CN102398912B - Dissolution technology of high alumina fly ash by method of sulphuric acid - Google Patents
Dissolution technology of high alumina fly ash by method of sulphuric acid Download PDFInfo
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- CN102398912B CN102398912B CN201010281024.0A CN201010281024A CN102398912B CN 102398912 B CN102398912 B CN 102398912B CN 201010281024 A CN201010281024 A CN 201010281024A CN 102398912 B CN102398912 B CN 102398912B
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Abstract
The invention discloses a dissolution technology of high alumina fly ash by a method of sulphuric acid, comprising the following steps: mixing high alumina fly ash with dilute sulfuric acid in proportion to obtain an original pulp A; sending the original pulp A into a dissolution unit through a dissolution charging pump, preheating through grade 1-3 sleevings to obtain a preheat pulp B; heating the sleevings to heat the preheat pulp B to obtain a heating pulp C; sending the heating pulp C in a digester for carrying out insulation dissolution to obtain a dissolved pulp D under the conditions of insulation and pressure maintaining; and carrying out 3-level self-evaporation cooling on the dissolved pulp D, and then sending the cooled dissolved pulp D and an acid sludge washing liquor E into a dilution trap to obtain a mixed pulp F. According to the invention, alumina is dissolved out from the high alumina fly ash and enters in the solution, and the dissolution rate of alumina is 85-90 %, so that the preparation for subsequent production process is made; the high alumina fly ash is utilized reasonably, the cost is low, the advantage of economic rationality is achieved, and the problem of corrosion of devices in the dissolution process is solved.
Description
Technical field
The present invention relates to a kind of aluminum oxide industry field, especially a kind of aluminous fly-ash dissolving-out process.
Background technology
Produce every year in the world at present more than 7,000 ten thousand tons of aluminum oxide, it is raw material that each alumina producer almost all adopts bauxite.China is maximum in the world alumina producing state, and approximately 3,000 ten thousand tons of aluminum oxide of annual production, account for 40% of Gross World Product.But China's bauxite resource is relatively poor, 6% left and right of bauxite reserves Jin Zhan world total reserves, ore grade is lower, and ore type mainly be take unmanageable diaspore as main, and complex treatment process, energy consumption are high, and production cost is also higher.Due to China's bauxite resource wretched insufficiency, can only rely on from external Ore Imported and solve raw material problem, approximately 3,000 ten thousand tons of China's year import Bauxite Ores, account for 50% left and right of domestic bauxite usage quantity.Ore resource is not enough, has seriously restricted the development of China's aluminum oxide industry, finds new alternative non-bauxite resource as aluminum oxide industry raw material, researchs and produces the task of top priority that Technology that aluminum oxide is new becomes China's aluminium industrial development.
Coal resources in China is very abundant, and coal production accounts for the first in the world, annual more than 20 hundred million tons of coals of output, and coal is most of will discharge a large amount of flyash for thermal power plant's generating after coal burning, and China's annual approximately discharge aluminous fly-ash (refers to Al in flyash
2o
3>=38%) more than 100,000,000 tons.Analyze after deliberation, aluminous fly-ash is mainly comprised of aluminum oxide, silicon oxide, the content of 2 kinds of compositions accounts for 80%, other compositions such as another iron content, magnesium, titanium, calcium, in some flyash, also contain the abundant rare precious metals such as gallium, be the raw material that metallurgical-grade aluminum oxide and gallium are extracted in comprehensive utilization, there is high industrial utilization and be worth.In the flyash of the northern area of China, alumina content is generally higher than southern area, if alumina content in the flyash of part mining area, the ground outputs such as Shanxi, Shaanxi, Inner Mongol, Ningxia, Xinjiang is conventionally in 40% left and right, belong to aluminous fly-ash, in the flyash of Ordos, inner Mongolia area, alumina content has up to 45～50%, this is suitable with the alumina content in external bauxite trihydrate, from chemical composition analysis, can be used as one of raw material extracting metallurgical-grade aluminum oxide completely.
