CN102205982B - Method for recycling acid in process of producing aluminum oxide by using fly ash acid method - Google Patents
Method for recycling acid in process of producing aluminum oxide by using fly ash acid methodDownload PDFInfo
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- CN102205982B CN102205982BCN 201110103721CN201110103721ACN102205982BCN 102205982 BCN102205982 BCN 102205982BCN 201110103721CN201110103721CN 201110103721CN 201110103721 ACN201110103721 ACN 201110103721ACN 102205982 BCN102205982 BCN 102205982B
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Abstract
Description
Technical field
The present invention relates to a kind of flyash acid system and produce the method for sour recycle in the alumina process.
Background technology
China is big coal country, with coal as the basic fuel of electrical production.The in recent years stable development of energy industry, the rapid increase that has brought the flyash quantity discharged causes huge pressure to Chinese national economy construction and ecotope.Owing to contain the valuable mineral resources such as aluminum oxide in the flyash, therefore the fine coal ashes being fully utilized, turns waste into wealth has become widely study hotspot content.Flyash extracts in the method for aluminum oxide, and acid system or using acid and alkali combination method just day by day are widely adopted because it extracts digesting efficiency of alumina height and the simple characteristics of technique.The hydrochloric acid that wherein technical process is produced carries out reusable edible research very high using value, can promote economic cycle development, realizes the efficient utilization of resource.
Acid system or using acid and alkali combination method prepare the recovery problem that unavoidably has hydrochloric acid in the alumina technology and exist from flyash.
CN1792802A discloses " a kind of method of extracting aluminum oxide from flyash ", flyash and the sulfuric acid reaction of the method after with roasting, filter, concentrate generation crystalline sulfuric acid aluminium, again generation aluminum oxide and sulfur trioxide gas are decomposed in the high-temperature calcination of crystalline sulfuric acid aluminium.
CN101234774A discloses " a kind of method that is prepared aluminum oxide by coal series kaolin rock or coal gangue ", the method is calcining and activating behind fragmentation, grinding with coal series kaolin rock or coal gangue, then generate liquor alumini chloridi with hydrochloric acid reaction, by salting-out process crystal aluminum chloride is settled out and separates, the crystal aluminum chloride calcining and decomposing generates aluminum oxide and hydrogen chloride gas.
CN1065255A discloses a kind of " technique for production of alumina by chlorhydric acid-soda method ", in the technique take hydrochloric acid as dissolution medium, ore Cheng Fenhou in small, broken bits, through high-temperature roasting, salt adding and hcl reaction in the high pressure enamel reaction still generate alkaline aluminium salt, through separating desiliconization.Alkaline aluminium salt evaporation concentration, Roasting Decomposition are made γ shape aluminum oxide and hydrogen chloride gas.Above patent is not all launched further experimental study to the acid recovery aspect, just simple the introduction.
Summary of the invention
The method that the purpose of this invention is to provide sour recycle in a kind of circulating fluid bed coal ash acid system production metallurgy grade aluminum oxide process.Method of the present invention may further comprise the steps:
1, magnetically separating and removing ion from fly ash: fluidization bed fly ash is looked its granularity, reach below 100 orders through pulverizing, adding water, to be made into solid content be that 20～40wt%, preferable range are the slurry of 30～35wt%, carry out magnetic separation at vertical ring magnetic separator, magnetic separation field intensity 1.0～2.0 ten thousand GS, preferable range are 1.5～1.75 ten thousand GS, according to the difference of iron level in the flyash, this process can repeat, until the iron oxide content in the ash is reduced to 1.0wt% following (in ferric oxide).Slurry after the magnetic separation obtains solid content after solid-liquid separation be that 25～50wt%, preferable range are the filter cake of 30～45wt%.
2, acid is molten: it is molten to place acid-resistant reacting kettle to carry out hydrochloric acid acid the filter cake after the magnetic separation, concentration of hydrochloric acid is 20～30wt%, in the hydrochloric acid in HCl and the flyash mol ratio of aluminum oxide be that 4: 1～9: 1, preferable range are 4.5: 1～6: 1, the stripping temperature is that 100 ℃～200 ℃, preferable range are 130 ℃～150 ℃, stripping pressure 0.1～2.5MPa, preferable range are 0.3～1.0MPa, and dissolution time is that 0.5h～4h, preferable range are 1.5h～2.5h; Acid is molten to obtain liquor alumini chloridi by solid-liquid separation.
