CN114604882A - Method for producing alumina by using fly ash and recycling auxiliary materials - Google Patents
Method for producing alumina by using fly ash and recycling auxiliary materials Download PDFInfo
- Publication number
- CN114604882A CN114604882A CN202210408872.6A CN202210408872A CN114604882A CN 114604882 A CN114604882 A CN 114604882A CN 202210408872 A CN202210408872 A CN 202210408872A CN 114604882 A CN114604882 A CN 114604882A
- Authority
- CN
- China
- Prior art keywords
- fly ash
- aluminum
- reaction
- nitric acid
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/24—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with nitric acid or nitrogen oxides
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/22—Inorganic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/27—Ammonia
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for producing alumina by using fly ash and recycling auxiliary materials, belonging to the field of fly ash resource utilization; the method comprises the following steps: s1, adding water into the fly ash, grinding, and selecting carbon in a flotation mode to obtain fly ash tailing slurry; s2, adding water to prepare slurry, then carrying out pressure leaching reaction, and filtering to obtain filtrate and silicon dioxide slag; s3, adding an adsorbent to perform iron removal reaction to obtain an iron-removed aluminum nitrate solution; s4, adding ammonia water to adjust the pH value to 5-8, and performing primary aluminum precipitation to obtain aluminum hydroxide and filtrate; s5, roasting the aluminum hydroxide to obtain an aluminum oxide product; s6, adjusting the pH value of the filtrate S4 to 9-12, and performing secondary calcium and magnesium precipitation to obtain calcium and magnesium slag and an ammonium nitrate solution; and S7, performing membrane electrolysis on the ammonium nitrate solution to obtain nitric acid and ammonia water, and recycling. The method has the advantages of low acid consumption, low impurity content of the leachate, low impurity removal cost, regeneration and recycling of acid and alkali double mediums and simple process.
Description
Technical Field
The invention relates to the technical field of fly ash resource utilization, in particular to a method for producing alumina by using fly ash and recycling auxiliary materials.
Background
At present, coal is still used in thermal power generation and heating plants in the north of China, and a large amount of fly ash is generated. The fly ash is widely applied to the industrial fields of construction, building materials, metallurgy, chemical industry, environmental protection, backfill, high-performance ceramic materials and the like, and can also be applied to the agricultural fields of soil improvement, field building and the like. The fly ash contains a large amount of alumina, silicon dioxide, iron, gallium, germanium and other rare metals, and the aluminum resource of China is very short, so that the resource utilization of the fly ash has important research significance and wide market prospect.
The method for extracting alumina from fly ash can be divided into acid method and alkali method. The alkaline recovery process is mature, but the process flow is long and the recovery cost is high. The acid method comprises a hydrochloric acid method and a sulfuric acid method at present, the content of iron in the fly ash is high, the fly ash is directly leached by acid in the existing acid method recovery process, almost all iron in the fly ash enters a leaching solution, the acid consumption is high, the leaching cost is high, the content of iron impurities in the leaching solution is high, and the impurity removal cost is high. In addition, in the hydrochloric acid leaching process, the hydrochloric acid is volatile, the equipment is seriously corroded, and particularly, special materials are needed for pressure leaching equipment, so the investment cost is high; the sulfuric acid method adopted for leaching has the defects of high leaching temperature, high pressure, high safety requirement of leaching equipment and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method which has low requirement on equipment, can realize the production utilization of calcium, magnesium, aluminum and silicon in fly ash, achieves high utilization rate of raw materials, particularly has high aluminum recovery rate and high purity, can realize the resource utilization of calcium and magnesium, and has small slag amount; the ammonia water and the nitric acid used in the invention can be recycled, and the recyclability of raw materials and auxiliary materials is realized.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for producing alumina by using fly ash and recycling auxiliary materials comprises the following steps:
