CN101973545A - Method for purifying high-purity graphite - Google Patents
Method for purifying high-purity graphite Download PDFInfo
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Abstract
The invention discloses a method for purifying high-purity graphite, which aims to effectively remove impurities from the graphite and make 99.99 percent the fixed carbon content of the graphite. The method comprises the following steps of: performing the steps of crushing, ball-milling, sieving and the like on raw graphite ore and performing ore-dressing on the treated graphite ore by adopting floatation equipment or gravity dressing equipment to obtain graphite concentrate; performing alkali leaching on the graphite concentrate in a pressurized reaction kettle and then performing normal-pressure acid leaching in an ultrasonic wave field or a microwave field; and leaching treated graphite powder by using a hydrofluoric acid or fluoride salt-containing sodium fluoride to obtain the high-purity graphite product.
Description
Technical field
The present invention relates to a kind of method of the high purity graphite of purifying, particularly by the method for graphite raw ore purification purity greater than 99.99% high purity graphite.
Background technology
High purity graphite be content of graphite at the graphite more than 99.99%, it is a kind of non-renewable strategic resource, is important war preparedness resource indispensable in military project and modern crafts and the hi-tech development always.
At present the production method of high purity graphite is mainly based on the wet-process purification method of flotation process, acid-base method, hydrofluoric acid method with based on the pyrogenic process method of purification of chlorinating roasting and pyroprocess.Deficiency such as these several production methods exist more or less that impurity-eliminating effect is poor, energy consumption height, environmental pollution are serious.
Summary of the invention
The invention provides a kind of method of the high purity graphite of purifying, can effectively remove the impurity in the graphite, make the content of the fixed carbon of graphite reach 99.99%, reach the method for high purity graphite requirement.The better performances of product, its technology is simple, advanced, easy handling, and the production efficiency height, facility investment is few, energy consumption is low, and smaller to the influence of environment, cost is low, and graphite products purity height can satisfy the requirement of high purity graphite.
Solving the technical scheme that technical problem of the present invention adopts is: the graphite raw ore through operations such as fragmentation, ball milling, screenings after, adopt floatation equipment or gravitational separation equipment that it is carried out the ore dressing processing, obtain the graphite concentrate.The graphite concentrate carries out alkali earlier and soaks processing in the compressive reaction still, then carry out the normal pressure acidleach and handle in ultrasonic wave field or microwave field.The system that last graphite adopts hydrofluoric acid or contains villiaumite is carried out deep impurity-removing, obtains highly purified graphite products; The leaching waste liquid of reacted each section is through recycling back recycle.Technical characterictic is as follows:
A kind of method of the high purity graphite of purifying, with the graphite raw ore is raw material, raw material is crystalline flake graphite or cryptocrystalline graphite, be characterised in that: after the fragmentation for several times of graphite raw ore process crusher, drop in the ball mill and grind, obtain the following graphite powder of 50 orders, the graphite material after pulverizing is dropped in the sieve apparatus carry out the powdered graphite classification, obtaining granularity is 100～1000 purpose graphite powders; Underproof Graphite Powder 99 is then put into again and is carried out ball milling repeatedly in the ball mill; Adopt floatation equipment or gravitational separation equipment that the graphite powder is carried out the ore dressing processing and obtain the graphite concentrate; Successively adopt pressurization alkali to soak with the normal pressure acidleach graphite concentrate is handled, wherein the normal pressure acidleach is at ultrasonic wave field or/and carry out under the microwave field; Graphite Powder 99 after the processing obtains highly purified graphite products again with hydrofluoric acid or contain the villiaumite Sodium Fluoride and leach.
Described flotation temperature is 20～60 ℃, and the weight liquid-solid ratio of flotation is 1～20: 1.
The solution that described pressurization alkali soaks is LiOH, NaOH, KOH, Na
2CO
3Or any one or a few mixing of ammonia aqueous solution; LiOH concentration is 5%～40%, and NaOH concentration is 5%～35%, and KOH concentration is 5%～27%, Na
2CO
3Concentration is 5%～30%; The weight liquid-solid ratio that pressurization alkali soaks is 1～10: 1, and temperature is 100～300 ℃, and reaction pressure is 0.3～30.0MPa, and the treatment time is 0.5～12 hour; Adopt lime as reagent reclaiming alkali lye.
The solution that described normal pressure acidleach is adopted is any one or a few mixing of hydrochloric acid, sulfuric acid, nitric acid or aqueous acetic acid; Concentration of hydrochloric acid is 5%～35%, and sulfuric acid concentration is 5%～80%, and concentration of nitric acid is 5%～60%, and acetate concentration is 5%～100%; The weight liquid-solid ratio of normal pressure acidleach is 1～8: 1, and temperature is 30～90 ℃, and the treatment time is 1h～100h.Ultrasonic frequency scope during the normal pressure acidleach is at 15～80KHz, and the microwave field range of frequency is at 300GHz～3GHz.