3, resin absorption: liquor alumini chloridi is passed in the resin column that the macroporous type resin cation (R.C.) is housed, utilize resin that the adsorptive power of iron is carried out deironing, obtain refined crystalline aluminium chloride liquid.Treatment temp is that room temperature～90 ℃, preferable range are 60 ℃～80 ℃ during absorption, the liquor alumini chloridi flow velocity be 1～4 times of resin volume/hour, preferable range be 2～3 times of resin volumes/hour.Resin column can adopt the mode of single-column or twin columns series winding.Resin is preferably D001,732,742,7020H, 7120H, JK008 or SPC-1 resin etc.
4, condensing crystal: refined crystalline aluminium chloride liquid is-0.03 at pressure～-0.07MPa, preferable range be-0.04～-0.06MPa, temperature is that 50～110 ℃, preferable range are condensing crystal under 70～80 ℃ the condition, obtain the crystal aluminum chloride crystal, the crystal weight that concentrated time control makes accounts for 40～65% of former refined crystalline aluminium chloride liquid weight.
5, calcining: crystal aluminum chloride calcine the preparation aluminum oxide in the High Temperature Furnaces Heating Apparatus of gas concentration unit: crystal aluminum chloride is 950～1100 ℃ at 900～1200 ℃, preferable range calcined 1～4 hour, or first with crystal aluminum chloride 300～500 ℃ of thermal degradation 1～2 hour, then be warming up to 900～1200 ℃ of calcinings 1～3 hour, obtain alumina product after the thermolysis and produce hydrogen chloride gas.
6, hydrogen chloride gas is cooled to below 100 ℃ by cooling tower, enter in the acid absorption column, water flow jet speed is 100～120L/min in the control acid absorption column, carries out acid gas and tentatively reclaims.
7, the acid gas that does not absorb fully in the absorption tower is imported in the vacuum cycle acid storage tank, control its vacuum tightness and be-0.05～-0.07KPa carries out the secondary recovery of hydrochloric acid.
8, emit absorbing acid in absorption tower and the acid storage tank, add in proportion the concentrated hydrochloric acid that entry or concentration are 37wt%, regulating its concentration is 20～30wt%, returns the sour molten step in the 2nd step.
As preferred implementation, the vertical ring magnetic separator that the inventive method is used number is disclosed vertical ring magnetic separator in 201010112520.3 as Chinese patent application, and the structure of vertical ring magnetic separator comprises: change, induction medium, upper yoke, lower yoke, magnet coil, opening for feed, mine tailing bucket and flushometer.Wherein, induction medium is installed in the change, 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, described upper yoke and lower yoke are separately positioned on interior, the outer both sides of ring of ring of change below, wherein, described induction medium is the Composite Steel expanded metals, every layer of expanded metal lath weaved into by the silk stalk, the edge of described silk stalk has rib shape wedge angle, described upper yoke is connected with opening for feed, and described lower yoke is connected with the mine tailing bucket that is used for discharging, and described flushometer is positioned at the change top.
Usefulness of the present invention is that technique is simple, and production process is easy to control, production cost is low, the hydrogenchloride product reusable edible of absorption.By method of the present invention, the cyclic utilization rate of hydrogenchloride can reach more than 99.5%.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
Fig. 2 is the vertical ring magnetic separator structural representation that the present invention uses.
Embodiment
Raw material adopts certain heat power plant's output circulating fluid bed coal ash, and its chemical ingredients is as shown in table 1.
Table 1: circulating fluid bed coal ash chemical ingredients (wt%)
| SiO2 | Al2O3 | TiO2 | CaO | MgO | TFe2O3 | FeO | K2O | Na2O | LOS | SO3 | Summation |
| 34.5 | 47.28 | 1.5 | 3.59 | 0.25 | 1.57 | 0.24 | 0.41 | 0.19 | 6.77 | 1.32 | 96.3 |
The structure of vertical ring magnetic separator used in the present invention comprises:change 101,induction medium 102,upper yoke 103,lower yoke 104,magnet coil 105, opening forfeed 106,mine tailing bucket 107 and flushometer 108.Wherein,induction medium 102 is installed in thechange 101,magnet coil 105 is arranged on aroundupper yoke 103 and thelower yoke 104, so thatupper yoke 103 andlower yoke 104 become a pair of generation vertical direction field pole, describedupper yoke 103 andlower yoke 104 are separately positioned in the ring ofchange 101 belows, encircle outer both sides, wherein, describedinduction medium 102 is the Composite Steel expanded metals, every layer of expanded metal lath weaved into by the silk stalk, the edge of described silk stalk has rib shape wedge angle, describedupper yoke 103 is connected with opening forfeed 106, and describedlower yoke 104 is connected with themine tailing bucket 107 that is used for discharging, and describedflushometer 108 is positioned atchange 101 tops.