s1, adding water into the fly ash, grinding to obtain ore pulp, and selecting carbon from the ore pulp in a flotation mode to obtain fly ash tailing pulp;
s2, adding water into the fly ash tailing slurry for slurrying, adding nitric acid for mixing, performing pressure leaching reaction, and filtering to obtain filtrate and silicon dioxide slag; the mass ratio of the fly ash tailing slurry to the water is 2-5: 1; the mass percentage concentration of the nitric acid is 20-60%, and the adding amount of the nitric acid is 1.0-1.8 times of the theoretical value of the acid consumption of the aluminum in the fly ash tailing slurry; the conditions of the pressure leaching reaction include: the reaction temperature is 120 ℃ and 190 ℃, the reaction pressure is 0.2-2.5MPa, the reaction time is 1-3h, and the stirring speed is 50-500 rpm;
s3, adding an adsorbent into the filtrate to perform iron removal reaction, filtering after full reaction to obtain an iron-removed aluminum nitrate solution and a used adsorbent, adding acid into the used adsorbent to regenerate and recover iron and gallium;
s4, adding ammonia water into the aluminum nitrate solution to adjust the pH value to 5-8, carrying out primary aluminum precipitation, fully reacting, and filtering to obtain aluminum hydroxide and a filtrate; the conditions of the one-section aluminum precipitation comprise: the temperature is 40-100 ℃, and the time is 0.5-3.5 h;
s5, washing the aluminum hydroxide for multiple times and then roasting to obtain an aluminum oxide product;
s6, adjusting the pH of the filtrate obtained in the step S4 to 9-12 by adopting ammonium bicarbonate, performing secondary calcium and magnesium precipitation, fully reacting, and filtering to obtain calcium and magnesium slag and an ammonium nitrate solution; the conditions for secondary calcium and magnesium precipitation comprise: the temperature is 40-100 ℃, and the time is 0.5-3.5 h;
and S7, electrolyzing the ammonium nitrate solution by adopting a membrane to obtain nitric acid and ammonia water, and respectively returning to the step S2 and the step S4 for recycling.
Preferably, in S1, the grinding is carried out to ensure that the granularity is below 100 meshes, and the water is used in an amount to ensure that the mass percentage concentration of the ore pulp is 15-45%.
Wherein, preferably, the water is used in an amount that the mass percentage concentration of the ore pulp is 15-20%.
Wherein, in S2, the mass ratio of the fly ash tailing slurry to the water is preferably 3-4: 1; the mass percentage concentration of the nitric acid is 20-30%, and the adding amount of the nitric acid is 1.0-1.2 times of the theoretical value of the acid consumption of the aluminum in the fly ash tailing slurry.
Wherein, preferably, in S2, the pressure leaching reaction conditions include: the reaction temperature is 150-190 ℃, the reaction pressure is 0.3-0.8MPa, the reaction time is 1-3h, and the stirring speed is 400-500 rpm.
Preferably, in S3, the adsorbent is PXS, which is a commercially available product and is not described herein again.
Wherein, preferably, the iron removal reaction conditions comprise: the temperature is 50-75 ℃ and the time is 1-3 h.
Wherein, preferably, the conditions of the one-section aluminum deposition comprise: the temperature is 60-80 ℃ and the time is 1-2 h.
Wherein, preferably, the secondary calcium and magnesium precipitation conditions comprise: the temperature is 60-70 ℃ and the time is 1-2.5 h.
Wherein, preferably, the method further comprises: the flotated carbon in S1 is used as fuel for steam generation for project heating.
Wherein, in S7, the membrane electrolysis is preferably carried out so that the mass concentration of the obtained nitric acid is 10-30% and the mass concentration of the ammonia water is 5-15%.
The technical scheme of the invention has the following beneficial effects:
in the scheme, the steps are mutually cooperated, and particularly, the impurities can be efficiently leached one by one according to a specific sequence under respective proper conditions, so that the aluminum can be recovered to the maximum extent, the utilization rate of raw materials is high, particularly, the recovery rate and the purity of the aluminum are high, the calcium and the magnesium are recycled, and the slag amount is small; the ammonia water and the nitric acid used in the invention can be recycled, and the recyclability of raw materials and auxiliary materials is realized. The method has the advantages of low acid consumption, low impurity content of the leachate, low impurity removal cost, regeneration and recycling of acid and alkali double mediums, low requirement on equipment, simple process and the like.
