CN1334240A - Process for preparing super-purity alumina from gaolinite (gaolin) - Google Patents
Process for preparing super-purity alumina from gaolinite (gaolin) Download PDFInfo
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- CN1334240A CN1334240A CN 00113876 CN00113876A CN1334240A CN 1334240 A CN1334240 A CN 1334240A CN 00113876 CN00113876 CN 00113876 CN 00113876 A CN00113876 A CN 00113876A CN 1334240 A CN1334240 A CN 1334240A
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Abstract
A process for preparing high-purity aluminium oxide (Al2O3) from gaolin or coal-series gaolinite includes reaction of gaolin clinker with acid to produce aluminium salt, adding alkali to form aluminate to effectively separate impurities (Fe, Ti, etc) out, adding acid to form hydrate of aluminium, drying and washing to remove alkali ions. Its advantages are high purity of Al2O3 (more than 99.9%), low cost, and no environmental pollution.
Description
The present invention relates to a kind ofly utilize kaolin and coal series kaolin rock (soil), especially utilize high-Fe-Ti kaolin, coal series kaolin rock (soil) and coal gangue hill as the technology of raw material production purity greater than 99.9% ultrapure alumina product.
The general high aluminum ore such as bauxitic clay and metallic aluminium of adopting of existing ultrapure alumina producing raw material produced, and the method for external employing has the Bayer process of improvement, organoaluminum method, aluminium carbonate ammonium method, tschermigite pyrolysis method etc.The method of domestic employing is mainly the tschermigite pyrolysis method, and this technology is suitable for producing on a small scale, and floor space is big, and personnel labor intensity is big, and operating environment is poor, and technical process is long, to the requirement height of raw material.
Coal series kaolin rock (soil) is bigger at China's reserves, though wherein be no lack of the fine ore, but the ore reserves that the ferrotitanium foreign matter content is high is bigger, especially the coal series kaolin rock (soil) that exists with the form of colliery solid waste-coal gangue hill, its great majority or the overwhelming majority are the high ores of foreign matter content, the utilization of this part solid waste (waste dump) is to purify environment of mining area, keeps the important factor of Sustainable Development in Mining Areas.
With kaolin and coal series kaolin rock (soil) is that the ultrapure method of alumina king Hai Zhou of raw material production once declared patent: a kind of method of alumina (patent No. 91111359.2), this method is raw material roasting in advance dehydration back and ammonium sulfate sintering, leach with dilute sulphuric acid, with the neutralization of alum liquid and ammonia, hydrate calcine alumina product.Acid-precipitation method alumina technology (patent No. 1083023), this method be with the mineral after the roasting dehydration, monoammonium sulfate add sulfuric acid, ammoniumsulphate soln leach tschermigite, feed hydrogen chloride gas and separate out crystal aluminum chloride, after the pyrolysis aluminum oxide.Salting-out process is produced aluminum oxide (patent No. 1126177), this method is with getting the aluminum chloride leach liquor after the hydrochloric acid soln leaching of returning in the Production Flow Chart, the hydrogen chloride gas of deviating from when adding pyrolysis crystal aluminum chloride and one section distillation in leach liquor is saltoutd, saltout and to carry out repeatedly, finally can get common granularity aluminum oxide and submicron order aluminum oxide.Li Baixun applies for a patent: this method of technique for production of alumina by chlorhydric acid-soda method (patent No. 1065255) is to isolate alkaline aluminium salt behind the hydrochloric acid leaching roasting soil, aluminum oxide after inspissation, the roasting is dissolved in sodium hydroxide and generates sodium metaaluminate, the adding aluminum hydroxide crystal seed gets aluminum hydroxide crystals, must smelt aluminum oxide after the calcining.The patent of Wang Ping: the production technique of alumina in Nano level (patent No. 1146973) utilizes kaolin or aluminium hydroxide to adopt the production technique of salting-out process to make refining aluminum chloride and alumina gel, and the calcined oxide alumina gel gets aluminum oxide.