Embodiment 1
Get fluidization bed fly ash and reach 150 orders through pulverizing, add water and make the slurry that admittedly contains for 30wt%, magnetic separation on vertical ring magnetic separator, magnetic separation field intensity 1.5 ten thousand Gs, magnetic separation three times is until iron oxide content is 0.8wt% in the flyash.With the filter cake that is admittedly contained after the press filtration of plate basket pressure filter for 34.5wt%.Filter cake is put into acid-resistant reacting kettle, and it is molten that the hydrochloric acid that adds 22wt% carries out acid, in the hydrochloric acid in HCl and the ash mol ratio of aluminum oxide be 5: 1,150 ℃ of temperature of reaction, in 2 hours reaction times, reaction pressure is 1.0MPa.The molten liquor alumini chloridi that obtains of acid passed into carry out deironing in the resin column, resin column is in the single-column mode, and the resin of employing is D001 (chemical plant, Anhui Province east), and treatment temp is 60 ℃, the liquor alumini chloridi flow velocity be 3 times of resin volumes/hour.The refined crystalline aluminium chloride liquid that generates sent into carry out evaporation concentration in the concentration tank, concentrated pressure-0.05MPa, 80 ℃ of thickening temperatures, the weight of control crystal accounts for 50% of former refined crystalline aluminium chloride liquid weight, obtains crystal aluminum chloride.Crystal aluminum chloride is decomposed into aluminum oxide at 400 ℃, 2 hours resolving times, then change High Temperature Furnaces Heating Apparatus over to, and obtained alumina product in 2 hours 1100 ℃ of lower calcinings.
The hydrogen chloride gas that calcining generates cools to 98 ℃ by cooling tower, enters in the acid absorption column.Water flow jet speed is 100L/min in the control acid absorption column, carries out acid gas and tentatively reclaims.The acid gas that does not absorb fully in the absorption tower is imported in the vacuum cycle acid storage tank, control its vacuum tightness and carry out the secondary recovery of hydrochloric acid for-0.05KPa.Sour liquid-absorbing is weighed and chemical analysis, and obtaining concentration of hydrochloric acid is 23.5wt%, and the rate of recovery of hydrogenchloride is 99.65%.Emit absorbing acid in absorption tower and the acid storage tank at last, adding water, to regulate its concentration be 22wt%, returns sour molten step.
Embodiment 2
Prepare the technological condition of metallurgical-grade aluminum oxide with Circulating Fluidized Bed Ash with embodiment 1.Wherein sour molten step adding concentration of hydrochloric acid is 26.5wt%.
The hydrogen chloride gas that calcining generates cools to 90 ℃ by cooling tower, enters in the acid absorption column, and water flow jet speed is that 120L/min carries out acid gas and tentatively reclaims in the control acid absorption column.The acid gas that does not absorb fully in the absorption tower is imported in the vacuum cycle acid storage tank, control its vacuum tightness and carry out the secondary recovery of hydrochloric acid for-0.07KPa.Sour liquid-absorbing is weighed and chemical analysis, and obtaining concentration of hydrochloric acid is 26.9wt%, and the rate of recovery of hydrogenchloride is 99.75%.At last, emit absorbing acid in absorption tower and the acid storage tank, adding water, to regulate its concentration be 26.5wt%, returns sour molten step.
Embodiment 3
Prepare the technological condition of aluminum oxide with Circulating Fluidized Bed Ash with embodiment 1, wherein sour molten step adding concentration of hydrochloric acid is 30wt%.
The hydrogen chloride gas that calcining generates cools to 94 ℃ by cooling tower, enters in the acid absorption column, and water flow jet speed is that 110L/min carries out acid gas and tentatively reclaims in the control acid absorption column.The acid gas that does not absorb fully in the absorption tower is imported in the vacuum cycle acid storage tank, control its vacuum tightness and carry out the secondary recovery of hydrochloric acid for-0.06KPa.Sour liquid-absorbing is weighed and chemical analysis, and obtaining concentration of hydrochloric acid is 25.4wt%, and the rate of recovery of hydrogenchloride is 99.69%.At last, emit absorbing acid in absorption tower and the acid storage tank, it is 30wt% that the hydrochloric acid that adds concentration and be 37wt% is regulated its concentration, returns sour molten step.