Drawings
FIG. 1 is a flow chart of a specific process of the present invention.
Detailed Description
In the present invention, the percentage contents are by mass unless otherwise specified.
The invention provides a method for producing alumina by using fly ash and recycling auxiliary materials, which comprises the following steps:
s1, adding water into the fly ash, grinding to obtain ore pulp, and selecting carbon from the ore pulp in a flotation mode to obtain fly ash tailing pulp;
s2, adding water into the fly ash tailing slurry for slurrying, adding nitric acid for mixing, performing pressure leaching reaction, and filtering to obtain filtrate and silicon dioxide slag;
the mass ratio of the fly ash tailing slurry to the water is 2-5: 1; the mass percentage concentration of the nitric acid is 20-60%, and the adding amount of the nitric acid is 1.0-1.8 times of the theoretical value of the acid consumption of the aluminum in the fly ash tailing slurry; the conditions of the pressure leaching reaction include: the reaction temperature is 120 ℃ and 190 ℃, the reaction pressure is 0.2-2.5MPa, the reaction time is 1-3h, and the stirring speed is 50-500 rpm;
s3, adding an adsorbent into the filtrate to perform iron removal reaction, filtering after full reaction to obtain an iron-removed aluminum nitrate solution and a used adsorbent, adding acid into the used adsorbent to regenerate and recover iron and gallium;
s4, adding ammonia water into the aluminum nitrate solution to adjust the pH value to 5-8, performing primary aluminum precipitation, fully reacting, and filtering to obtain aluminum hydroxide and a filtrate; the conditions of the one-section aluminum precipitation comprise: the temperature is 40-100 ℃, and the time is 0.5-3.5 h;
s5, washing the aluminum hydroxide for multiple times and then roasting to obtain an aluminum oxide product; preferably, the conditions of the calcination include: the temperature is 950 ℃ and 1050 ℃, and the time is 1-3 h.
S6, adjusting the pH of the filtrate obtained in the step S4 to 9-12 by adopting ammonium bicarbonate, performing secondary calcium and magnesium precipitation, fully reacting, and filtering to obtain calcium and magnesium slag and an ammonium nitrate solution; the secondary calcium and magnesium precipitation conditions comprise: the temperature is 40-100 ℃, and the time is 0.5-3.5 h;
and S7, electrolyzing the ammonium nitrate solution by adopting a membrane to obtain nitric acid and ammonia water, and respectively returning to the step S2 and the step S4 for recycling.
The method of the invention can fully improve the recovery rate of aluminum, can recycle auxiliary materials, has low acid consumption, low impurity content of the leachate, low impurity removal cost, low requirement on equipment, simple process and the like, and has the advantages of regeneration and recycling of acid-base double mediums.
Preferably, in S1, the grinding is carried out to ensure that the granularity is below 100 meshes, and the water is used in an amount to ensure that the mass percentage concentration of the ore pulp is 15-45%.
More preferably, the water is used in an amount such that the pulp has a mass percentage concentration of 15-20%. The preferred scheme is more beneficial to the subsequent maximum floating of carbon.
Wherein, in S2, the mass ratio of the fly ash tailing slurry to the water is preferably 3-4: 1; the mass percentage concentration of the nitric acid is 20-30%, and the adding amount of the nitric acid is 1.0-1.2 times of the theoretical value of the acid consumption of the aluminum in the fly ash tailing slurry. The preferred scheme is more beneficial to leaching silicon to the maximum extent and obtaining filtrate containing aluminum.
Wherein, preferably, in S2, the pressure leaching reaction conditions include: the reaction temperature is 150-190 ℃, the reaction pressure is 0.3-0.8MPa, the reaction time is 1-3h, and the stirring speed is 400-500 rpm. The preferred scheme is more beneficial to leaching silicon to the maximum extent and obtaining filtrate containing aluminum.
Wherein, in S3, the adsorbent is PXS.
Wherein, preferably, the iron removal reaction conditions comprise: the temperature is 50-75 ℃ and the time is 1-3 h. The preferable scheme is more beneficial to adsorbing and tapping iron to the maximum extent.
