CN1241533A - Intensified sintering process for alumina production - Google Patents
Intensified sintering process for alumina production Download PDFInfo
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- CN1241533A CN1241533A CN 99109676 CN99109676A CN1241533A CN 1241533 A CN1241533 A CN 1241533A CN 99109676 CN99109676 CN 99109676 CN 99109676 A CN99109676 A CN 99109676A CN 1241533 A CN1241533 A CN 1241533A
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Abstract
The alumina producing process includes the steps of raw slurry preparation of grinding the material including high aluminum/silicon ratio ore, lime, coal, evaporating carbon material and alkali, sintering raw slurry to obtain chamotte; chamotte digestion and separation with red mud to obtain coarse liquid; press digesting desiliconization and silicon dreg separation to obtain the first refined liquid; normal pressure desiliconization and silicon dreg separation to obtain the second refined liquid; carbonization and separation of the second refined liquid to obtain aluminum hydroxide slurry, and separation, washing and roasting of aluminum hydroxide slurry to obtain alumina product.
Description
The present invention relates to a kind of process for making alumina, particularly a kind of process for making alumina of intensified sintering.
The aluminum oxide industry production method mainly is an alkaline process in the world at present, comprise sintering process and bayer's process and two kinds of integrated processs that basic skills is combined to form thus, 90% alumina product adopts bayer process production in the world, its raw material is high aluminium silicon ratio (A/S) ore, be lower than 4.5 bauxite for alumina silica ratio and adopt bayer's process just very uneconomical, have only the employing sintering process; Adopt the major country of sintering process explained hereafter aluminum oxide that USSR (Union of Soviet Socialist Republics), China and Greece are arranged in the world, the sintering process of China is introduced from USSR (Union of Soviet Socialist Republics), though through the theoretical investigationes in more than 40 years and production practice, improved sintering process technology, but theoretical frame is not broken through, and is referred to as traditional sintering process production technique.
Traditional sintering process grog prescription adopts low alkali ([N/R]＜1.0), high calcium ([C/S]＞2.0) its theoretical core of filling a prescription to be: aluminum oxide and sodium oxide in the charge pulp of low A/S ore preparation generate sodium aluminate in the grog sintering process, major impurity SiO2, TiO2 and CaO generate Dicalcium Phosphate (Feed Grade) and uhligite respectively, and impurity F e2O3 and sodium oxide generate sodium ferrite.At the stripping separation circuit, sodium aluminate solution is in alkali lye, unsettled α-Dicalcium Phosphate (Feed Grade) of the minute quantity that generates in the grog sintering process and dissolution fluid interact, cause a small amount of SiO2 to enter solution and a spot of aluminum oxide loses because of secondary reaction, and most of Dicalcium Phosphate (Feed Grade) and uhligite are insoluble to solution is the main body of abandoning red mud, sodium ferrite is in process in leaching, and sodium oxide enters solution, and ferric oxide enters red mud.Be based upon the sintering process production technique on this theoretical basis thereby have following shortcoming:
1, the ore grade of Chu Liing is lower, burns till grog alumina content low (having only 34%-35%), a/s low (≤3.4), thereby the solid materials amount that causes whole production system to handle is big.
2, sintering temperature height, firing range are narrow, and particularly along with the raising of grog A/S, the operation of calcining kiln is difficulty more and more, and the ceiling value of A/S that burns till grog in the production is 3.5.
3, because in the sintering process, SiO2 is most of to form 2CaO.SiO2 with CaO2, and a small amount of unsettled α '-2CaO.SiO2 forms and the existence of free CaO, and the secondary reaction loss becomes the weak link that the conventional sintering method is difficult to overcome, and causes digesting efficiency of alumina to reduce.
4, because the grog alumina content is low, solubility rate is low, and the stripping operation is subjected to the influence of isolating restriction of red mud and secondary reaction, and the dissolution fluid alumina concentration is low, the wet method system alumina concentration is generally lower.
5, in order to limit the carrying out of secondary reaction, adopt low α K dissolving-out technology (stripping α K is about 1.2) and Nc concentration is had certain limited field, adopt carbon mother liquid and red mud wash liquor as the important component part of adjusting liquid.The stripping liquid concentration level finally maintains about 115g/l, and prepared seminal fluid alumina concentration has only 90-95g/l after twice desiliconization.The operation of wet method system lower concentration causes wet method system liquid measure internal circulating load big.
6, produce traditional bigger solids melt treatment capacity, bigger liquid circulation amount, cause total system throughput under same equipment preparation condition to reduce, power consumption such as former, combustion, material and water, electricity, wind, vapour increase, and the production economic and technical norms are low, and production cost is higher.
