor, add oxygenant 25% and complexing agent 30%, then add pure water 80L, stir 30min, stirring velocity 500r/min, obtain mixed solution D;
Step 6, to be delivered on drying plant by mixed solution D and dry, bake out temperature is 550 DEG C, and the water content after oven dry is 0.05%, and carbon content is 99.9993%, obtained product.
In the present invention, in step 1, stirring velocity is 200r/min, and churning time is 20min.
In the present invention, described pure water be through ion exchange resin treatment cross not containing Ca
2+, Mg
2+, CL
-, Si
2+the water of foreign ion.
In the present invention, in steps of 5, sulfuric acid, concentration that described oxygenant is 93% by concentration be 94% nitric acid, concentration be 30% hydrochloric acid and concentration be that 42% hydrofluoric acid forms, the weight ratio of each material is sulfuric acid 40%: nitric acid 2%: hydrochloric acid 35%: hydrofluoric acid 25%;
In the present invention, in steps of 5, described complexing agent is the composition of ethylenediamine tetraacetic acid (EDTA), Neutral ammonium fluoride and dimercaprol dimercaptopropanol, and the weight ratio of each material is ethylenediamine tetraacetic acid (EDTA) 31%: Neutral ammonium fluoride 35%: dimercaprol dimercaptopropanol 30%.
Embodiment 3
A kind of micro crystal graphite purifying method, comprises the following steps:
Step 1, the graphite 460kg getting carbon content 75% put into reactor, and adding weight percent is successively the sulfuric acid of 12%, hydrofluoric acid, the nitric acid of 0.3%, the hydrochloric acid of 21% of 23%, add 125L pure water and dissolve, stir after mixing;
Step 2, the temperature in reactor is risen to 88 DEG C, reaction 3.5h, once stir every 1h in reaction process, each churning time 5min, each stirring velocity is 440r/min, after reaction terminates, opens the exhaust relief valve on reactor, waste gas in reactor is discharged, obtained mixed liquor A;
Step 3, insert in cooling tower by mixed liquor A, inject the pure water that weight is mixed liquor A doubling dose in cooling tower, marginal not waterside is stirred, and the temperature be stirred in cooling tower is only down to 15 DEG C, after completing cooling, opens the baiting valve of cooling tower, obtains mixed liquid B;
Step 4, mixed liquid B is inserted washer after, the pure water that weight is mixed liquid B doubling dose is injected in washer, marginal not waterside is washed, washing speed is 230r/min, washing to the pH value of mixed liquid B be 6.5 to stop, after the washing speed of washer is adjusted to 900r/min, carry out centrifuge dehydration, dewater to the water content of mixed liquid B be 9% only, obtained mixed solution C;
Step 5, again by dehydration after mixed solution C put into reactor, add oxygenant 22% and complexing agent 33%, then add pure water 90L, stir 35min, stirring velocity 420r/min, obtain mixed solution D;
Step 6, to be delivered on drying plant by mixed solution D and dry, bake out temperature is 580 DEG C, and the water content after oven dry is 0.06%, and carbon content is 99.9994%, obtained product.
In the present invention, in step 1, stirring velocity is 250r/min, and churning time is 22min.
In the present invention, described pure water be through ion exchange resin treatment cross not containing Ca
2+, Mg
2+, CL
-, Si
2+the water of foreign ion.
In the present invention, in steps of 5, sulfuric acid, concentration that described oxygenant is 93% by concentration be 94% nitric acid, concentration be 25% hydrochloric acid and concentration be that 48% hydrofluoric acid forms, the weight ratio of each material is sulfuric acid 35%: nitric acid 3%: hydrochloric acid 34%: hydrofluoric acid 30%;
In the present invention, in steps of 5, described complexing agent is the composition of ethylenediamine tetraacetic acid (EDTA), Neutral ammonium fluoride and dimercaprol dimercaptopropanol, and the weight ratio of each material is ethylenediamine tetraacetic acid (EDTA) 33%: Neutral ammonium fluoride 33%: dimercaprol dimercaptopropanol 32%.