Wherein, preferably, the conditions of the one-section aluminum deposition comprise: the temperature is 60-80 ℃, and the time is 1-2 h. This preferred embodiment is more favorable for maximum precipitation of aluminum.
Wherein, preferably, the secondary calcium and magnesium precipitation conditions comprise: the temperature is 60-70 ℃ and the time is 1-2.5 h. The preferred scheme is more favorable for precipitating calcium and magnesium to the maximum extent.
Wherein, preferably, the method further comprises: the flotated carbon in S1 is used as fuel for steam generation for project heating.
Wherein, in S7, the membrane electrolysis is preferably carried out so that the mass concentration of the obtained nitric acid is 10-30% and the mass concentration of the ammonia water is 5-15%.
The skilled person can control the conditions of the membrane electrolysis by including: the concentration of the ammonium nitrate, the temperature of the electrolytic cell and the current intensity are used for adjusting the concentration of the nitric acid and the ammonia water which are required to be obtained.
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Example 1
A method for producing alumina by using fly ash and recycling auxiliary materials is shown in figure 1 and comprises the following steps:
(1) adding water into fly ash, grinding the fly ash to be less than 100 meshes to obtain ore pulp, wherein the mass percentage concentration of the ore pulp is 15%, floating carbon in the ore pulp to obtain fly ash tailing pulp, and the mass fraction of chemical elements of the fly ash tailing comprises: fe is 1.85%; 19.19% of Al; the Si content is 27%; ca is 4.55%; mg is 0.56%; ga is 160 g/t.
(2) And adding water into the fly ash tailing slurry for slurrying, then carrying out nitric acid pressure leaching reaction, and filtering to obtain an aluminum nitrate solution and silicon dioxide slag. The nitric acid pressure leaching conditions comprise: the mass ratio of the fly ash tailing slurry to water is 4:1, the mass percentage concentration of nitric acid is 20%, the adding amount of nitric acid is 1.1 times of the theoretical value of the acid consumption of aluminum in the fly ash tailing slurry, the leaching temperature is 150 ℃, the stirring speed is 500rpm, the leaching time is 1h, and the pressure is increased to 0.3 MPa. The recovery rate of the silicon dioxide is 61 percent, and the mass fraction of chemical elements of the silicon dioxide slag (by-product) comprises the following components: fe is 0.94%; al is 4.12%; si is 29.92%; ca is 0.30%; mg is 0.13%.
(3) Adding an adsorbent PXS into the filtrate, reacting for 1h at 60 ℃, and filtering to obtain an iron-removed aluminum nitrate solution;
(4) and adding ammonia water into the aluminum nitrate solution for primary aluminum precipitation, fully reacting, and filtering to obtain aluminum hydroxide and filtrate. The first-stage aluminum precipitation adjustment comprises the following steps: the pH value of the end point is controlled to be 5.0, the temperature of the precipitation reaction is 60 ℃, and the reaction time is 1 h. Washing aluminum hydroxide for multiple times, and roasting at 1000 ℃ for 2h to obtain aluminum oxide, wherein the aluminum oxide comprises the following chemical elements in percentage by mass: fe is 0.087%; al is 52.35%; si is 0.01%; na is 0.05%. The aluminum recovery was 92%.
(5) And (3) adjusting the pH of the filtrate by ammonium bicarbonate (ammonium bicarbonate) to precipitate calcium and magnesium at a second stage, fully reacting, and filtering to obtain calcium and magnesium slag and an ammonium nitrate solution. The secondary aluminum precipitation adjustment comprises the following steps: the pH value of the end point is controlled to be 10.0, the temperature of the precipitation reaction is 60 ℃, and the reaction time is 1 h.
(6) And (3) electrolyzing the ammonium nitrate solution by adopting a membrane, and controlling the concentration of ammonium nitrate, the temperature of an electrolytic bath and the current intensity to obtain nitric acid with the concentration of 15% and ammonia water with the concentration of 10%.