In view of this, how to utilize original equipment, adopt sintering process to handle the aluminum ore of high aluminium silicon ratio, make the output capacity height, technology is simple, cost is low, and the present invention grinds wound motivation place just.
Aluminum oxide is researched and produced the practical experience of processing and other fields to designer of the present invention and to the objective reality needs, on the basis of feasibility study repeatedly, do a brand-new technological design formation, the generation that gets a kind of intensified sintering technology of the present invention eventually by means of being engaged in for many years.
At the deficiencies in the prior art, the objective of the invention is to design a kind of high A/S ore and take sintering process to produce alumina technology, it still has excellent economy and output capacity.
Grog prescription of the present invention adopts saturated alkali to fill a prescription than ([C/S]＜1.5) than ([N/R]=1), unsaturated calcium, its theoretical foundation is: aluminum oxide and sodium oxide in the charge pulp of high A/S ore preparation generate sodium aluminate in the grog sintering process, major impurity SiO2 and TiO2 also have water glass, sodium aluminium silicate to exist except forming Dicalcium Phosphate (Feed Grade), uhligite respectively.Aluminum oxide in process in leaching mesosilicic acid sodium, sodium aluminium silicate, silicon oxide, sodium oxide can enter solution, be unlikely to cause the loss of aluminum oxide and sodium oxide, the SiO2 that enters solution is sloughed in follow-up desiliconization process, presses the sodium white residue that boils the desiliconization generation to add and effluxes after sodium oxide is further reclaimed in milk of lime reinforcement stripping.
Purpose of the present invention can realize as follows: the lime that high aluminium silicon ratio ore and Wingdale and coal are fired into, coal, evaporate carbon mother, ground caustic carries out raw material and grinds and make qualified charge pulp, charge pulp obtains grog through firing process, grog is carried out stripping, separate through red mud again and obtain thick liquid, thick liquid boils desiliconization through pressure, the white residue separation obtains seminal fluid one time, frequent again pressure-off silicon, calcium-silicon slag separates, obtain the secondary seminal fluid, the secondary seminal fluid can obtain aluminum hydroxide slurry through carbon branch and kind branch respectively, again through separating, aluminium hydroxide after the washing obtains the aluminum oxide finished product through roasting, carbon mother liquid returns batching through evaporation, seed precipitation solution directly send the stripping operation to adjust liquid, thereby realize the recycle of alkali, one time silicon destarch liquid effluxes after washing through milk of lime reinforcement stripping and the separating obtained red mud of red mud through the sodium white residue of white residue resulting separation, and the washing lotion that obtains is re-used as the recycle of adjustment liquid.Atmospheric silicon removing gained calcium-silicon slag after white residue separates returns batching.
Fig. 1 is a process flow diagram of the present invention.
The purpose that raw material grinds is to obtain the slip of certain fineness and proportioning and suitable water content, The difference of the present invention and conventional sintering method is that at first the grog proportioning adopts saturated alkali ratio, unsaturated calcium ratio Prescription, thus the difference of raw mix formula caused. The present invention is by to deeply grinding in the clinkersintering process Study carefully discovery: Al2O3, Na2O, SiO2, TiO2, CaO just begin during low temperature anti-at the sintering process initial stage Should, generate sodium aluminosilicate (Na2OAl2O32SiO2), when CaO exists, along with temperature Raising and the sodium aluminosilicate that carries out of sintering reaction be broken down into sodium aluminate (Na2OAl2O3) and silicic acid Dicalcium (2CaOSiO2), the final result of reaction still is sodium aluminate, silicon if calcium oxide is excessive Acid dicalcium and free calcium oxide are if the quantity not sufficient of calcium oxide is with whole generation dicalcium silicates, oxidation Silicon exists with dicalcium silicate, sodium metasilicate, sodium aluminosilicate form, if there is not calcium oxide to have (reality During test, owing to contain calcium oxide in the ore, the calcium oxide content in the grog is generally about 2%), Silica mainly exists with sodium metasilicate, sodium aluminosilicate form. Research finds that the grog of different calcium ratio exists During stripping, the silica content difference in the dissolution fluid is very big. When being unworthy of calcium, the silica in the grog is exhausted Major part enters solution, and along with the raising of calcium ratio, the dissolution rate of the silica in the grog reduces gradually. Suitably allocate CaO into, make calcium than 1.5, the mass ratio that burns till grog is higher. The present invention considers grog Burn till the control of the technical indicator of the technical process such as quality and grog stripping, red mud separation and desiliconization, Determine that calcium is than prescription. Compare with traditional sintering process, since the reduction of calcium ratio, the oxygen in the dissolution fluid SiClx concentration increases, and for the loss amount of avoiding a desiliconization process sodium oxide molybdena increases, the present invention adopts With adding milk of lime to reclaim sodium oxide molybdena wherein, take off and efflux after white residue behind the sodium enters laterite washing. By In adopting high aluminium silicon ratio ore and low calcium than prescription, the sodium white residue directly effluxes after washing, in the grog Alumina content is greatly improved, and therefore, grog reduced ratio, red mud output capacity reduce greatly, ton The aluminium oxide solid materiel flux significantly reduces; The wet method systems such as stripping liquid concentration, seminal concentration are dense simultaneously Degree also improves greatly, and the minimizing of total system solid, liquid amount treating capacity, the raising of dissolution rate are so that production capacity is big Amplitude improves, and various consumption significantly reduce, and economic and technical norms are obviously improved.