Embodiment 4
A kind of micro crystal graphite purifying method, comprises the following steps:
Step 1, the graphite 490kg getting carbon content 72% put into reactor, and adding weight percent is successively the sulfuric acid of 13%, hydrofluoric acid, the nitric acid of 0.31%, the hydrochloric acid of 22.5% of 24%, add 128L pure water and dissolve, stir after mixing;
Step 2, the temperature in reactor is risen to 87 DEG C, reaction 3.5h, once stir every 1h in reaction process, each churning time 4.5min, each stirring velocity is 470r/min, after reaction terminates, opens the exhaust relief valve on reactor, waste gas in reactor is discharged, obtained mixed liquor A;
Step 3, insert in cooling tower by mixed liquor A, inject the pure water that weight is mixed liquor A doubling dose in cooling tower, marginal not waterside is stirred, and the temperature be stirred in cooling tower is only down to 16 DEG C, after completing cooling, opens the baiting valve of cooling tower, obtains mixed liquid B;
Step 4, mixed liquid B is inserted washer after, the pure water that weight is mixed liquid B doubling dose is injected in washer, marginal not waterside is washed, washing speed is 270r/min, washing to the pH value of mixed liquid B be 6.7 to stop, after the washing speed of washer is adjusted to 880r/min, carry out centrifuge dehydration, dewater to the water content of mixed liquid B be 8.8% only, obtained mixed solution C;
Step 5, again by dehydration after mixed solution C put into reactor, add oxygenant 23% and complexing agent 35%, then add pure water 88L, stir 35min, stirring velocity 460r/min, obtain mixed solution D;
Step 6, to be delivered on drying plant by mixed solution D and dry, bake out temperature is 570 DEG C, and the water content after oven dry is 0.08%, and carbon content is 99.9995%, obtained product.
In the present invention, in step 1, stirring velocity is 280r/min, and churning time is 26min.
In the present invention, described pure water be through ion exchange resin treatment cross not containing Ca
2+, Mg
2+, CL
-, Si
2+the water of foreign ion.
In the present invention, in steps of 5, sulfuric acid, concentration that described oxygenant is 92.8% by concentration be 94.2% nitric acid, concentration be 22% hydrochloric acid and concentration be that 44% hydrofluoric acid forms, the weight ratio of each material is sulfuric acid 35%: nitric acid 2.5%: hydrochloric acid 33.8%: hydrofluoric acid 27%;
The present invention in, in steps of 5, described complexing agent is the composition of ethylenediamine tetraacetic acid (EDTA), Neutral ammonium fluoride and dimercaprol dimercaptopropanol, and the weight ratio of each material is ethylenediamine tetraacetic acid (EDTA) 32%: Neutral ammonium fluoride 34%: dimercaprol dimercaptopropanol 34%.
Adopt the micro crystal graphite purifying method that embodiment 1 ~ 4 provides, technique is simple, and energy consumption is low, easy handling, and production efficiency is high, and current consumption is low, does not need large-scale processing units, has greatly saved production cost, and purity is higher simultaneously.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (5)
1. a micro crystal graphite purifying method, comprises the following steps:
Step 1, the graphite 450 ~ 500kg getting carbon content 70% ~ 80% put into reactor, adding weight percent is successively the sulfuric acid of 10% ~ 15%, hydrofluoric acid, the nitric acid of 0.2% ~ 0.32%, the hydrochloric acid of 20% ~ 24% of 20% ~ 25%, add 120 ~ 130L pure water after mixing to dissolve, stir;
Step 2, the temperature in reactor is risen to 86 ~ 90 DEG C, reaction 3 ~ 4h, once stir every 1h in reaction process, each churning time 4 ~ 6min, each stirring velocity is 400 ~ 500r/min, after reaction terminates, opens the exhaust relief valve on reactor, waste gas in reactor is discharged, obtained mixed liquor A;
Step 3, insert in cooling tower by mixed liquor A, inject the pure water that weight is mixed liquor A doubling dose in cooling tower, marginal not waterside is stirred, the temperature be stirred in cooling tower is only down to 12 ~ 18 DEG C, after completing cooling, open the baiting valve of cooling tower, obtain mixed liquid B;
Step 4, mixed liquid B is inserted washer after, the pure water that weight is mixed liquid B doubling dose is injected in washer, marginal not waterside is washed, washing speed is 200 ~ 300r/min, washing to the pH value of mixed liquid B be 6.4 ~ 6.9 to stop, after the washing speed of washer is adjusted to 800 ~ 1000r/min, carry out centrifuge dehydration, dewater to the water content of mixed liquid B be 8% ~ 10% only, obtained mixed solution C;
Step 5, again by dehydration after mixed solution C put into reactor, add oxygenant 20% ~ 25% and complexing agent 30% ~ 40%, then add pure water 80 ~ 100L, stir 30 ~ 40min, stirring velocity 400 ~ 500r/min, obtain mixed solution D;
Step 6, to be delivered on drying plant by mixed solution D and dry, bake out temperature is 550 ~ 600 DEG C, and the water content after oven dry is 0.05 ~ 0.09%, and carbon content is 99.9993% ~ 99.9996%, obtained product.