Example 2
A method for producing alumina by using fly ash and recycling auxiliary materials comprises the following steps:
(1) adding water into fly ash, grinding the fly ash to be less than 100 meshes to obtain ore pulp, wherein the mass percentage concentration of the ore pulp is 20%, floating carbon in the ore pulp to obtain fly ash tailing pulp, and the mass fraction of chemical elements of the fly ash tailing comprises: fe is 1.93%; 19.37 percent of Al; si is 28.1%; ca is 5.78%; mg is 0.54%; ga is 160 g/t.
(2) And adding water into the fly ash tailing slurry for slurrying, then carrying out nitric acid pressure leaching reaction, and filtering to obtain an aluminum nitrate solution and silicon dioxide slag. The nitric acid pressure leaching conditions comprise: the mass ratio of the fly ash tailing slurry to water is 3:1, the mass percentage concentration of nitric acid is 30%, the adding amount of nitric acid is 1.2 times of the theoretical value of the acid consumption of the fly ash tailing aluminum, the leaching temperature is 170 ℃, the stirring speed is 500rpm, the leaching time is 2h, and the pressure is increased to 0.5 MPa. The recovery rate of the silicon dioxide is 55 percent, and the mass fraction of the chemical elements of the silicon dioxide byproduct comprises the following components: fe is 0.52%; 3.64 percent of Al; the Si content is 30.87%; ca is 0.21%; mg is 0.11%.
(3) Adding an adsorbent PXS into the filtrate, reacting for 1h at 70 ℃, and filtering to obtain an iron-removed aluminum nitrate solution;
(4) and adding ammonia water into the aluminum nitrate solution for primary aluminum precipitation, fully reacting, and filtering to obtain aluminum hydroxide and filtrate. The first-stage aluminum precipitation adjustment comprises the following steps: the pH value of the end point is controlled to be 6.0, the temperature of the precipitation reaction is 80 ℃, and the reaction time is 2 hours. Washing aluminum hydroxide for multiple times, and roasting at 1000 ℃ for 2h to obtain aluminum oxide, wherein the aluminum oxide comprises the following chemical elements in percentage by mass: fe is 0.027%; 52.16% of Al; si is 0.01%; na is 0.04%. The aluminum recovery was 93%.
(5) And adjusting the pH of the filtrate by ammonium bicarbonate, precipitating calcium and magnesium in a second stage, fully reacting, and filtering to obtain calcium and magnesium slag and an ammonium nitrate solution. The secondary aluminum precipitation adjustment comprises the following steps: the pH value of the end point is controlled to be 11.0, the temperature of the precipitation reaction is 65 ℃, and the reaction time is 1 h.
(6) And (3) electrolyzing the ammonium nitrate solution by adopting a membrane, and controlling the concentration of ammonium nitrate, the temperature of an electrolytic bath and the current intensity to obtain nitric acid with the concentration of 15% and ammonia water with the concentration of 10%.
Example 3
A method for producing alumina by using fly ash and recycling auxiliary materials comprises the following steps:
(1) adding water into fly ash, grinding the fly ash to be less than 100 meshes to obtain ore pulp, wherein the mass percentage concentration of the ore pulp is 15%, floating carbon in the ore pulp to obtain fly ash tailing pulp, and the mass fraction of chemical elements of the fly ash tailing comprises: fe is 1.85%; 19.19% of Al; 27 percent of Si; ca is 4.55%; mg is 0.56%; ga is 160 g/t.
(2) And adding water into the fly ash tailing slurry for slurrying, then carrying out nitric acid pressure leaching reaction, and filtering to obtain an aluminum nitrate solution and silicon dioxide slag. The nitric acid pressure leaching conditions comprise: the mass ratio of the fly ash tailing slurry to water is 4:1, the mass percentage concentration of nitric acid is 30%, the adding amount of nitric acid is 1.0 time of the theoretical value of the acid consumption of aluminum in the fly ash tailing, the leaching temperature is 190 ℃, the stirring speed is 500rpm, the leaching time is 3h, and the pressure is increased to 0.8 MPa. The recovery rate of the silicon dioxide is 51 percent, and the mass fraction of the chemical element components of the silicon dioxide byproduct comprises: fe is 0.24%; al is 2.07%; si is 32.56%; 0.15 percent of Ca; mg is 0.08%.
