CN101654244A - Method for preparing high-purity graphite from high-carbon graphite - Google Patents
Method for preparing high-purity graphite from high-carbon graphite Download PDFInfo
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- CN101654244A CN101654244A CN200910094952A CN200910094952A CN101654244A CN 101654244 A CN101654244 A CN 101654244A CN 200910094952 A CN200910094952 A CN 200910094952A CN 200910094952 A CN200910094952 A CN 200910094952A CN 101654244 A CN101654244 A CN 101654244A
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Abstract
The invention relates to a method for preparing high-purity graphite from high-carbon graphite, which has the following steps: mixing high-carbon graphite milled to 98 percent and filtered by a sieveof 0.0033 mm and a solution of hydrochloric acid for size mixing, carrying out stirring acid immersion at a temperature controlled from 60 to 120 DEG C, lixiviating the graphite after 2 to 4 hours, after the lixiviation of hydrochloric acid, washing the graphite by pure water to be neural to be mixed with a solution of sodium hydroxide for size mixing, carrying out alkali leaching in a pressurizing kettle, and effectively lixiviating impurities such as aluminum, and the like in the high-carbon graphite, wherein the lixiviating rate of the impurities is 99.6 percent, and the content of the fixed carbon in the obtained high-purity graphite is higher than 99.99 percent. The invention has short technical flow, and easy realization of industrial production, and the impurities such as aluminum,ferrum, calcium, zinc, copper and the like are efficiently and directly lixiviated, meanwhile, the lixivium of hydrochloric acid and the lixivium of pressurized alkali are mutually neutralized to obtain the sodium chloride for industrial use, no environmental pollution is caused, a closed circulation system is formed in the technical process, no outward discharge exists, and the production cost isreduced.
Description
Technical field
The present invention relates to a kind of Wet-process metallurgy method of removing impurity such as aluminium in the high-carbon graphite, iron, calcium, copper, zinc, more particularly, is a kind of method of being produced high purity graphite by high-carbon graphite.
Background technology
Graphite is in nature is present in as marble, quartzite, schist and leaf gneiss iso-metamorphism rock.It is the soft mineral of a germplasm, so graphite is also referred to as blacklead, pencil lead and mineral charcoal.The Mohs' hardness of graphite is 1～2, and shows complete basal cleavage; The proportion of pure graphite is 2.23, and theoretical density is 2.26 gram/cubic centimetres; Color is extremely black, opaque by ash, and metalluster is arranged; Sometimes show dark earthy gloss; Have flexible nonelasticly, higher electrical and thermal conductivity performance is arranged, and fireproof high-temperature resistant, fusing point reaches 3850 degree, and the unreactiveness of graphite is very strong, erosion that can acid and alkali-resistance.Be divided into high purity graphite, high-carbon graphite, medium-carbon graphite and low-carbon-content graphite four classes according to fixed carbon content.
High purity graphite: fixed carbon content is more than or equal to 99.9%; High-carbon graphite: fixed carbon content 94.0%～99.9%; Medium-carbon graphite: fixed carbon content 80%～94%; Low-carbon-content graphite: fixed carbon content is more than or equal to 50.0%～80.0%.
High purity graphite has anti-pyritous characteristic below 3000 ℃, and high temperature is indeformable, the electric conductivity height, and rub resistance can be used for the various heating units in large scale industry stove or the vacuum oven, heating chamber, siege, heating tube, support, graphite plate etc.And high-carbon graphite is owing to contain impurity such as aluminium, iron, calcium, copper, zinc, and range of application is much smaller, also falls far short on the price.Be necessary to explore a kind of effective ways and remove impurity such as aluminium in the high-carbon graphite, iron, calcium, copper, zinc, make the content of fixed carbon reach 99.99%, reach the method for high purity graphite requirement.
Summary of the invention
The invention provides a kind of overcome existingly insufficiently produce the method for high purity graphite by high-carbon graphite, it is simple, reliable easily row, impurities removing efficiency high, an eco-friendly full Wet-smelting method of a kind of smelting process.
The present invention realizes by following steps: (1), cross the high-carbon graphite of 0.0033mm sieve and hydrochloric acid soln that concentration is 50～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio to 98% with levigate, controlled temperature stirs acidleach for 60～120 ℃, leached through 2～4 hours, impurity such as the calcium in the high-carbon graphite, copper, zinc, iron are leached, and aluminium is then stayed in the carbon nuclear in a large number;
(2) till the high-carbon graphite after hydrochloric acid leaches is washed till neutrality with pure water;
(3) being washed till neutral high-carbon graphite and concentration is that the sodium hydroxide solution of 60～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, 120～200 ℃ of controlled temperature, pressure 1.5MPa～1.8Mpa, carrying out 2～4 hours pressurization alkali in autoclave soaks, impurity such as aluminium in this step medium high carbon graphite are leached, and the content of fixed carbon is greater than 99.99% in the high purity graphite of acquisition.