The flyash waste that normally thermal power plant discharges, stores up mainly as a kind of industrial residue at present, and this had both taken a large amount of soils, and severe contamination environment, for safeguarding the safe operation in lime-ash stockyard, also need lime-ash stockyard to safeguard, this has just increased the production cost of power plant.Coastland is due to populous, industry prosperity, sometimes flyash is used for building the road, the material of construction such as brickmaking, this only belongs to low-grade, the low value-added application of flyash, and economically underdeveloped area or west area, flyash is still stored up mainly as industrial residue.On the whole, China and World Developed Countries still in the experimental study stage, are being found the approach that it rationally utilizes to total utilization of PCA problem.
In recent years, for the present situation of China's bauxite resource wretched insufficiency, the many scientific research departments of China and universities and colleges, actively develop non-bauxite resource production metallurgy grade aluminum oxide research, and emphasis is research aluminous fly-ash comprehensive utilization production metallurgy grade aluminum oxide.Each research unit's basis achievement in research separately, has proposed some and has processed the new process of aluminous fly-ashs, and main direction of studying is as follows:
(1) alkaline process: the main stream approach that is aluminous fly-ash comprehensive utilizating research.It mainly uses for reference the sintering process production technique of existing alumina industry maturation, utilize sintering process technique can process feature low-grade, low alumina-silica ratio ore, aluminous fly-ash, Wingdale (or lime), alkali are pressed to certain proportioning, be prepared into charge pulp and carry out sintering, sintered clinker is through stripping, desiliconization, decomposition, roasting and obtain metallurgical-grade aluminum oxide product.The advantage of this method is that Technology is ripe, can obtain qualified alumina product.But the shortcoming of this method is a lot, be mainly that lime dosage is huge, red mud amount is large, concentration sodium aluminate solution is low, production energy consumption is high, its investment and cost are high, and it is technical feasible but unreasonable economically for this method.
(2) salt acid system: adopt hydrochloric acid and aluminous fly-ash to prepare burden in proportion, aluminum oxide under certain temperature and pressure condition in stripping flyash, obtain liquor alumini chloridi, then through slagging-off, obtain pure liquor alumini chloridi, liquor alumini chloridi obtains alumina product through evaporative crystallization, roasting, and its advantage is that flow process is simple, the quantity of slag is little, production cost is low.Shortcoming is that removing iron from solution of aluminum chloride and removal of impurities are more difficult, hydrochloric acid is very serious to the corrosion of equipment at 80～160 ℃ of temperature, and some Design and material problems need further be researched and solved.
Summary of the invention
The object of the invention is: a kind of aluminous fly-ash sulfuric acid process dissolving-out process is provided, can makes the alumina leaching in aluminous fly-ash, make it enter solution, and production cost is low, little to equipment loss, to overcome the deficiencies in the prior art.
The present invention is achieved in that aluminous fly-ash sulfuric acid process dissolving-out process, and aluminous fly-ash is mixed in proportion with dilute sulphuric acid, makes raw pulp A; Raw pulp A is sent in dissolving device by stripping fresh feed pump at normal temperatures, by 1～3 grade of sleeve pipe, carry out preheating, the raw pulp A temperature after preheating reaches 85～90 ℃, obtains preheating ore pulp B; Sleeve pipe is heated to 145～155 ℃ again, makes preheating ore pulp B be heated to 145～155 ℃, obtain heating ore pulp C; Heating ore pulp C is sent in autoclave again and be incubated stripping, under the condition of 175～185 ℃ of insulations, pressurize 0.8～1.0MPa, stripping 60～90min, obtains stripping slurry D; Stripping slurry D is together sent in dilution trap with acid sludge washing lotion E after 3 grades of self-evaporatint n.s are cooled to 115～118 ℃, obtain temperature and be the mixed slurry F of 100～110 ℃, be the intermediate product that dissolving-out process obtains.
The mass percent concentration of dilute sulphuric acid is 25～40%.
The blending ratio of aluminous fly-ash and dilute sulphuric acid adopts the ratio of alumina leaching chemical reaction Theoretical Calculation amount 1.0 values.
The secondary steam that stripping slurry D is produced through 3 grades of self-evaporatint n.s turns back in sleeve pipe, for preheating procedure.
20～21 ℃ of every grade of self-evaporatint n. coolings of stripping slurry D.
In autoclave, be provided with agitator, agitator, in the process of insulation stripping, keeps heating ore pulp C to stir.
The inner tube of sleeve pipe is lead alloy inner tube, and outer tube is stainless steel tube.
Autoclave and agitator are that lead alloy material is made.
Owing to having adopted technique scheme, compared with prior art, the present invention adopts sulfuric acid process to process aluminous fly-ash, make the alumina leaching in aluminous fly-ash, and it is entered in solution, its digesting efficiency of alumina is up to 85～90%, for follow-up production process is got ready; The present invention is rationally utilized aluminous fly-ash, and with low cost, economical rationality, and solved the problem that equipment is corroded in stripping.The inventive method is simple, easily implements, and result of use is good.
Accompanying drawing explanation
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Embodiments of the invention 1: aluminous fly-ash sulfuric acid process dissolving-out process, the dilute sulphuric acid that the aluminous fly-ash that is 45% by the mass percentage content of aluminum oxide is 35% with mass percent concentration adopts the ratio of alumina leaching chemical reaction Theoretical Calculation amount 1.0 values to mix, and makes raw pulp A; Raw pulp A is sent in dissolving device (dissolving device comprises sleeve pipe, autoclave and flash-pot) by stripping fresh feed pump at normal temperatures, (inner tube of sleeve pipe is lead alloy inner tube first to utilize steam that 1～3 grade of sleeve pipe is heated to 88 ℃, outer tube is stainless steel tube), by 1～3 grade of sleeve pipe, raw pulp A is carried out to preheating, raw pulp A temperature after preheating reaches 85～87 ℃, obtains preheating ore pulp B; Again pass into again steam sleeve pipe is heated to 150 ℃, thereby make preheating ore pulp B be heated to 150 ℃, obtain heating ore pulp C; Again heating ore pulp C is sent into and in autoclave, be incubated stripping, under the condition of 180 ℃ of insulations, pressurize 1.0MPa, stripping 90min, in autoclave, be provided with agitator (autoclave and agitator are that lead alloy material is made), agitator is in the process of insulation stripping, maintenance is stirred heating ore pulp C, obtains stripping slurry D; Stripping slurry D is cooled to 118 ℃ through 3 grades of self-evaporatint n.s, and the secondary steam that stripping slurry D is produced through 3 grades of self-evaporatint n.s turns back in sleeve pipe, for preheating procedure, and 21 ℃ of every grade of self-evaporatint n. coolings of stripping slurry D; Stripping slurry D after cooling and the acid sludge washing lotion E that returns of acid sludge separating, washing are together sent in dilution trap, obtain temperature and be the mixed slurry F of 105 ℃, be the intermediate product that dissolving-out process obtains (mixed slurry F is mainly the acid sludge slip that alum liquor and acid sludge form).
Embodiments of the invention 2: aluminous fly-ash sulfuric acid process dissolving-out process, the dilute sulphuric acid that the aluminous fly-ash that is 40% by the mass percentage content of aluminum oxide is 38% with mass percent concentration adopts the ratio of alumina leaching chemical reaction Theoretical Calculation amount 1.0 values to mix, and makes raw pulp A; Raw pulp A is sent in dissolving device (dissolving device comprises sleeve pipe, autoclave and flash-pot) by stripping fresh feed pump at normal temperatures, (inner tube of sleeve pipe is lead alloy inner tube first to utilize steam that 1～3 grade of sleeve pipe is heated to 90 ℃, outer tube is stainless steel tube), by 1～3 grade of sleeve pipe, raw pulp A is carried out to preheating, raw pulp A temperature after preheating reaches 87 ℃, obtains preheating ore pulp B; Again pass into again steam sleeve pipe is heated to 150 ℃, thereby make preheating ore pulp B be heated to 150 ℃, obtain heating ore pulp C; Again heating ore pulp C is sent into and in autoclave, be incubated stripping, under the condition of 185 ℃ of insulations, pressurize 0.95MPa, stripping 70min, in autoclave, be provided with agitator (autoclave and agitator are that lead alloy material is made), agitator is in the process of insulation stripping, maintenance is stirred heating ore pulp C, obtains stripping slurry D; Stripping slurry D is cooled to 114 ℃ through 3 grades of self-evaporatint n.s, and the secondary steam that stripping slurry D is produced through 3 grades of self-evaporatint n.s turns back in sleeve pipe, for preheating procedure, and 21 ℃ of every grade of self-evaporatint n. coolings of stripping slurry D; Stripping slurry D after cooling and the acid sludge washing lotion E that returns of acid sludge separating, washing are together sent in dilution trap, obtain temperature and be the mixed slurry F of 100 ℃, be the intermediate product that dissolving-out process obtains.
Because aluminous fly-ash reacts with the stripping of dilute sulphuric acid for thermopositive reaction, therefore lean on their stripping reaction heat, can after raw pulp A is heated to 145～155 ℃, certainly be warmed up to 160 ℃, and proceed stripping reaction and be certainly warmed up to 180 ℃ of left and right in entering the autoclave insulation stripping tank of postorder.The inner tube of sleeve pipe is lead alloy inner tube, and lead alloy material can sulfuric acid corrosion resistant in this temperature range; Autoclave and agitator material selection lead alloy material, can prevent at high temperature etching apparatus of sulfuric acid like this; The secondary steam that utilizes flash-pot to produce carries out preheating to raw pulp, plays the object of save energy; The material of flash-pot is also selected lead alloy material.
Claims (6)
1. an aluminous fly-ash sulfuric acid process dissolving-out process, is characterized in that: aluminous fly-ash is mixed in proportion with dilute sulphuric acid, make raw pulp A; Raw pulp A is sent in dissolving device by stripping fresh feed pump at normal temperatures, by 1～3 grade of sleeve pipe, carry out preheating, the raw pulp A temperature after preheating reaches 85～90 ℃, obtains preheating ore pulp B; Sleeve pipe is heated to 145～155 ℃ again, makes preheating ore pulp B be heated to 145～155 ℃, obtain heating ore pulp C; Heating ore pulp C is sent in autoclave again and be incubated stripping, under the condition of 175～185 ℃ of insulations, pressurize 0.8～1.0MPa, stripping 60～90min, obtains stripping slurry D; Stripping slurry D is together sent in dilution trap with acid sludge washing lotion E after 3 grades of self-evaporatint n.s are cooled to 115～118 ℃, obtain temperature and be the mixed slurry F of 100～110 ℃, be the intermediate product that dissolving-out process obtains; The blending ratio of aluminous fly-ash and dilute sulphuric acid adopts the ratio of alumina leaching chemical reaction Theoretical Calculation amount 1.0 values; 20～21 ℃ of every grade of self-evaporatint n. coolings of stripping slurry D.
2. aluminous fly-ash sulfuric acid process dissolving-out process according to claim 1, is characterized in that: the mass percent concentration of dilute sulphuric acid is 25～40%.
3. aluminous fly-ash sulfuric acid process dissolving-out process according to claim 1, is characterized in that: the secondary steam that stripping slurry D is produced through 3 grades of self-evaporatint n.s turns back in sleeve pipe, for preheating procedure.
4. aluminous fly-ash sulfuric acid process dissolving-out process according to claim 1, is characterized in that: in autoclave, be provided with agitator, agitator, in the process of insulation stripping, keeps heating ore pulp C to stir.
5. aluminous fly-ash sulfuric acid process dissolving-out process according to claim 1, is characterized in that: the inner tube of sleeve pipe is lead alloy inner tube, and outer tube is stainless steel tube.
6. aluminous fly-ash sulfuric acid process dissolving-out process according to claim 4, is characterized in that: autoclave and agitator are that lead alloy material is made.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004154614A (en) * | 2002-11-01 | 2004-06-03 | Kobe Steel Ltd | Method for treating aluminum dross residual ash |
| CN1927716A (en) * | 2006-08-29 | 2007-03-14 | 吉林大学 | Preparation method of alumina |
| CN101811713A (en) * | 2009-08-21 | 2010-08-25 | 东北大学设计研究院（有限公司） | Pipeline and dwell tank desiliconization method of fly ash |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004154614A (en) * | 2002-11-01 | 2004-06-03 | Kobe Steel Ltd | Method for treating aluminum dross residual ash |
| CN1927716A (en) * | 2006-08-29 | 2007-03-14 | 吉林大学 | Preparation method of alumina |
| CN101811713A (en) * | 2009-08-21 | 2010-08-25 | 东北大学设计研究院（有限公司） | Pipeline and dwell tank desiliconization method of fly ash |
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