(3) Adding an adsorbent A into the filtrate, reacting for 2 hours at 70 ℃, and filtering to obtain an iron-removed aluminum nitrate solution;
(4) and adding ammonia water into the aluminum nitrate solution for primary aluminum precipitation, fully reacting, and filtering to obtain aluminum hydroxide and filtrate. The first-stage aluminum precipitation adjustment comprises the following steps: the pH value of the end point is controlled to be 7.0, the temperature of the precipitation reaction is 75 ℃, and the reaction time is 2 hours. Washing aluminum hydroxide for multiple times, and roasting at 1000 ℃ for 2h to obtain aluminum oxide, wherein the aluminum oxide comprises the following chemical elements in percentage by mass: fe is 0.012%; al is 52.87%; si is 0.01%; na is 0.03%. The aluminum recovery was 93.8%.
(5) And adjusting the pH of the filtrate by ammonium bicarbonate, precipitating calcium and magnesium in a second stage, fully reacting, and filtering to obtain calcium and magnesium slag and an ammonium nitrate solution. The secondary aluminum precipitation adjustment comprises the following steps: the pH value of the end point is controlled to be 11.0, the temperature of the precipitation reaction is 75 ℃, and the reaction time is 1 h.
(6) And (3) electrolyzing the ammonium nitrate solution by adopting a membrane, and controlling the concentration of ammonium nitrate, the temperature of an electrolytic bath and the current intensity to obtain nitric acid with the concentration of 20% and ammonia water with the concentration of 12%.
Example 4
The procedure is as in example 3, except that the one-stage aluminum precipitation temperature is 100 ℃.
The recovery of aluminum in this example was 85% and the Al content in the alumina was 48%.
Example 5
The procedure is as in example 3, except that the period of time for the precipitation of aluminum is 3.2 hours.
The recovery of aluminum in this example was 86% and the Al content in the alumina was 49%.
While the foregoing is directed to the preferred embodiment of the present invention, it will be appreciated by those skilled in the art that various changes and modifications may be made therein without departing from the principles of the invention as set forth in the appended claims.
Claims (10)
1. A method for producing alumina by using fly ash and recycling auxiliary materials is characterized by comprising the following steps:
s1, adding water into the fly ash, grinding to obtain ore pulp, and selecting carbon from the ore pulp in a flotation mode to obtain fly ash tailing pulp;
s2, adding water into the fly ash tailing slurry for slurrying, adding nitric acid for mixing, performing pressure leaching reaction, and filtering to obtain filtrate and silicon dioxide slag;
wherein the mass ratio of the fly ash tailing pulp to the water is 2-5: 1; the mass percentage concentration of the nitric acid is 20-60%, and the adding amount of the nitric acid is 1.0-1.8 times of the theoretical value of the acid consumption of the aluminum in the fly ash tailing slurry; the conditions of the pressure leaching reaction include: the reaction temperature is 120 ℃ and 190 ℃, the reaction pressure is 0.2-2.5MPa, the reaction time is 1-3h, and the stirring speed is 50-500 rpm;
s3, adding an adsorbent into the filtrate to perform iron removal reaction, filtering after full reaction to obtain an iron-removed aluminum nitrate solution and a used adsorbent, adding acid into the used adsorbent to regenerate and recover iron and gallium;
s4, adding ammonia water into the aluminum nitrate solution to adjust the pH value to 5-8, performing primary aluminum precipitation, fully reacting, and filtering to obtain aluminum hydroxide and a filtrate; the conditions of the one-section aluminum precipitation comprise: the temperature is 40-100 ℃, and the time is 0.5-3.5 h;
s5, washing the aluminum hydroxide for multiple times and then roasting to obtain an aluminum oxide product;
s6, adjusting the pH of the filtrate obtained in the step S4 to 9-12 by adopting ammonium bicarbonate, performing secondary calcium and magnesium precipitation, fully reacting, and filtering to obtain calcium and magnesium slag and an ammonium nitrate solution; the secondary calcium and magnesium precipitation conditions comprise: the temperature is 40-100 ℃, and the time is 0.5-3.5 h;
and S7, electrolyzing the ammonium nitrate solution by adopting a membrane to obtain nitric acid and ammonia water, and respectively returning to the step S2 and the step S4 for recycling.