More than these methods to the requirement of raw material is all quite high or than higher, than higher raw material, its production cost is too high, causes to produce for foreign matter contents such as the higher especially ferrotitaniums of foreign matter content.In addition, the environmental pollution of salting-out process is comparatively serious, and acid mist is excessive, and the requirement that reaches ultrapure aluminum oxide need repeatedly be saltoutd, and technical process is long.
The purpose of this invention is to provide a kind of easy to operate, low production cost and non-environmental-pollution, be fit to use kaolin, coal series kaolin rock (soil) especially to the technology of the high ultrapure aluminum oxide of raw material scale operation of foreign matter content.
For achieving the above object, the technical solution used in the present invention is as follows:
Utilize kaolinite (soil) to produce the technology of ultrapure aluminum oxide, its special character is: above-mentioned production technique is undertaken by following several steps: (a) raw material calcining, activation back are generated the aluminium salt liquid body with acid-respons, after filtration, get rid of white residue, (b) the aluminium salt liquid body adds alkali formation aluminate, foreign ions such as Fe, Ti have effectively been separated, (c) aluminate adds the hydrate that acid forms aluminium, the hydrate drying of aluminium, washing, reach disposable rejecting basic ion, (d) with the dehydration of the hydrate of aluminium, after calcining, breaing up, ultrapure aluminum oxide.
In the drying process of above-mentioned (c) step, effectively raise the specific surface area of the hydrate of aluminium, its drying temperature is 450 ℃-950 ℃, is not less than 120 minutes time of drying; Best drying temperature is 650 ℃-850 ℃, and be 100 minutes time of drying.
Above-mentioned (b) step aluminium salt liquid body adds alkali and forms in the process of aluminate, and its reaction times is 120-240 minute, and the granularity of may command contamination precipitation thing again through Depth Filtration and microfiltration, is effectively separated these impurity.
With after the pulverizing of raw material process, raw material granularity reaches the 60-80 order, adopts the dynamic suspension calcining kiln to calcine for 10 seconds at 750-800 ℃ condition low suspension in above-mentioned (a) step.
Describe in detail below in conjunction with the drawings and specific embodiments:
Fig. 1 is that kaolin, kaolinite (soil) are produced ultrapure alumina technology synoptic diagram
The technique that the present invention produces super-purity aluminum oxide is to realize like this, kaolin, Coaseries kaolin are through after pulverizing, raw material granularity reaches about the 60-100 order, this powder adopts dynamic suspension calcining kiln calcining under 750-800 ℃ the condition low suspension about 10 seconds, make the chemism of raw material reach the highest, Al2O
3Leaching rate reach more than 90%; Calcine later material and acid reaction and generate the aluminium salt liquid body, liquid is got rid of white residue after filtering, and white residue can be used as the raw material of production White Carbon black and further processes. The aluminium salt liquid body generates aluminate with alkali reaction again, at this moment aluminium all exists with the form of liquid, impurity Fe, Ti etc. have then formed the hyrate of easy precipitation, after Separation of Solid and Liquid, separate fully with aluminate, for the higher ore of raw material iron content, impurity can be used as the raw material of production iron oxide red and further processes. Pure aluminate forms the hyrate of aluminium behind the rejecting impurity through neutralization, then after washing reaches certain purity, dewater, dry and calcining, break up and be alumina content greater than 99.9%, granularity is less than the super-purity aluminum oxide product of 10 μ m, (see photo).
This invention in forming the aluminate process, impurity is precipitated with the form of hyrate, form the easily material of precipitation, control sedimentary granularity, can effectively separate the precipitated impurities materials such as Fe, Ti, the impurity material that precipitates reaches the purpose of rejecting fully after filtration. The total amount of Fe, Ti, Ca, Mg impurity can be reduced to below 0.02% in the product that the method is processed.
Table 1 is impurity testing result table:
| Project | Quantitative spectrochemical analysis result (%) | ||
| Fe 2O 3 | CaO | MgO | |
| Raw material | 1.63 | 0.04 | 0.03 |
| After the deironing | 0.007 | 0.003 | 0.002 |
| Rejecting rate (%) | 99.57 | 92.50 | 93.33 |
After the impurity such as ferrotitanium were rejected, aluminate changed into the hyrate of aluminium, and the content of basic ion is higher in the hyrate of aluminium, adopts general method to be difficult to reject the purity of super-purity aluminum oxide product requirement.