Claims (18)
1. a flyash acid system is produced the method for sour recycle in the alumina process, comprising:
1), magnetically separating and removing ion from fly ash: flyash reaches below 100 orders through pulverizing, adds water and is made into the slurry that solid content is 20～40wt%, carries out magnetic separation at vertical ring magnetic separator, magnetic separation field intensity 1.0～2.0 ten thousand GS; Slurry after the magnetic separation obtains the filter cake that solid content is 25～50wt% after solid-liquid separation;
2), acid is molten: it is molten to place acid-resistant reacting kettle to carry out hydrochloric acid acid the filter cake after the magnetic separation, concentration of hydrochloric acid is 20～30wt%, in the hydrochloric acid in HCl and the flyash mol ratio of aluminum oxide be 4: 1～9: 1, the stripping temperature is 100 ° of C～200 ° C, stripping pressure 0.1～2.5MPa, dissolution time are 0.5h～4h; Acid is molten to obtain liquor alumini chloridi by solid-liquid separation;
3), resin absorption: liquor alumini chloridi is passed into deironing in the resin column that the macroporous type resin cation (R.C.) is housed, obtain refined crystalline aluminium chloride liquid, treatment temp is room temperature ~ 90 ℃, the liquor alumini chloridi flow velocity be 1～4 times of resin volume/hour; Wherein, described resin is D001,732 or 742 resins;
4), condensing crystal: refined crystalline aluminium chloride liquid is-0.03 at pressure～-0.07MPa, temperature is condensing crystal under the condition of 50～110 ° of C, obtains the crystal aluminum chloride crystal;
5), calcining: crystal aluminum chloride was calcined 1～4 hour under 900～1200 ° of C, obtained alumina product and produce hydrogen chloride gas;
6), hydrogen chloride gas is cooled to below 100 ℃ by cooling tower, enter in the acid absorption column, water flow jet speed is 100 ~ 120L/min in the control acid absorption column, carries out acid gas and tentatively reclaims;
7), unabsorbed acid gas in the absorption tower is imported in the vacuum cycle acid storage tank, control its vacuum tightness and be-0.05 ~-0.07KPa, carry out the secondary recovery of hydrochloric acid;
8), emit absorbing acid in absorption tower and the acid storage tank, add in proportion the concentrated hydrochloric acid that entry or concentration are 37wt%, regulating its concentration is 20～30wt%, returns the 2nd) step acid is molten.
2. method according to claim 1 is characterized in that, the field intensity of magnetic separation described in the step 1) is 1.5～1.75 ten thousand GS.
3. method according to claim 1 and 2 is characterized in that, after the magnetically separating and removing ion from fly ash step, the content in the ferric oxide of ferric oxide in the flyash is lower than 1.0wt%.
4. method according to claim 1 and 2, it is characterized in that, employed vertical ring magnetic separator in the magnetically separating and removing ion from fly ash step, its structure comprises: change, induction medium, upper yoke, lower yoke, magnet coil, opening for feed, mine tailing bucket and flushometer; Wherein, induction medium is installed in the change, 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, described upper yoke and lower yoke are separately positioned on interior, the outer both sides of ring of ring of change below, wherein, described induction medium is the Composite Steel expanded metals, every layer of expanded metal lath weaved into by the silk stalk, the edge of described silk stalk has rib shape wedge angle, described upper yoke is connected with opening for feed, and described lower yoke is connected with the mine tailing bucket that is used for discharging, and described flushometer is positioned at the change top.
5. method according to claim 1 is characterized in that step 2) in the hydrochloric acid in HCl and the flyash mol ratio of aluminum oxide be 4.5: 1～6: 1.
6. method according to claim 1 is characterized in that, described resin column adopts single-column or double-column series mode.
7. method according to claim 1 is characterized in that, the calcining temperature of step 5) is 950～1100 ° of C.
8. method according to claim 1 is characterized in that, step 5) be with crystal aluminum chloride 300～500 ℃ of thermal degradation 1～2 hour, then be warming up to 900～1200 ° of C calcinings 1～3 hour, obtain alumina product and produce hydrogen chloride gas.