It is the core of sintering process technology that grog burns till, the main component Al2O3 in the raw material, Na2O, Fe2O3, TiO2, SiO2, CaO by burn till reaction generated respectively sodium aluminate (Na2OAl2O3) that can be water-soluble, Sodium ferrite (Na2OFe2O3) (for prescription of the present invention, also have sodium metasilicate (Na2OSiO2), Sodium aluminosilicate (Na2OAl2O32SiO2)), stable dicalcium silicate (2CaOSiO2) is (main If the dicalcium silicate of β and γ form) and the unsettled dicalcium silicate of part (mainly be α and α ' Dicalcium silicate); Cause the instability of technology, the present invention burns till does not have α ' and α silicic acid substantially in the grog Dicalcium. The operation of conventional sintering method calcining kiln is particular about " fast, short-flame, just burn ", burns till grog The alumina silica ratio Up limit is 3.5. It is the high aluminium silicon ratio grog that the present invention burns till grog, for kiln system Operation carried out a series of adjustment. Suitably strengthen front wind, widen rear wind; Take long flame operation; System temperature behind the raising kiln, kiln end temperature is greater than 200 ℃; Suitably reduce the rotating speed of kiln; Grog unit weight Be controlled at the 0.9-1.15 scope, this is one of key technology of the present invention.
The purpose of grog stripping be to make useful component in the grog be dissolved in alkali lye or by with alkali lye mutually Effect is so that useful component enters solution system, and impurity is owing to being insoluble to solution or mutually doing with solution Exist with solid forms with entering red mud.
The conventional sintering method has free calcium oxide to have impurity two owing to adopt high-calcium formula in the grog Silica exists with the dicalcium silicate form, particularly wherein a part of dicalcium silicate with unsettled α and α ' dicalcium silicate form exists, so that secondary response is more serious in the process in leaching, causes aluminium oxide Loss becomes the chronic illness that the conventional sintering method is difficult to overcome. Be the loss of as far as possible avoiding secondary response to cause, Dissolving-out process adopts low α k dissolving-out technology, and strictly controls Nc concentration, and the factory that has also adopts Two sections grinding process flow processs and the way that increases special filtering equipment to be reducing the secondary response loss, although Obtained some effects, but not only increased equipment investment, operating cost also increases simultaneously.
It is high A/S grog that the present invention burns till grog, adopts unsaturated calcium than prescription, not trip in the grog From calcium oxide, the content of dicalcium silicate is relatively less, does not substantially have unsettled α and α ' silicic acid two Calcium exists, and has avoided the secondary response of stripping workshop section, thus can adopt high α k dissolving-out technology, molten Go out α k=1.35-1.45, replace the carbon mother liquid preparation to adjust liquid with seed precipitation solution. Because oxidation in the grog Aluminium increased content (〉=43%), red mud output capacity significantly reduce and owing to have adopted high α k stripping skill Art, dissolution fluid alumina concentration reach (conventional sintering method, dissolution fluid alumina concentration about 180g/l Only have about 115g/l), for the raising of wet method system concentration is laid a good foundation, this is pass of the present invention Two of key technology.
Red mud separates the liquid-solid separation of stripping slurries, and purpose is to realize separating of liquid phase useful component and solid impurity.