This invention has been investigated thoroughly the occurrence status of basic ion in the hyrate of aluminium by various means of testing, research and test are found, the occurrence status of basic ion in the hyrate of aluminium has three kinds, one is absorption alkali, account for the 45-50% of basic ion total amount, it two is intergranular alkali, account for 48% of basic ion total amount, it three is crystalline alkali, account for the 3-5% of basic ion total amount, general washing only has effect to absorption alkali, only the content of alkali can be dropped to about 0.3% after the washing, and the alkali that rear two kinds of forms are existed, common washing be do not have resultful.
Test, research sum up the washing methods of a kind of effective rejecting absorption alkali and intergranular alkali, this method is that the hyrate with aluminium is 450 ℃-950 ℃ at baking temperature, be not less than drying time under 120 minutes conditions dry, increase as much as possible the specific area of material, make compose deposit with alumina gel in basic ion expose fully, and then through washing, reach the purpose of disposable rejecting absorption alkali and intergranular alkali, the content of alkali can drop to below the 0.03-0.02% in the product after this method washing.
Table 2 is Al (OH)3The clean result of middle sodium ion:
| Sample | Analytical results (%) | ?Na 2O content (%) | ||
| ????SiO 2 | ????Fe 2O 3 | ???Na 2O | ||
| Raw material | ????0.002 | ????0.004 | ???0.601 | ????100 |
| After the common washing | ????0.002 | ????0.004 | ???0.310 | ????48.42 |
| After the special washing | ???0.02 | ????48.25 | ||
| Remaining | ???0.02 | ????3.33 | ||
Embodiment 1:
Raw ore Al
2O
3: 38.36%;
Raw material granularity 60-80 order;
Calcining temperature 750-800 ℃;
Calcination time 12 seconds
Acidleach condition normal pressure;
Fine filtering condition＜2 μ m particles are worn the filter rate less than 2%;
Drying temperature 450-950 ℃;
Time of drying＜120 minute;
Calcining temperature＞1300 ℃;
Product purity Al
2O
3＞99.90%;
Product granularity＜10 μ m content are greater than 98%.
Embodiment 2:
Raw ore Al
2O
3: 33.28%;
Fe
2O
3：3.18％；
TiO
2：1.29％；
CaO：0.20％；
MgO：0.12％；
Raw material granularity 60-80 order;
Calcining temperature 750-800 ℃;
Calcination time 10 seconds
Acidleach condition normal pressure;
Fine filtering condition＜2 μ m particles are worn the filter rate less than 2%;
Drying temperature 650-850 ℃;
Time of drying＜120 minute;
Calcining temperature＞1300 ℃;
Product purity Al
2O
3＞99.90%;
Product granularity＜10 μ m content are greater than 98%.
Embodiment 3:
Raw ore Al
2O
3: 29.56%;
Fe
2O
3：9.37％；
TiO
2：1.06％；
CaO：0.12％；
MgO：0.11％；
Raw material granularity 60-80 order;
Calcining temperature 750-800 ℃;
Calcination time 13 seconds
Acidleach condition normal pressure;
Fine filtering condition＜2 μ m particles are worn the filter rate less than 2%;
800 ℃ of drying temperatures;
100 minutes time of drying;
Calcining temperature＞1300 ℃;
Product purity Al
2O
3＞99.90%;
Product granularity＜10 μ m content are greater than 98%.
Produce the byproduct red iron oxide simultaneously
Production technology of the present invention need not be carried out special removal of impurities processing to raw ore, thereby greatly reduces production cost, has simplified production technology, has reduced environmental pollution, and these impurity are got rid of in production process naturally. Another advantage of the present invention is, it is suitable for the processing of the higher solid waste such as kaolin, coal series kaolin rock (soil) and hillock of the high impurity ore that especially ferrotitanium content is high such as ferrotitanium content, and the content of the production cost of product and impurity is without obvious relation.