2. The method of claim 1, wherein in S1, the grinding is performed to make the particle size below 100 meshes, and the water is used to make the mass percentage concentration of the ore pulp be 15-45%.
3. The method according to claim 2, characterized in that in S1, the water is used in an amount to make the pulp have a mass concentration of 15-20%.
4. The method according to claim 1, wherein in S2, the mass ratio of the fly ash tailing slurry to the water is 3-4: 1; the mass percentage concentration of the nitric acid is 20-30%, and the adding amount of the nitric acid is 1.0-1.2 times of the theoretical value of the acid consumption of the aluminum in the fly ash tailing slurry.
5. The method of claim 1, wherein in S2, the conditions of the pressure leaching reaction include: the reaction temperature is 150-190 ℃, the reaction pressure is 0.3-0.8MPa, the reaction time is 1-3h, and the stirring speed is 400-500 rpm.
6. The method according to claim 1, wherein, in S3,
the adsorbent is PXS;
the iron removal reaction conditions comprise: the temperature is 50-75 ℃ and the time is 1-3 h.
7. The method of claim 1, wherein the conditions for the length of aluminum deposition comprise: the temperature is 60-80 ℃ and the time is 1-2 h.
8. The method of claim 1, wherein the secondary calcium and magnesium precipitation conditions comprise: the temperature is 60-70 ℃ and the time is 1-2.5 h.
9. The method of claim 1, further comprising: the flotated carbon in S1 is used as fuel for steam generation for project heating.
10. The method according to claim 1, wherein in S7, the membrane electrolysis is performed so that the mass concentration of the obtained nitric acid is 10-30% and the mass concentration of the obtained ammonia water is 5-15%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210408872.6A CN114604882A (en) | 2022-04-19 | 2022-04-19 | Method for producing alumina by using fly ash and recycling auxiliary materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210408872.6A CN114604882A (en) | 2022-04-19 | 2022-04-19 | Method for producing alumina by using fly ash and recycling auxiliary materials |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114604882A true CN114604882A (en) | 2022-06-10 |
Family
ID=81868459
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210408872.6A Pending CN114604882A (en) | 2022-04-19 | 2022-04-19 | Method for producing alumina by using fly ash and recycling auxiliary materials |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114604882A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB139470A (en) * | 1920-02-19 | 1921-03-10 | Det Norske Aktieselskab | Improvements in or relating to the removal of iron from solutions of aluminium nitrate sulphate or chloride |
| FR1324189A (en) * | 1962-06-05 | 1963-04-12 | Anaconda Co | Alumina production process |
| JPS5973434A (en) * | 1982-10-20 | 1984-04-25 | Agency Of Ind Science & Technol | Method for purifying aluminum salt |
| CN88103282A (en) * | 1987-06-02 | 1988-12-21 | 皮奇尼铅公司 | The method of extraction and gallium-purifying from Bayer-liquid |
| CN101863500A (en) * | 2010-06-04 | 2010-10-20 | 中南大学 | Method for producing alumina with aluminum-containing metallurgical material |
| RU2574247C1 (en) * | 2014-10-06 | 2016-02-10 | Общество с ограниченной ответственностью "НьюКем Текнолоджи" | Method for processing alumina-containing raw material and method for opening alumina-containing raw material in processing thereof |
| KR20190131724A (en) * | 2018-05-17 | 2019-11-27 | 한국알루미나 주식회사 | Preparation method of high purity alumina |
| CN113582213A (en) * | 2021-07-26 | 2021-11-02 | 四川顺应动力电池材料有限公司 | Method for comprehensively utilizing fly ash |
-
2022