Because the unit weight of grog is low, stripping liquid concentration improves, the obvious variation of the settling property of red mud, but strainability is better.The present invention separates the different isolation technique of employing to red mud and studies, adopt rotary drum filter plant and sedimentation strainer, various filtration, filtering equipment all can satisfy industrial needs, research subsequently shows again, if red mud boils the crystal seed of desiliconization as pressure, pressure is boiled desiliconization and also can be obtained satisfied desiliconization effect.White residue and fine through the red-mud settlement performance after the pyroprocessing can satisfy industrial needs fully, and the present invention adopts turner as separating device, and this is three of a gordian technique of the present invention.
The purpose of desiliconization is further to reduce the silica content in the solution, reduces the content of silicon oxide impurity in the product.The desiliconization of the thick liquid of high density is a technical barrier of failing to capture for a long time always.The present invention is owing to adopted high α k dissolving-out technology in the stripping operation, the forward and backward seed precipitation solution that all do not add of desiliconization is adjusted solution α k, the desiliconization slurries contain 〉=60g/l admittedly, the Flocculating Settling Technology that adopts 220, desiliconization slurries of a desiliconization index realizes liquid, the solid separation, the milk of lime add-on that atmospheric silicon removing control is suitable, adopt and strengthen the desiliconization technology, control suitable temperature, time and suitable reaction conditions, desiliconization index reaches more than 600, and this is four of a key problem in technology of the present invention.
The present invention not only studies for being based upon new theoretic each technological process, has taked to be different from the process control technology index and the working method of conventional sintering method, and is a complete alumina by sintering new process of production.Complete new process for making alumina must have and overlaps the new material balance that technology therewith is complementary.Of the present invention finishing that is the foundation of the material balance that new.Because the present invention is used to handle high-grade aluminum ore, alumina content in the grog is far above the grog of conventional sintering method, require the alkali number of joining in the raw material obviously to increase, soda balance is the key that can whole technology connect enforcement, and the prerequisite that throughput improves more than 30% is that the charge pulp change of soil water content is little.The present invention studies carbon mother liquid Ns, Nc, Nk, A equilibrium concentration and different evaporation technologies, adopts technology such as crystallization and evaporation, sedimentation concentrate can satisfy the needs of soda balance of the present invention, and this is five of a gordian technique of the present invention.
The present invention and conventional sintering method compare, and raw material consumption reduces 10%-15%, and power consumption, fuel consumption, process energy consumption reduce 20%-25%; Quality product seconds rate 100%, the ratio of first-grade products 40%; Under equal equipment level conditions, production capacity improves more than 30%, has simplified technical process.
Embodiment: the industry operation that commerical test of the present invention adopts the existing long pass central siphon mill of Central Region aluminium manufacturer, Φ 4.5 * 100M calcining kiln, stripping mill, desiliconization unit and other equipments of industrial product to carry out 25 days in Central Region aluminium manufacturer, burn till and 16000 tons in stripping grog concrete technical indicator and control condition:
(1) raw material: ore: Al2O3 〉=content 68%, A/S 〉=10.5
(2) raw material grinds: [N/R]=1.03 ± 0.04 moisture content＜40%
[C/S]=1.65-1.75 fineness+120#＜12%
(3) grog burns till prescription [N/R]=1.02 ± 0.02, [C/S]=1.5 ± 0.03, and firing temperature is not less than 1250 ℃.
(4) stripping: the unit cubic meter is adjusted liquid stripping clinker quantity 350-400 kilogram, 90-100 ℃ of stripping temperature, stripping α k=1.35-1.45, dissolution fluid alumina concentration 〉=180 gram/l.
(5) red mud separating underflow L/S≤4
(6) desiliconization, the high pressure desiliconization, each desilicator and flash-pot, dashpot pressure and temp are with traditional sintering process, and desiliconization dope contains 〉=60g/l admittedly, a desiliconization index 220-230; Atmospheric silicon removing: milk of lime add-on 6g/l, 105 ℃ of desiliconization temperature, desiliconization time 60-120 minute, secondary seminal fluid siliceous modulus 〉=600.
The key technical indexes that obtains is as follows: 1, grog alumina content 43%-45%, A/S, 8.0 ± 0.5; 2, dissolution fluid alumina concentration 170-190g/l; 3, seminal fluid alumina concentration 〉=160g/l; 4, seminal fluid A/S is more than 600.