The concentration of described hydrofluoric acid: 1%～45%, the concentration that contains villiaumite Sodium Fluoride NaF is 1～20%; The weight liquid-solid ratio 1～9: 1 that hydrofluoric acid or Sodium Fluoride are handled, temperature is 40～90 ℃, the treatment time is 1h～24h.
Above-mentioned pressurization alkali soaks: the graphite concentrate after the ore dressing drops in the compressive reaction still, adds alkaline solution, and the control reaction conditions reacts impurity and alkali lye in the graphite concentrate.After reaction finishes, realize solid-liquid separation.Solid adopts pure water to wash till the pH=7, and liquid adopts lime to carry out alkali liquid regeneration.
Above-mentioned normal pressure acidleach: wash to mix with the acid solution of above-mentioned condition to neutral graphite and size mixing, the control reaction conditions further reacts the impurity in the graphite with acid.Reaction process is carried out in ultrasonic wave field or microwave field.Reacted graphite adopts hydrofluoric acid at last or contains the villiaumite Sodium Fluoride and carries out deep impurity-removing, to remove the silicic acid that acidic conditions generates down.The spent acid that produces in the acidleach process adopts the mode of ion exchange resin or extraction to carry out acid solution regeneration.
The acid waste water and the alkaline waste water that produce in the washing process neutralize mutually, and add the F in the lime precipitation solution.Water after neutralization retrieval system again washs.Whole technological process is free from environmental pollution.
The invention has the beneficial effects as follows: the graphite raw ore through flotation or gravity treatment, pressurization alkali soak, acidleach obtains high purity graphite after handling, and add ultrasonic wave field or microwave field in the acidleach process.Technical process is short, realizes suitability for industrialized production easily, and equipment is simple, and security is good, and energy consumption is low, and production cost is low, and environmental pollution is little; The content of fixed carbon is greater than 99.99% in the high purity graphite that obtains.
Embodiment
Below by embodiment the present invention is described in further detail.
Embodiment one
Use the crystalline flake graphite of carbon content 10wt% to be raw material, raw material is advanced crusher in crushing, ball mill ball milling successively, and adopt sieve apparatus that Graphite Powder 99 is sieved powder, obtaining granularity is 150 purpose graphite powders, adopt floatation equipment that it is carried out preliminary removal of impurities then, obtain the graphite concentrate.
With concentration is that 5% NaOH solution is that 1: 1 weight part carries out alkali to the graphite concentrate and soaks processing according to liquid-solid ratio in the compressive reaction still, and control reaction temperature is 110～130 ℃, and reaction pressure is 25MPa, and the treatment time is 12h.Reacted material is realized solid-liquid separation, and cleans to pH=7 with pure water.Be 10% hydrochloric acid soln again with reacted material concentration according to liquid-solid ratio be that 8: 1 weight part carries out acidleach and goes out to handle, the control reaction conditions is that normal pressure, temperature of reaction are 90 ℃, and the treatment time is 50h; Add microwave field in the acidleach process, microwave frequency is 3GHz.It is that 20% hydrofluoric acid solution carries out deep impurity-removing and leaches and handle that reacted Graphite Powder 99 filters the last concentration that adopts in back, the weight part liquid-solid ratio of hydrofluoric acid treatment is 5: 1, temperature is 60 ℃, treatment time is 5h, product after the processing adopts routine techniques to obtain highly purified graphite products through washing to neutral after drying, its purity is 99.991%, and the product total percent of ash is 0.009%.Al wherein
2O
3Residual volume be 18ppmw, Fe
2O
3Residual volume be 14ppmw, SiO
2Residual volume be 23ppmw, other total impurities is less than 15ppmw.
More than the various waste liquids that produce of every reaction back through the recycling recycles, the waste liquid that alkali soaks after the processing adopts lime to carry out alkali liquid regeneration, the waste liquid after acidleach is handled adopts extraction or ion exchange resin to carry out acid solution regeneration.
Embodiment two
Use the crystalline flake graphite of carbon content 15wt% to be raw material, raw material is advanced crusher in crushing, ball mill ball milling successively, and adopt sieve apparatus that Graphite Powder 99 is sieved powder, obtaining granularity is 250 purpose graphite powders, adopt gravitational separation equipment that it is carried out preliminary removal of impurities then, obtain the graphite concentrate.
With concentration is 30% KOH and 20% Na
2CO
3Mixing solutions is that 5: 1 weight part carries out alkali to the graphite concentrate and soaks processing according to liquid-solid ratio in the compressive reaction still, and control reaction temperature is 180～200 ℃, and reaction pressure is 15MPa, and the treatment time is 6h.Reacted material is realized solid-liquid separation, and uses pure water to clean to pH=7.Be 15% salpeter solution again with reacted material concentration according to liquid-solid ratio be that 1: 1 weight part carries out acidleach and goes out to handle, the control reaction conditions is that normal pressure, temperature of reaction are 50 ℃, treatment time is 20h, adds ultrasonic wave field in the acidleach process, and ultrasonic frequency is 17KHz.It is that 10% hydrofluoric acid solution carries out deep impurity-removing and leaches and handle that reacted Graphite Powder 99 filters the last concentration that adopts in back, the weight part liquid-solid ratio of hydrofluoric acid treatment is 2: 1, temperature is 40 ℃, treatment time is 7h, product after the processing adopts routine techniques to obtain highly purified graphite products through washing to neutral after drying, its purity is 99.995%, and the product total percent of ash is 0.005%, wherein Al
2O
3Residual volume be 10ppmw, Fe
2O
3Residual volume be 7ppmw, SiO
2Residual volume be 11ppmw, other total impurities is less than 5ppmw.