- 2022-04-19 CN CN202210408872.6A patent/CN114604882A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB139470A (en) * | 1920-02-19 | 1921-03-10 | Det Norske Aktieselskab | Improvements in or relating to the removal of iron from solutions of aluminium nitrate sulphate or chloride |
| FR1324189A (en) * | 1962-06-05 | 1963-04-12 | Anaconda Co | Alumina production process |
| JPS5973434A (en) * | 1982-10-20 | 1984-04-25 | Agency Of Ind Science & Technol | Method for purifying aluminum salt |
| CN88103282A (en) * | 1987-06-02 | 1988-12-21 | 皮奇尼铅公司 | The method of extraction and gallium-purifying from Bayer-liquid |
| CN101863500A (en) * | 2010-06-04 | 2010-10-20 | 中南大学 | Method for producing alumina with aluminum-containing metallurgical material |
| RU2574247C1 (en) * | 2014-10-06 | 2016-02-10 | Общество с ограниченной ответственностью "НьюКем Текнолоджи" | Method for processing alumina-containing raw material and method for opening alumina-containing raw material in processing thereof |
| KR20190131724A (en) * | 2018-05-17 | 2019-11-27 | 한국알루미나 주식회사 | Preparation method of high purity alumina |
| CN113582213A (en) * | 2021-07-26 | 2021-11-02 | 四川顺应动力电池材料有限公司 | Method for comprehensively utilizing fly ash |
Non-Patent Citations (2)
| Title |
|---|
| 刘延红等: ""酸性体系中镓回收工艺技术"", 《轻金属》, no. 6, pages 20 - 24 * |
| 王丽萍;李超;郭昭华;王永旺;陈东;: "酸浸法生产氧化铝过程除铁技术新进展", 无机盐工业, no. 09 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102206755B (en) | Method for separating and recovering valuable elements from neodymium-iron-boron wastes | |
| CN101817561B (en) | Method for pollution-free production of sodium chromate by pressure leaching of chromite | |
| CN114105171B (en) | Method for comprehensively utilizing lepidolite resources and lithium hydroxide prepared by method | |
| CN112939046A (en) | Comprehensive recycling method of coal-based solid waste | |
| CA2808627C (en) | Processing of manganous sulphate/dithionate liquors | |
| CN102586606A (en) | Method for recovering rare earth, vanadium and nickel from waste FCC/ROC catalyst containing vanadium and nickel | |
| CN110066920B (en) | Method for selectively leaching and separating vanadium and iron from stone coal vanadium ore | |
| CN101450814A (en) | Novel method for extracting vanadic anhydride from stone coal vanadium ore | |
| CN101956070A (en) | Recovery method of molybdenum concentrates | |
| CN113292057B (en) | Recovery method of waste lithium iron phosphate battery | |
| CN106745128A (en) | A kind of method of aluminium lime-ash removal of impurities | |
| CN111172390B (en) | Method for treating valuable metal sulfide concentrate by using oxygen pressure | |
| CN113279048A (en) | Method for preparing high-purity iron phosphate from iron-containing slag | |
| CN113582213A (en) | Method for comprehensively utilizing fly ash | |
| CN110972479B (en) | Method for producing zinc oxide by twice leaching method | |
| CN114920245A (en) | Mineralized substance for carbon dioxide sequestration and application thereof | |
| CN115286019A (en) | Method for producing high-purity lithium carbonate from spodumene | |
| CN109721081B (en) | Method for extracting lithium from lithium-rich fly ash alkaline mother liquor | |
| CN113512652B (en) | Method for extracting gallium metal from coal-series solid waste | |
| CN212532311U (en) | System for gangue production aluminium oxide | |
| CN111777087A (en) | System and method for producing alumina from coal gangue | |
| CN109182868B (en) | Low-impurity vanadium-aluminum alloy and preparation method thereof | |
| CN113735179B (en) | Method for preparing high-purity ferric sulfate by utilizing ferro-manganese | |
| CN114604882A (en) | Method for producing alumina by using fly ash and recycling auxiliary materials | |
| CN110817930A (en) | Method for producing zinc ammonium carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |