CN102145906B - Method for preparing low-iron aluminum chloride crystals by using fly ash as raw material - Google Patents
Method for preparing low-iron aluminum chloride crystals by using fly ash as raw material Download PDFInfo
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- CN102145906B CN102145906B CN2011101037546A CN201110103754A CN102145906B CN 102145906 B CN102145906 B CN 102145906B CN 2011101037546 A CN2011101037546 A CN 2011101037546A CN 201110103754 A CN201110103754 A CN 201110103754A CN 102145906 B CN102145906 B CN 102145906B
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 144
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000013078 crystal Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 40
- 239000010881 fly ash Substances 0.000 title claims abstract description 36
- 239000002994 raw material Substances 0.000 title abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 238000007885 magnetic separation Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- 239000012065 filter cake Substances 0.000 claims description 14
- 238000005554 pickling Methods 0.000 claims description 14
- 239000006148 magnetic separator Substances 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 230000006698 induction Effects 0.000 claims description 6
- 230000008719 thickening Effects 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 235000021110 pickles Nutrition 0.000 abstract 3
- 238000000227 grinding Methods 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- 238000011017 operating method Methods 0.000 description 15
- 239000010883 coal ash Substances 0.000 description 13
- 239000012530 fluid Substances 0.000 description 9
- 238000001914 filtration Methods 0.000 description 7
- 238000003828 vacuum filtration Methods 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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- Compounds Of Iron (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for preparing low-iron aluminium chloride crystals by using fly ash as a raw material, which comprises the following steps of: (1) grinding the fly ash and carrying out wet magnetic separation to remove iron; (2) performing a reaction on the fly ash subjected to iron removal and hydrochloric acid to obtain pickle liquor; (3) carrying out decompressing concentration on the pickle liquor, and cooling and crystallizing the obtained pickle liquor to obtain slurry of aluminium chloride crystals; and (4) carrying out solid-liquid separation on the slurry of the aluminium chloride crystals, leaching with leacheate and carrying out solid-liquid separation and drying to obtain low-iron aluminium chloride crystal products. The method has the advantages of wide raw material resources, low cost, simple operation steps, easily controlled production process, stable production quality and the like. The content of iron (Fe) in the aluminium chloride crystal products obtained by the method is not higher than 0.025 percent by weight.
Description
Technical field
The present invention relates to a kind of method for preparing crystal aluminum chloride, especially a kind of is the method for the low iron crystal aluminum chloride of feedstock production with flyash.
Background technology
Flyash is the waste that the coal-burning power plant discharges; China is to be the country of main energy sources with coal; Annual flyash from power plant emission is up to more than one hundred million tons; A large amount of soils are are not only occupied in the discharging of flyash, and serious environment pollution, how to handle and utilize flyash to become an important problems.On the other hand; Contain multiple utilizable component in the flyash, research shows, contains the aluminium (in aluminum oxide) of 30-50% in the circulating fluid bed coal ash usually; In resource deficient day by day today; From flyash, extract aluminium, the preparation crystal aluminum chloride is the effective way that makes flyash turn waste into wealth, fully utilize, and has good social benefit and economic benefit.
At present, the preparation method of low iron crystal aluminum chloride normally to be raw material through white lake or aluminum oxide after the deironing, makes with hydrochloric acid reaction, and its raw material sources are single, and production cost is high.And with flyash be raw material directly the crystal aluminum chloride of preparation contain impurity such as iron usually, be difficult to remove with general method.
It is the method for feedstock production crystal aluminum chloride with the circulating fluid bed coal ash that CN200710055504.3 discloses a kind of; This method adopts the technology that directly acid is dissolved from circulating fluid bed coal ash, to make liquor alumini chloridi; Slag liquid is separated obtain supernatant; After the supernatant concentration crystallization, further make solid crystal aluminum chloride product through spraying drying again.Because the iron in the flyash very easily is dissolved in acid, and in the method, therefore the measure of the deironing that there is no need can cause the iron-holder in the product crystal aluminum chloride high, and the existence meeting of iron has a negative impact to the physics and the chemical property of crystal aluminum chloride product.