9. method according to claim 1 is characterized in that, crystal weight is 40 ~ 65% of former refined crystalline aluminium chloride liquid weight behind the condensing crystal.
10. method according to claim 1 is characterized in that, in the step 1), flyash reaches below 100 orders through pulverizing, adds water and is made into the slurry that solid content is 30～35wt%.
11. method according to claim 1 is characterized in that, in the step 1), the slurry after the magnetic separation obtains the filter cake that solid content is 30～45wt% after solid-liquid separation.
12. method according to claim 1 is characterized in that step 2) in, the stripping temperature is 130 ° of C～150 ° C.
13. method according to claim 1 is characterized in that step 2) in, stripping pressure is 0.3～1.0MPa.
14. method according to claim 1 is characterized in that step 2) in, dissolution time is 1.5h～2.5h.
15. method according to claim 1 is characterized in that, in the step 3), treatment temp is 60 ° of C～80 ° C.
16. method according to claim 1 is characterized in that, in the step 3), the liquor alumini chloridi flow velocity be 2～3 times of resin volumes/hour.
17. method according to claim 1 is characterized in that, in the step 4), condensing crystal pressure is-0.04～-0.06MPa.
18. method according to claim 1 is characterized in that, in the step 4), the condensing crystal temperature is 70～80 ° of C.
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| CN 201110103721CN102205982B (en) | 2010-04-27 | 2011-04-25 | Method for recycling acid in process of producing aluminum oxide by using fly ash acid method |
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| CN201010161865.8 | 2010-04-27 | ||
| CN 201010161865CN101863498A (en) | 2010-04-27 | 2010-04-27 | Method for recycling acid in process of producing alumina from fly ash by acid method |
| CN 201110103721CN102205982B (en) | 2010-04-27 | 2011-04-25 | Method for recycling acid in process of producing aluminum oxide by using fly ash acid method |
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| CN102205982Btrue CN102205982B (en) | 2013-01-02 |
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| CN 201110103721ActiveCN102205982B (en) | 2010-04-27 | 2011-04-25 | Method for recycling acid in process of producing aluminum oxide by using fly ash acid method |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811712A (en) | 2010-04-27 | 2010-08-25 | 中国神华能源股份有限公司 | Method for preparing metallurgical-grade aluminum oxide by using fluid-bed fly ash |
| CN103303948A (en)* | 2012-03-16 | 2013-09-18 | 西安航天动力试验技术研究所 | Impurity removal method in process of preparing alumina from fly ash by using acid method |
| CN103449483A (en)* | 2012-05-29 | 2013-12-18 | 西安航天动力试验技术研究所 | Impurity removing method in process of preparing alumina from fly ash by utilizing acid method |
| CN103449487A (en)* | 2012-05-29 | 2013-12-18 | 西安航天动力试验技术研究所 | Impurity removing method in process of preparing alumina from fly ash by using acid method |
| CN104628019A (en)* | 2013-11-15 | 2015-05-20 | 李进凯 | Method for separating and recovering aluminum oxide form coal ash |
| 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 |
| AT515557B1 (en)* | 2014-05-28 | 2015-10-15 | Andritz Ag Maschf | Process for the preparation of packaging material |
| CN106966415A (en)* | 2017-03-29 | 2017-07-21 | 西安航天动力试验技术研究所 | The process of aluminum oxide in a kind of acidity extraction coal-powder boiler flyash |
| CN110342554A (en)* | 2018-04-03 | 2019-10-18 | 国家能源投资集团有限责任公司 | The method of flyash extraction aluminum and coproducing lithium carbonate |
| CN110963515B (en)* | 2019-12-27 | 2021-09-10 | 四川顺应动力电池材料有限公司 | Method for recovering alumina from fly ash |
| CN111620358A (en)* | 2020-05-14 | 2020-09-04 | 江西鹏腾实业有限公司 | Preparation method of high-purity white crystalline aluminum chloride |
| CN112811468B (en)* | 2020-12-25 | 2023-05-23 | 四川省绵阳市华意达化工有限公司 | Method for improving quality of chromic anhydride |
| CN119608745B (en)* | 2025-02-14 | 2025-06-17 | 鄂尔多斯市蒙泰铝业有限责任公司 | A method for recovering and recycling free acid in fly ash or coal gangue acid leaching solution |
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| 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
- 2010-04-27CNCN 201010161865patent/CN101863498A/enactivePending
- 2011
- 2011-04-25CNCN 201110103721patent/CN102205982B/enactiveActive
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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