Above-mentioned raw material high-carbon stone China and Mexico fixed carbon content is between 94.0%～99.9%; Single impurity content of planting is no more than 5% in the high-carbon graphite, i.e. aluminium＜5%, iron＜5%, calcium＜5%, copper＜5%, zinc＜5%.
Above-mentioned pickling liquor and alkali immersion liquid neutralize mutually, and sodium-chlor is reclaimed in evaporation, and the wash water after the acidleach returns the acidleach section usefulness of sizing mixing, and the wash water after alkali soaks returns the pressurization alkali section of the soaking usefulness of sizing mixing; Whole technological process is closed system, and is free from environmental pollution.It is one section leaching that pressurization alkali soaks.
Beneficial effect of the present invention is: high-carbon graphite leaches through hydrochloric acid, leach with the alkali pressurization pure water washing back, technical process is short, realize suitability for industrialized production easily, wherein impurity such as aluminium, iron, calcium, zinc, copper are efficient directly leaches, impurity leaching yield 99.6%, the content of fixed carbon is greater than 99.99% in the high purity graphite of acquisition; Hydrochloric acid leachate and pressurization alkali leaching liquor neutralize mutually simultaneously, obtain industrial sodium-chlor, and environment is not constituted pollution, and technological process forms the closed circulation system, not outwards discharging, and reduced production cost.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The fixed carbon content of embodiment 1, high-carbon graphite is 94.5%, calcic 1.7%, and cupric 0.1%, iron content 1.32% contains aluminium 1.28%, contains zinc 1.1%, and is levigate to 98% mistake 0.0033mm sieve.
The hydrochloric acid soln that the high-carbon graphite that sieves and concentration are 50～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, add in the beaker, heat at water-bath, 60～120 ℃ of temperature, carry out the leaching about 2 hours, till high-carbon graphite after hydrochloric acid leaches was washed till neutrality with pure water, the wash water after the acidleach returned the acidleach section usefulness of sizing mixing; The sodium hydroxide solution that is washed till neutral high-carbon graphite and concentration and is 60～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, adds then in the autoclave, and 150 ℃ of controlled temperature, pressure 1.5MPa leaches by about 2 hours pressurizations.
Detected result is: aluminium leaching yield 99.43%, zinc leaching rate 99.67%, calcium leaching yield 100%, copper leaching rate 100%, iron leaching yield 99.34%.
Leach end after wash, dry, obtain high purity graphite, the content of its fixed carbon reaches 99.99%.After pickling liquor and alkali immersion liquid neutralized mutually, sodium-chlor was reclaimed in evaporation, and the wash water after the acidleach returns the acidleach section usefulness of sizing mixing, and the wash water after alkali soaks returns the pressurization alkali section of the soaking usefulness of sizing mixing.
The fixed carbon content of embodiment 2, high-carbon graphite is 98.0%, calcic 0.81%, and cupric 0.45%, iron content 0.32% contains aluminium 0.22%, contains zinc 0.2%, and is levigate to 98% mistake 0.0033mm sieve.
The hydrochloric acid soln that the high-carbon graphite that sieves and concentration are 50～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, add in the beaker, in the water-bath heating, 60～120 ℃ of temperature are carried out the leaching about 3 hours; Till high-carbon graphite after hydrochloric acid leaches was washed till neutrality with pure water, the wash water after the acidleach returned the acidleach section usefulness of sizing mixing; The sodium hydroxide solution that is washed till neutral high-carbon graphite and concentration and is 60～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, adds then in the autoclave, and 160 ℃ of controlled temperature, pressure 1.8MPa leaches by about 3 hours pressurizations.
Aluminium leaching yield 99.89%, zinc leaching rate 98.93%, calcium leaching yield 100%, copper leaching rate 100%, iron leaching yield 99.34%.
Leach end after wash, dry, the content of its fixed carbon reaches 99.99%.After pickling liquor and alkali immersion liquid neutralized mutually, sodium-chlor was reclaimed in evaporation, and the wash water after the acidleach returns the acidleach section usefulness of sizing mixing, and the wash water after alkali soaks returns the pressurization alkali section of the soaking usefulness of sizing mixing.
The fixed carbon content of embodiment 3, high-carbon graphite is 99.9%, calcic 0.012%, and cupric 0.035%, iron content 0.031% contains aluminium 0.010%, contains zinc 0.012%, and is levigate to 98% mistake 0.0033mm sieve.