2. micro crystal graphite purifying method according to claim 1, is characterized in that, in step 1, stirring velocity is 200 ~ 300r/min, and churning time is 20 ~ 30min.
3. micro crystal graphite purifying method according to claim 1, is characterized in that, described pure water be through ion exchange resin treatment cross not containing Ca
2+, Mg
2+, CL
-, Si
2+the water of foreign ion.
4. micro crystal graphite purifying method according to claim 1, it is characterized in that, in steps of 5, sulfuric acid, concentration that described oxygenant is 92% ~ 93% by concentration be 94 ~ 95% nitric acid, concentration be 20% ~ 30% hydrochloric acid and concentration be that 42% ~ 50% hydrofluoric acid forms, the weight ratio of each material is sulfuric acid 31% ~ 40%: nitric acid 2% ~ 4%: hydrochloric acid 33% ~ 35%: hydrofluoric acid 25% ~ 33%.
5. micro crystal graphite purifying method according to claim 1, it is characterized in that, in steps of 5, described complexing agent is the composition of ethylenediamine tetraacetic acid (EDTA), Neutral ammonium fluoride and dimercaprol dimercaptopropanol, and the weight ratio of each material is ethylenediamine tetraacetic acid (EDTA) 31% ~ 34%: Neutral ammonium fluoride 32% ~ 35%: dimercaprol dimercaptopropanol 30% ~ 36%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629704A (en) * | 2016-10-14 | 2017-05-10 | 成都理工大学 | Preparation technology of high-purity graphite covering agent for copper alloy melting |
| CN107337203A (en) * | 2017-08-31 | 2017-11-10 | 张旭 | The method for preparing high purity graphite |
| CN110395726A (en) * | 2019-09-04 | 2019-11-01 | 湖南有色金属研究院 | A kind of method of purification of micro crystal graphite mine |
| CN112047336A (en) * | 2020-10-19 | 2020-12-08 | 王振波 | Process for fluorine-free chemical purification of natural graphite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1919729A (en) * | 2006-09-11 | 2007-02-28 | 洛阳市冠奇工贸有限责任公司 | Ultra-high purity purifying technique for native graphite |
| CN102001649A (en) * | 2010-11-25 | 2011-04-06 | 洛阳市冠奇工贸有限责任公司 | Purification method for high-purity natural graphite |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919729A (en) * | 2006-09-11 | 2007-02-28 | 洛阳市冠奇工贸有限责任公司 | Ultra-high purity purifying technique for native graphite |
| CN102001649A (en) * | 2010-11-25 | 2011-04-06 | 洛阳市冠奇工贸有限责任公司 | Purification method for high-purity natural graphite |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629704A (en) * | 2016-10-14 | 2017-05-10 | 成都理工大学 | Preparation technology of high-purity graphite covering agent for copper alloy melting |
| CN107337203A (en) * | 2017-08-31 | 2017-11-10 | 张旭 | The method for preparing high purity graphite |
| CN107337203B (en) * | 2017-08-31 | 2020-09-01 | 鸡西市东北亚矿产资源有限公司 | Method for preparing high-purity graphite |
| CN110395726A (en) * | 2019-09-04 | 2019-11-01 | 湖南有色金属研究院 | A kind of method of purification of micro crystal graphite mine |
| CN112047336A (en) * | 2020-10-19 | 2020-12-08 | 王振波 | Process for fluorine-free chemical purification of natural graphite |
| CN112047336B (en) * | 2020-10-19 | 2022-06-10 | 王振波 | Process for fluorine-free chemical purification of natural graphite |
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| Publication number | Publication date |
|---|---|
| CN104495809B (en) | 2017-12-19 |
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