Claims (6)
1, a kind of intensified sintering process for alumina production, it is characterized in that the high aluminium silicon ratio ore, lime, coal, evaporate carbon mother, ground caustic carries out raw material and grinds and make qualified charge pulp, charge pulp obtains grog through firing process, grog is carried out stripping, separate through red mud again and obtain thick liquid, thick liquid boils desiliconization through pressure, the white residue separation obtains seminal fluid one time, frequent again pressure-off silicon, calcium-silicon slag separates, obtain the secondary seminal fluid, the secondary seminal fluid can obtain aluminum hydroxide slurry through carbonization and kind branch respectively, again through separating, aluminum oxide after the washing obtains the aluminum oxide finished product through roasting, carbon mother liquid returns batching through evaporation, seed precipitation solution directly send the stripping operation to adjust liquid, thereby realize the recycle of alkali, silicon destarch liquid takes off through milk of lime through the sodium white residue of white residue resulting separation to be received and red mud that red mud is separating obtained effluxes after washing, and the washing lotion that obtains is re-used as and adjusts the liquid recycle.Atmospheric silicon removing gained calcium-silicon slag after white residue separates returns batching.
2, technology according to claim 1 is characterized in that the grog proportioning adopts saturated alkali ratio, unsaturated calcium than prescription.
3, technology according to claim 1 is characterized in that grog burns till employing and strengthens preceding wind, widens after wind; System temperature behind the raising kiln, kiln end temperature is greater than 200 ℃; Take long flame operation; Suitably reduce the rotating speed of kiln; Grog unit weight is controlled at the 0.9-1.15 scope.
4, technology according to claim 1 is characterized in that process in leaching adopts high α k dissolving-out technology, and stripping α k=1.35-1.45 replaces the carbon mother liquid preparation to adjust liquid with seed precipitation solution.
5, technology according to claim 1 is characterized in that the configuration of high-concentration sodium aluminate solution deep desilication process and equipment.
6, technology according to claim 1 is characterized in that guaranteeing the whole process soda balance and the crystallization and evaporation sedimentation of inventing is concentrated to the above evaporation technology configuration of NT300g/l.
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| CN100532263C (en) * | 2007-09-18 | 2009-08-26 | 中国铝业股份有限公司 | Treatment method for filtering white residue in production of alumina by mixture combination process |
| CN102277594A (en) * | 2011-08-13 | 2011-12-14 | 祝向辉 | Manufacturing method of aluminum ingot being less prone to producing needle-like beta-AlFeSi impurity phase |
| CN103351013A (en) * | 2013-06-27 | 2013-10-16 | 中国铝业股份有限公司 | Method for producing aluminum oxide by sintering process |
| CN106315637A (en) * | 2015-07-03 | 2017-01-11 | 北京华索科技股份有限公司 | Filter cake reutilization method in production process of aluminum oxide and system thereof |
| CN106365187A (en) * | 2016-08-30 | 2017-02-01 | 内蒙古大唐国际再生资源开发有限公司 | Preparation method of raw slurry used in process of producing aluminum oxide through sintering method |
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| CN114349032A (en) * | 2022-02-22 | 2022-04-15 | 淄博坤厚新材料科技有限公司 | Aluminum oxide blank calcining process and equipment |
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| CN1314591C (en) * | 2004-05-14 | 2007-05-09 | 山东铝业股份有限公司 | Process for preparing alumina by two-component sintering method |
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| CN100361897C (en) * | 2005-11-28 | 2008-01-16 | 中国铝业股份有限公司 | Sintering process sodium aluminate solution desilicification method |
| CN100542959C (en) * | 2006-05-17 | 2009-09-23 | 中国铝业股份有限公司 | Ash conversion method in a kind of alumina producing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| IN168397B (en) * | 1983-04-18 | 1991-03-23 | Vni Pi Aljuminievoi Magnievoi | |
| US4865589A (en) * | 1987-04-22 | 1989-09-12 | Ludwig Simmet | Instrument for the transfer of materials such as sperm and embryos |
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| CN102277594A (en) * | 2011-08-13 | 2011-12-14 | 祝向辉 | Manufacturing method of aluminum ingot being less prone to producing needle-like beta-AlFeSi impurity phase |
| CN103351013A (en) * | 2013-06-27 | 2013-10-16 | 中国铝业股份有限公司 | Method for producing aluminum oxide by sintering process |
| CN106315637A (en) * | 2015-07-03 | 2017-01-11 | 北京华索科技股份有限公司 | Filter cake reutilization method in production process of aluminum oxide and system thereof |
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| CN114538489A (en) * | 2022-03-18 | 2022-05-27 | 四川轻化工大学 | Method and system for preparing efficient powdery accelerator from aluminum ash |
| CN114940506A (en) * | 2022-04-01 | 2022-08-26 | 国家电投集团山西铝业有限公司 | Liquid caustic soda sintering method in alumina production series process and clinker |
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