Claims (4)
1, utilize kaolinite (soil) to produce the technology of ultrapure aluminum oxide, it is characterized in that: above-mentioned production technique is undertaken by following several steps: (a) will generate the aluminium salt liquid body with acid-respons after raw material pulverizing, calcining, the activation, after filtration, get rid of white residue, (b) the aluminium salt liquid body adds alkali formation aluminate, foreign ions such as Fe, Ti have effectively been separated, (c) aluminate adds the hydrate that acid forms aluminium, the hydrate drying of aluminium, washing, reach disposable rejecting basic ion, (d) with the dehydration of the hydrate of aluminium, after calcining, breaing up, ultrapure aluminum oxide.
2, the technology of utilizing kaolinite (soil) to produce ultrapure aluminum oxide according to claim 1, it is characterized in that: in the drying process of above-mentioned (c) step, effectively raise the specific surface area of the hydrate of aluminium, its drying temperature is 450 ℃-950 ℃, is not less than 120 minutes time of drying; Best drying temperature is 650 ℃-850 ℃, and be 100 minutes time of drying.
3, the technology of utilizing kaolinite (soil) to produce ultrapure aluminum oxide according to claim 1 and 2, it is characterized in that: above-mentioned (b) step aluminium salt liquid body adds alkali and forms in the process of aluminate, its reaction times is 120-240 minute, the granularity of may command contamination precipitation thing, through Depth Filtration and microfiltration, effectively separate these impurity again.
4, the technology of utilizing kaolinite (soil) to produce ultrapure aluminum oxide according to claim 3, it is characterized in that: in above-mentioned (a) step raw material is passed through after the pulverizing, raw material granularity reaches the 60-80 order, adopts the dynamic suspension calcining kiln to calcine for 10 seconds at 750-800 ℃ condition low suspension.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100465096C (en) * | 2007-05-08 | 2009-03-04 | 浙江大学 | Method for preparing sheet alumina using coal series kaolin rock or flyash as raw material |
| CN104399426A (en) * | 2014-12-08 | 2015-03-11 | 中国矿业大学 | Production method of aluminum-doped hydroxyapatite defluorinating filter material |
| CN106241843A (en) * | 2016-07-19 | 2016-12-21 | 武汉理工大学 | A kind of method that aluminium hydroxide is prepared in polyaluminium waste slag of aluminum acid system recovery |
| CN113003579A (en) * | 2021-03-23 | 2021-06-22 | 内蒙古科技大学 | Green method for comprehensive utilization of coal gangue |
| CN116462490A (en) * | 2023-04-27 | 2023-07-21 | 无锡成旸科技股份有限公司 | High-hardness alumina grinding powder and preparation method thereof |
-
2000
- 2000-07-14 CN CN 00113876 patent/CN1334240A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100465096C (en) * | 2007-05-08 | 2009-03-04 | 浙江大学 | Method for preparing sheet alumina using coal series kaolin rock or flyash as raw material |
| CN104399426A (en) * | 2014-12-08 | 2015-03-11 | 中国矿业大学 | Production method of aluminum-doped hydroxyapatite defluorinating filter material |
| CN104399426B (en) * | 2014-12-08 | 2017-04-26 | 中国矿业大学 | Production method of aluminum-doped hydroxyapatite defluorinating filter material |
| CN106241843A (en) * | 2016-07-19 | 2016-12-21 | 武汉理工大学 | A kind of method that aluminium hydroxide is prepared in polyaluminium waste slag of aluminum acid system recovery |
| CN113003579A (en) * | 2021-03-23 | 2021-06-22 | 内蒙古科技大学 | Green method for comprehensive utilization of coal gangue |
| CN113003579B (en) * | 2021-03-23 | 2023-03-24 | 内蒙古科技大学 | Green method for comprehensive utilization of coal gangue |
| CN116462490A (en) * | 2023-04-27 | 2023-07-21 | 无锡成旸科技股份有限公司 | High-hardness alumina grinding powder and preparation method thereof |
| CN116462490B (en) * | 2023-04-27 | 2023-12-12 | 无锡成旸科技股份有限公司 | High-hardness alumina grinding powder and preparation method thereof |
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