Embodiment three
Use the cryptocrystalline graphite of carbon content 30wt% to be raw material.Raw material is advanced crusher in crushing, ball mill ball milling successively, and adopt sieve apparatus that Graphite Powder 99 is sieved powder, obtaining granularity is 350 purpose graphite powders, adopts gravitational separation equipment that it is carried out preliminary removal of impurities then, obtains the graphite concentrate.
With concentration is that the KOH mixing solutions of 25% LiOH and 5% is that 8: 1 weight part carries out alkali to the graphite concentrate and soaks processing according to liquid-solid ratio in the compressive reaction still, and control reaction temperature is 250～280 ℃, and reaction pressure is 20MPa, and the treatment time is 4h.Reacted material is realized solid-liquid separation, and uses pure water to clean to pH=7.Be the sulfuric acid of 20% hydrochloric acid soln and 15% and 30% acetic acid mixing solutions again with reacted material concentration according to liquid-solid ratio be that 4: 1 weight part carries out the normal pressure acidleach and handles, control reaction temperature is 60 ℃, and the treatment time is 80h.Successively add microwave field and ultrasonic wave field in the acidleach process, microwave frequency is 50GHz, and frequency of ultrasonic is 50KHz, and the time respectively is 40 hours.Reacted Graphite Powder 99 filters the back, and last to adopt concentration be 10% Sodium Fluoride NaF solution according to liquid-solid ratio is that 4: 1 weight part leaches processing, product after the processing adopts routine techniques to obtain highly purified graphite products through washing to neutral after drying, its purity is 99.993%, and the product total percent of ash is 0.007%.Al wherein
2O
3Residual volume be 12ppmw, Fe
2O
3Residual volume be 14ppmw, SiO
2Residual volume be 23ppmw, other total impurities is less than 11ppmw.
Claims (7)
1. the method for the high purity graphite of purifying is a raw material with the graphite raw ore, it is characterized in that: after the fragmentation of graphite raw ore process, ball milling and the screening, obtaining granularity is 100～1000 purpose graphite powders; Adopt floatation equipment or gravitational separation equipment that the graphite powder is carried out the ore dressing processing and obtain the graphite concentrate; Successively adopt pressurization alkali to soak with the normal pressure acidleach graphite concentrate is handled, wherein the normal pressure acidleach is at ultrasonic wave field or/and carry out under the microwave field; Graphite Powder 99 after the processing obtains highly purified graphite products again with hydrofluoric acid or contain the villiaumite Sodium Fluoride and leach.
2. the method for purification high purity graphite according to claim 1, temperature is 20～60 ℃ when being primarily characterized in that flotation, the weight liquid-solid ratio of flotation is 1～20: 1.
3. the method for purification high purity graphite according to claim 1, the solution that the alkali that it is characterized in that pressurizeing soaks is LiOH, NaOH, KOH, Na
2CO
3Or any one or a few mixing of ammonia aqueous solution; LiOH concentration is 5%～40%, and NaOH concentration is 5%～35%, and KOH concentration is 5%～27%, Na
2CO
3Concentration is 5%～30%; The weight liquid-solid ratio that pressurization alkali soaks is 1～10: 1, and temperature is 100～300 ℃, and reaction pressure is 0.3～30.0MPa, and the treatment time is 0.5～12 hour; Adopt lime as reagent reclaiming alkali lye.
4. the method for purification high purity graphite according to claim 1, the solution that it is characterized in that the normal pressure acidleach are any one or a few mixing of hydrochloric acid, sulfuric acid, nitric acid or aqueous acetic acid; Concentration of hydrochloric acid is 5%～35%, and sulfuric acid concentration is 5%～80%, and concentration of nitric acid is 5%～60%, and acetate concentration is 5%～100%; The weight liquid-solid ratio of normal pressure acidleach is 1～8: 1, and temperature is 30～90 ℃, and the treatment time is 1h～100h.
5. the method for purification high purity graphite according to claim 1 is characterized in that the concentration of hydrofluoric acid: 1%～45%, and the concentration that contains villiaumite Sodium Fluoride NaF is 1～20%; The weight liquid-solid ratio 1～9: 1 that hydrofluoric acid or Sodium Fluoride are handled, temperature is 40～90 ℃, the treatment time is 1h～24h.
6. the method for purification high purity graphite according to claim 1 is characterized in that: described raw material is crystalline flake graphite or cryptocrystalline graphite.
7. the method for purification high purity graphite according to claim 1, the ultrasonic frequency scope when it is characterized in that the normal pressure acidleach is at 15～80KHz, and the microwave field range of frequency is at 300GHz～3GHz.
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