Still flyash direct production of no use is hanged down the method for iron crystal aluminum chloride at present, and therefore, being necessary to design a kind of is the method for the low iron crystal aluminum chloride of feedstock production with flyash, so that overcome above-mentioned defective.
Summary of the invention
The objective of the invention is to deficiency to above-mentioned prior art, to provide a kind of be the method for the low iron crystal aluminum chloride of feedstock production with flyash.
Provided by the present invention is the method for the low iron crystal aluminum chloride of feedstock production with flyash, may further comprise the steps:
(1) flyash is crushed to below 100 orders, adds water and be made into the slurry that solid content is 20-40wt%, after wet magnetic separation deironing and solid-liquid separation, obtain filter cake;
(2) adding hydrochloric acid in step (1) the gained filter cake is carried out acid and dissolve, after solid-liquid separation and washing, obtain pickling liquor again;
(3) concentrating under reduced pressure is carried out in the gained pickling liquor to step (2), and the liquid after concentrating obtains the crystal aluminum chloride slurries through cooling crystallization;
(4) step (3) gained crystal aluminum chloride slurries are carried out solid-liquid separation, use leacheate drip washing, after solid-liquid separation and drying, obtain low iron crystal aluminum chloride product again.
Following further explain method provided by the present invention, but therefore the present invention does not receive any restriction.
Step (1): flyash is crushed to below 100 orders; Adding water, to be made into solid content be 20-40wt%; The slurry of preferred 30-35wt%; The iron oxide content (in red oxide of iron) that carries out in magnetic separation to the flyash through magnetic separator is reduced to below the 1.0wt%, and obtaining solid content through solid-liquid separation is 25-50wt%, the filter cake of preferred 30-45wt%.
Said magnetic separator can be selected the various magnetic plants that are suitable for the opaque Material deironing commonly used for use.Preferably, said magnetic separator is applied for the disclosed vertical-ring magnetic separator that is used for deferrization of pulverized coal ash in No. 201010112520.3 for China's invention, and this magnetic separator comprises: change, induction medium, upper yoke, lower yoke, magnet coil, opening for feed, mine tailing bucket and flushometer; Induction medium is installed in the change, and magnet coil is arranged on around upper yoke and the lower yoke, so that upper yoke and lower yoke become a pair of generation vertical direction field pole; Said upper yoke and lower yoke are separately positioned on interior, the outer both sides of ring of ring of change below; Wherein, said induction medium is the Composite Steel expanded metals, and every layer of XPM weaved into by the silk stalk; The edge of said silk stalk has rib shape wedge angle; Said upper yoke is connected with opening for feed, and said lower yoke is connected with the mine tailing bucket that is used for discharging, and said flushometer is positioned at the change top.
The magnetic separation condition of said vertical-ring magnetic separator is: field intensity 1.0-2.0 ten thousand GS, preferred 1.5-1.75 ten thousand GS, electric current 30-40A.
Said magnetic separation process can repeat 2-4 time, preferred 2-3 time.
Step (2): with adding concentration in step (1) the gained filter cake is 20-37wt%, and it is molten that the hydrochloric acid of preferred 20-30wt% carries out acid, in the hydrochloric acid in HCl and the flyash mol ratio of aluminum oxide be 4: 1-9: 1; Preferred 4.5: 1-6: 1, stripping temperature is 100-200 ℃; Preferred 130-150 ℃, stripping pressure are 0.1-2.5MPa, and preferred 0.3-1.0MPa, dissolution time are 0.5-4.0h, preferred 1.5-2.5h; Through solid-liquid separation and washing, obtain pickling liquor again.
Said pickling liquor pH value is preferably 1-3.
Said solid-liquid separation can adopt any solid-liquid separating method commonly used, for example, uses sedimentation, filtration under diminished pressure, and pressure filtration all can.
Conventional washing methods is adopted in said washing, and water washs sour molten slag.Said washing process can repeat more than 2 or 2 times, for example 2-4 time, to sour molten slag near neutrality till, for example, the pH value of sour molten slag is about 5-6.
Step (3): concentrating under reduced pressure is carried out in the gained pickling liquor to step (2); Concentrating pressure is-0.03--0.07MPa, and preferred-0.04--0.06MPa, thickening temperature is 50-110 ℃, preferred 70-80 ℃; Liquid after concentrating is separated out crystal aluminum chloride through cooling, obtains the crystal aluminum chloride slurries.
Said step (3) is in when cooling, the crystal weight that control is separated out account for the former weight of aluminum chloride liquid 40% to 65% between, make most of aluminum chloride crystallization separate out, and impurity such as a small amount of iron(ic)chloride are still stayed in the middle of the solution because concentration is lower.
Step (4): step (3) gained crystal aluminum chloride slurries are carried out solid-liquid separation; After removing most of moisture content; Carry out the impurity such as iron(ic)chloride that the crystal aluminum chloride surface adhesion is removed in drip washing with leacheate, carry out solid-liquid separation once more, after drying, obtain low iron crystal aluminum chloride product.Residue mother liquor after the solid-liquid separation returns step (3) condensing crystal again.
The compound method of leacheate is in the said step (4): will hang down the iron crystal aluminum chloride and at room temperature be dissolved in the water, and be mixed with saturated liquor alumini chloridi.Said low iron crystal aluminum chloride is preferably the low iron crystal aluminum chloride for preparing through the inventive method.
Said step (4) is when drip washing, and the consumption of leacheate is a 50-300 milliliter per kilogram crystal aluminum chloride, preferred 100-200 milliliter per kilogram crystal aluminum chloride.
Said solid-liquid separation and drying can adopt the routine operation method, use spinning or vacuum belt filter, and drying temperature is preferably 70-100 ℃.
Compared with prior art, the beneficial effect that the present invention had is:
1, adopting circulating fluid bed coal ash is the feedstock production crystal aluminum chloride, and raw material sources are extensive, and cost is low.From this trade waste of flyash, extract crystal aluminum chloride product, have good economic benefits and social benefit with high added value.
2, method that temperature (100-200 ℃) acid is dissolved in the employing is extracted aluminium from flyash, high to the extraction yield of aluminium, reach more than 80%, and the raw material availability height, the level of residue of generation is little.
3, the method that adopts magnetic separation, crystallization, drip washing to combine realizes the removal of iron, and this method operation steps is simple, and production process is easy to control, good iron removal effect.
4, the resulting crystal aluminum chloride product of the present invention, its iron (Fe) content is not higher than 0.025wt%.
Embodiment
Pass through embodiment further explain method provided by the present invention below, but therefore the present invention does not receive any restriction.
Raw material adopts the circulating fluid bed coal ash of certain heat power plant's output, and its chemical ingredients is as shown in table 1.
Table 1 circulating fluid bed coal ash chemical ingredients (wt%)
| SiO 2 | Al 2O 3 | TiO 2 | CaO | MgO | Fe 2O 3 | FeO | K 2O | Na 2O | LOS | SO 3 | Summation |
| 34.70 | 46.28 | 1.48 | 3.61 | 0.21 | 1.54 | 0.22 | 0.39 | 0.17 | 7.17 | 1.32 | 95.77 |
Embodiment 1
(1) gets the fluid bed powder coal ash and be crushed to 200 orders; Add water and process the slurry that solid content is 33wt%; Use in No. 201010112520.3, China's invention application the magnetic separation 3 times under 1.2 ten thousand GS of the disclosed vertical-ring magnetic separator that is used for deferrization of pulverized coal ash; Iron oxide content in the flyash is reduced to 0.8wt%, with plate basket pressure filter (Henan Yu Zhou pressure filter factory, model: BAS320) obtain the filter cake that solid content is 37.5wt% after the press filtration;
(2) filter cake is put into acid-resistant reacting kettle; The technical hydrochloric acid that adds concentration and be 28wt% carries out acid and dissolves and react, in the hydrochloric acid in HCl and the flyash mol ratio of aluminum oxide be 4.5: 1,150 ℃ of stripping temperature; Stripping pressure 1.0MPa; Dissolution time 2h, reaction product obtains pH value and is 1.5 pickling liquor after the press filtration of above-mentioned plate basket pressure filter, washing;
(3) concentrating under reduced pressure is carried out in pickling liquor; Concentrating pressure is-0.05MPa, 90 ℃ of thickening temperatures, and the liquid after concentrating at room temperature naturally cooling is separated out crystal aluminum chloride; Obtain the aluminum chloride slurries, the crystal weight that control is separated out accounts for 40% of the former weight of aluminum chloride liquid.
(4) the aluminum chloride slurries are carried out vacuum filtration after, carry out drip washing by the per kilogram crystal aluminum chloride with 150 milliliters leacheate, and carry out vacuum filtration once more rapidly, after 70 ℃ of dryings, obtain low iron crystal aluminum chloride product.
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.023wt%.
Embodiment 2
Except that step (1), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (1) is adjusted into:
(1) gets the fluid bed powder coal ash and be crushed to 300 orders; Add water and process the slurry that solid content is 35wt%; Use in No. 201010112520.3, China's invention application the magnetic separation 4 times under 1.75 ten thousand GS of the disclosed vertical-ring magnetic separator that is used for deferrization of pulverized coal ash; Iron oxide content in the flyash is reduced to 0.5wt%, with plate basket pressure filter (Henan Yu Zhou pressure filter factory, model: BAS320) obtain the filter cake that solid content is 38wt% after the press filtration;
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.020wt%.
Embodiment 3
Except that step (1), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (1) is adjusted into:
(1) gets the fluid bed powder coal ash and be crushed to 200 orders; Add water and process the slurry that solid content is 30wt%; Use in No. 201010112520.3, China's invention application the magnetic separation 2 times under 2.0 ten thousand GS of the disclosed vertical-ring magnetic separator that is used for deferrization of pulverized coal ash; Iron oxide content in the flyash is reduced to 0.7wt%, with plate basket pressure filter (Henan Yu Zhou pressure filter factory, model: BAS320) obtain the filter cake that solid content is 35wt% after the press filtration;
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.022wt%.
Embodiment 4
Except that step (2), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (2) is adjusted into:
(2) filter cake is put into acid-resistant reacting kettle; Adding concentration is that the technical hydrochloric acid of 36wt% carries out the molten reaction of acid, and the mol ratio of aluminum oxide is 5: 1 in hydrochloric acid and the flyash, 200 ℃ of stripping temperature; Stripping pressure 2.1MPa; Dissolution time 2h, reaction product obtains pH value and is 1.5 pickling liquor after the press filtration of above-mentioned plate basket pressure filter, washing;
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.021wt%.
Embodiment 5
Except that step (2) and (3), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in step (2) and (3) is adjusted into respectively:
(2) filter cake is put into acid-resistant reacting kettle; Adding concentration is that the technical hydrochloric acid of 22wt% carries out the molten reaction of acid, and the mol ratio of aluminum oxide is 6: 1 in hydrochloric acid and the flyash, 110 ℃ of stripping temperature; Stripping pressure 0.2MPa; Dissolution time 2h, reaction product obtains pH value and is 1.4 pickling liquor after the press filtration of above-mentioned plate basket pressure filter, washing;
(3) concentrating under reduced pressure is carried out in pickling liquor; Concentrating pressure is-0.03MPa, 75 ℃ of thickening temperatures, and the liquid after concentrating at room temperature naturally cooling is separated out crystal aluminum chloride; Obtain the crystal aluminum chloride slurries, the crystal that control is separated out accounts for 65% of the former weight of aluminum chloride liquid.
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.025wt%.
Embodiment 6
Except that step (3), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (3) is adjusted into:
(3) pickling liquor is sent into carried out evaporation concentration in the glass lining concentration tank; Pressure-0.04MPa when concentrating, 70 ℃ of thickening temperatures, the liquid after concentrating is naturally cooling at room temperature; Obtain rough crystal aluminum chloride slurries, the crystal that control is separated out accounts for 50% of the former weight of aluminum chloride liquid.
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.024wt%.
Embodiment 7
Except that step (4), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (4) is adjusted into:
(4) the aluminum chloride slurries are carried out vacuum filtration after, carry out drip washing by the per kilogram crystal aluminum chloride with 300 milliliters leacheate, and carry out vacuum filtration once more rapidly, after 70 ℃ of dryings, obtain low iron crystal aluminum chloride product.
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.019wt%.
Contrast experiment's example 1
Omit step (1), other operating procedure condition is all identical with embodiment 1, and directly acid is molten without magnetic separation to be about to flyash, the preparation crystal aluminum chloride.
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.041wt%.
Contrast experiment's example 2
Omit the lessivation in the step (4), other operating procedure condition is all identical with embodiment 1, and promptly the operating procedure condition in the step (4) is adjusted into:
(4) the aluminum chloride slurries are directly carried out vacuum filtration after, after 70 ℃ of dryings, obtain low iron crystal aluminum chloride product.
Through measuring, the content of iron in the crystal aluminum chloride product (Fe) is 0.037wt%.
Claims (14)
1. one kind is the method for the low iron crystal aluminum chloride of feedstock production with flyash, may further comprise the steps:
(1) flyash is crushed to below 100 orders, adds water and be made into the slurry that solid content is 20-40wt%, after iron removal by magnetic separation and solid-liquid separation, obtain filter cake;
(2) adding hydrochloric acid in step (1) the gained filter cake is carried out acid and dissolve, after solid-liquid separation and washing, obtain pickling liquor again;
(3) concentrating under reduced pressure is carried out in the gained pickling liquor to step (2), and the liquid after concentrating obtains the crystal aluminum chloride slurries through cooling crystallization;
(4) step (3) gained crystal aluminum chloride slurries are carried out solid-liquid separation, use leacheate drip washing, after solid-liquid separation and drying, obtain low iron crystal aluminum chloride product again,
It is molten that the hydrochloric acid that adds concentration in the wherein said step (2) and be 20-37wt% carries out acid, in the hydrochloric acid in HCl and the flyash mol ratio of aluminum oxide be that 4.5:1-6:1, stripping temperature are that 130-150 ℃, stripping pressure are that 0.3-1.0MPa, dissolution time are 1.5-2.5h.
2. method according to claim 1 is characterized in that, said step (1) is reduced to below the 1.0wt% through the iron oxide content that magnetic separator carries out in magnetic separation to the flyash, obtains the filter cake that solid content is 25-50wt% through solid-liquid separation.
3. method according to claim 2 is characterized in that, in the said step (1), obtains the filter cake that solid content is 30-45wt% through solid-liquid separation.
4. method according to claim 2 is characterized in that, said magnetic separator is a vertical-ring magnetic separator; Comprise: change, induction medium, upper yoke, lower yoke, magnet coil, opening for feed, mine tailing bucket and flushometer, induction medium is installed in the change, and magnet coil is arranged on around upper yoke and the lower yoke; So that upper yoke and lower yoke become a pair of generation vertical direction field pole, said upper yoke and lower yoke are separately positioned on interior, the outer both sides of ring of ring of change below, wherein; Said induction medium is the Composite Steel expanded metals; Every layer of XPM weaved into by the silk stalk, and the edge of said silk stalk has rib shape wedge angle, and said upper yoke is connected with opening for feed; Said lower yoke is connected with the mine tailing bucket that is used for discharging, and said flushometer is positioned at the change top.
5. method according to claim 4 is characterized in that, the magnetic separation condition of said vertical-ring magnetic separator is: field intensity 1.0-2.0 ten thousand GS.
6. method according to claim 5 is characterized in that, said field intensity is 1.5-1.75 ten thousand GS.
7. according to claim 1 or 5 described methods, it is characterized in that it is molten that the hydrochloric acid that adds concentration in the said step (2) and be 20-30wt% carries out acid.
8. method according to claim 7 is characterized in that, obtains the pickling liquor of pH value for 1-3 in the said step (2).
9. according to claim 1 or 8 described methods, it is characterized in that concentrating pressure in the said step (3) is-0.03--0.07MPa that thickening temperature is 50-110 ℃.
10. method according to claim 9 is characterized in that, concentrating pressure in the said step (3) is-0.04--0.06MPa that thickening temperature is 70-80 ℃.
11. method according to claim 9 is characterized in that, said step (3) is in when cooling, the crystal weight that control is separated out account for the former weight of aluminum chloride liquid 40% to 65% between.
12., it is characterized in that the compound method of leacheate is in the said step (4): will hang down the iron crystal aluminum chloride and at room temperature be dissolved in the water, and be mixed with saturated liquor alumini chloridi according to claim 1 or 11 described methods.
13., it is characterized in that the consumption of leacheate is a 50-300 milliliter per kilogram crystal aluminum chloride in the said step (4) according to each described method among the claim 1-6,8 or 11.
14. method according to claim 13 is characterized in that, the consumption of leacheate is a 100-200 milliliter per kilogram crystal aluminum chloride in the said step (4).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101037546A CN102145906B (en) | 2010-04-27 | 2011-04-25 | Method for preparing low-iron aluminum chloride crystals by using fly ash as raw material |
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| CN201010161827.2 | 2010-04-27 | ||
| CN 201010161827 CN101838003A (en) | 2010-04-27 | 2010-04-27 | Method for preparing low-ferrum crystalline aluminium chloride from coal ash |
| CN2011101037546A CN102145906B (en) | 2010-04-27 | 2011-04-25 | Method for preparing low-iron aluminum chloride crystals by using fly ash as raw material |
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| CN102145906A CN102145906A (en) | 2011-08-10 |
| CN102145906B true CN102145906B (en) | 2012-10-17 |
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| CN 201010161827 Pending CN101838003A (en) | 2010-04-27 | 2010-04-27 | Method for preparing low-ferrum crystalline aluminium chloride from coal ash |
| CN2011101037546A Active CN102145906B (en) | 2010-04-27 | 2011-04-25 | Method for preparing low-iron aluminum chloride crystals by using fly ash as raw material |
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| CN103738990B (en) * | 2013-12-17 | 2015-09-09 | 中国神华能源股份有限公司 | A kind of method utilizing crystal aluminum chloride to produce aluminum oxide |
| CN103803617B (en) * | 2013-12-30 | 2016-03-16 | 中国神华能源股份有限公司 | A kind of flyash acid system produces the method for aluminum oxide |
| CN105347380A (en) * | 2015-10-29 | 2016-02-24 | 长安大学 | Spraying method for removing iron |
| CN105540632A (en) * | 2015-12-21 | 2016-05-04 | 华东理工常熟研究院有限公司 | Method for purifying crystalline aluminum chloride |
| CN113292088B (en) * | 2021-05-19 | 2023-04-14 | 神华准能资源综合开发有限公司 | Method for producing low-magnesium and low-calcium alumina from crystalline aluminum chloride |
| CN115007321A (en) * | 2022-03-31 | 2022-09-06 | 神华准能资源综合开发有限公司 | Method for recovering carbon from gangue acid leaching residue |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4652433A (en) * | 1986-01-29 | 1987-03-24 | Florida Progress Corporation | Method for the recovery of minerals and production of by-products from coal ash |
| CN201179479Y (en) * | 2008-04-03 | 2009-01-14 | 抚顺隆基磁电设备有限公司 | Vertical revolving ring induction type wet strong magnetic separator |
-
2010
- 2010-04-27 CN CN 201010161827 patent/CN101838003A/en active Pending
-
2011
- 2011-04-25 CN CN2011101037546A patent/CN102145906B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4652433A (en) * | 1986-01-29 | 1987-03-24 | Florida Progress Corporation | Method for the recovery of minerals and production of by-products from coal ash |
| CN201179479Y (en) * | 2008-04-03 | 2009-01-14 | 抚顺隆基磁电设备有限公司 | Vertical revolving ring induction type wet strong magnetic separator |
Non-Patent Citations (1)
| Title |
|---|
| 刀正超.浅谈强磁选机感应介质几何形状、单元尺寸对选别指标的影响.《云南冶金》.1982,(第5期),34页右栏第3-15行. * |
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| CN102145906A (en) | 2011-08-10 |
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