The hydrochloric acid soln that the high-carbon graphite that sieves and concentration are 50～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, add in the beaker, in the water-bath heating, 60～120 ℃ of temperature are carried out the leaching about 4 hours; Till high-carbon graphite after hydrochloric acid leaches was washed till neutrality with pure water, the wash water after the acidleach returned the acidleach section usefulness of sizing mixing; The sodium hydroxide solution that is washed till neutral high-carbon graphite and concentration and is 60～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, adds then in the autoclave, and 180 ℃ of controlled temperature, pressure 1.8MPa leaches by about 4 hours pressurizations
Aluminium leaching yield 99.21%, zinc leaching rate 100%, calcium leaching yield 100%, copper leaching rate 99.31%, iron leaching yield 100%.
Leach end after wash, dry, the content of its fixed carbon reaches 99.99%.After pickling liquor and alkali immersion liquid neutralized mutually, sodium-chlor was reclaimed in evaporation, and the wash water after the acidleach returns the acidleach section usefulness of sizing mixing, and the wash water after alkali soaks returns the pressurization alkali section of the soaking usefulness of sizing mixing.
Claims (5)
1, produce the method for high purity graphite by high-carbon graphite, it is characterized in that step is:
(1), the levigate hydrochloric acid soln that is 50～100g/l to the high-carbon graphite and the concentration of 98% mistake 0.0033mm sieve is sized mixing by 3: 1 mixed of liquid-solid ratio, controlled temperature stirs acidleach for 60～120 ℃, leached through 2～4 hours, impurity such as the calcium in the high-carbon graphite, copper, zinc, iron are leached, and aluminium is then stayed in the carbon nuclear in a large number;
(2) till the high-carbon graphite after hydrochloric acid leaches was washed till neutrality with pure water, the wash water after the acidleach returned the acidleach section usefulness of sizing mixing;
(3) being washed till neutral high-carbon graphite and concentration is that the sodium hydroxide solution of 60～100g/l is sized mixing by 3: 1 mixed of liquid-solid ratio, 120～200 ℃ of controlled temperature, pressure 1.5MPa～1.8Mpa, carrying out 2～4 hours pressurization alkali in autoclave soaks, impurity such as aluminium in this step medium high carbon graphite are leached, and the content of fixed carbon is greater than 99.99% in the high purity graphite of acquisition.
2, produce the method for high purity graphite according to claim 1 is described by high-carbon graphite, it is characterized in that: described raw material high-carbon stone China and Mexico fixed carbon content is between 94.0%～99.9%.
3, produce the method for high purity graphite according to claim 1 is described by high-carbon graphite, it is characterized in that: single impurity content of planting is no more than 5% in the high-carbon graphite, i.e. aluminium＜5%, iron＜5%, calcium＜5%, copper＜5%, zinc＜5%.
4, produce the method for high purity graphite according to claim 1 is described by high-carbon graphite, it is characterized in that: it is that one section pressurization is leached that described pressurization alkali soaks.
5, produce the method for high purity graphite according to claim 1 is described by high-carbon graphite, it is characterized in that: pickling liquor and alkali immersion liquid neutralize mutually, and sodium-chlor is reclaimed in evaporation; Wash water after the acidleach returns the acidleach section usefulness of sizing mixing, and the wash water after alkali soaks returns the pressurization alkali section of the soaking usefulness of sizing mixing.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973545A (en) * | 2010-11-08 | 2011-02-16 | 昆明冶金研究院 | Method for purifying high-purity graphite |
| CN102583360A (en) * | 2012-04-16 | 2012-07-18 | 丁慧贤 | Method for purifying graphite by using microwave |
| CN102659100A (en) * | 2012-06-01 | 2012-09-12 | 成都中超碳素科技有限公司 | Preparation method of high-density fine-grain graphite material |
| CN103449425A (en) * | 2013-08-30 | 2013-12-18 | 黑龙江科技大学 | Method for preparing high-purity graphite through purifying natural high-carbon flake graphite by using alkaline-acid complexing method |
| CN104098092A (en) * | 2014-08-03 | 2014-10-15 | 北京矿冶研究总院 | Method for purifying natural microcrystalline graphite |
-
2009
- 2009-09-11 CN CN200910094952A patent/CN101654244A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973545A (en) * | 2010-11-08 | 2011-02-16 | 昆明冶金研究院 | Method for purifying high-purity graphite |
| CN101973545B (en) * | 2010-11-08 | 2012-09-05 | 昆明冶金研究院 | Method for purifying high-purity graphite |
| CN102583360A (en) * | 2012-04-16 | 2012-07-18 | 丁慧贤 | Method for purifying graphite by using microwave |
| CN102659100A (en) * | 2012-06-01 | 2012-09-12 | 成都中超碳素科技有限公司 | Preparation method of high-density fine-grain graphite material |
| CN103449425A (en) * | 2013-08-30 | 2013-12-18 | 黑龙江科技大学 | Method for preparing high-purity graphite through purifying natural high-carbon flake graphite by using alkaline-acid complexing method |
| CN104098092A (en) * | 2014-08-03 | 2014-10-15 | 北京矿冶研究总院 | Method for purifying natural microcrystalline graphite |
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Open date: 20100224 |