CN112110466A - Method for removing iron impurities in fly ash and intermediate product thereof - Google Patents
Method for removing iron impurities in fly ash and intermediate product thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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Abstract
The invention belongs to the technical field of inorganic chemistry, and relates to a method for removing iron impurities in fly ash and an intermediate product thereof. The intermediate product of the method is as follows: and (3) hydrolyzing the iron-containing aluminum chloride product produced by the fly ash at low temperature to obtain an amorphous intermediate product of aluminum oxide. The invention provides a method for removing iron element in fly ash and intermediate product thereof by deep basic research and process research, which adopts a potential-controlled iron extraction technology, namely, when an iron-containing material is in acid dissolution, the potential and pH value of a solution are controlled within a certain range, so that an iron-containing phase is Fe2+The form exists stably, meanwhile, the aluminum-containing phase is ensured not to be dissolved (or dissolved in trace), and the iron content in the aluminum-containing solid phase is lower than 0.3 percent through solid-liquid separation. Through the implementation of the technical scheme of the invention, the impurity iron in the fly ash and the intermediate product can be effectively removed at low cost, the method can be used for aluminum electrolysis production, has great economic effect, and simultaneously utilizes the solidWaste and has great social benefit.
Description
Technical Field
The invention belongs to the technical field of inorganic chemistry, relates to a method for removing iron impurities in fly ash and an intermediate product thereof, and particularly relates to a method for converting different iron compounds into ferrous ions to enter a solution in the acid dissolution process of fly ash and AlCl prepared from fly ash3·6H2Removing iron impurities from an amorphous alumina intermediate product obtained after pyrolysis of an O product.
Background
A large amount of fly ash solid waste is generated in China every year and needs to be treated, wherein the content of alumina in the high-alumina fly ash is higher than 40%, and the high-alumina fly ash has great recycling value. At present, methods for producing alumina and alumina-containing intermediate products by using fly ash as a raw material exist, but a series of problems need to be solved, and for an alkaline process, the technology needs to be improved to realize solid waste reduction treatment; for the acid method, the cost of removing impurities from the acid solution is too high, and the quality of the alumina is difficult to guarantee. Particularly, the removal of impurity iron is particularly important, iron removal in the production process of the acid-process alumina at present is to dissolve iron compounds, and then remove iron ions by adopting an ion exchange method, so that the iron removal cost is relatively high; the other technology for applying the fly ash to aluminum electrolysis is to dissolve the fly ash in acid to remove iron and calcium, and an aluminum-containing phase is retained in a solid phase, and the obtained aluminum-containing solid phase extract is directly used for aluminum electrolysis to produce aluminum-silicon alloy, and the iron removal method of the technology usually adopts a goethite method to remove iron: namely, ferric iron ions are made into Fe (OH) by adjusting the pH value of the solution3Is deposited separately from the solution.The aluminum-containing minerals are partially dissolved in the acid dissolution process by adopting the goethite method, and the iron removal amount is positively correlated with the loss amount of the aluminum-containing minerals and is difficult to balance.
Disclosure of Invention
Aiming at the problems in the prior art and the requirement of low-cost iron removal of fly ash in China, the invention provides a method for removing iron element in fly ash and an intermediate product thereof through deep basic research and process research, and a potential-controlled iron extraction technology is adopted, namely when an iron-containing material is in acid dissolution, the potential and the pH value of a solution are controlled within a certain range, so that an iron-containing phase is made to be Fe2+The form exists stably, meanwhile, the aluminum-containing phase is ensured not to be dissolved (or dissolved in trace), and the iron content in the aluminum-containing solid phase is lower than 0.3 percent through solid-liquid separation. The method has the characteristics of low energy consumption and high product quality, can meet the requirements of the aluminum electrolysis industry, and has important significance for the development of the aluminum industry and the treatment of solid waste of the fly ash in China. The intermediate product of the method is as follows: and (3) hydrolyzing the iron-containing aluminum chloride product produced by the fly ash at low temperature to obtain an amorphous intermediate product of aluminum oxide.
The technical scheme provided by the invention is as follows, and the solution potentials in the invention all take the standard hydrogen electrode potential as reference:
a technical method for removing iron element impurities in fly ash or intermediate products is characterized by comprising the following steps:
(1) and (3) screening the fly ash or the intermediate product by using an abrasive material to ensure that the particle size of the material is less than 0.1mm, thereby obtaining a solid-phase material.
(2) Preparing acid solution with pH value of 0-4, preferably using one or more of hydrochloric acid, sulfuric acid and nitric acid, and H in the solution+Concentrations above 1mol/L (i.e.pH values below 0) also have an effect, except that the amount of dissolved aluminum-containing phase increases.
(3) Putting the acid solution into a dissolution tank, and mixing the acid solution and the dissolution tank according to a liquid-solid ratio of 3:1-5:1 adding solid phase materials to dissolve out iron elements in the solid phase materials. The dissolving temperature is between 20 and 100 ℃, and the selection of the dissolving temperature is related to the components of the fly ash or the intermediate product and the components of the dissolving liquid: the fly ash is preferably at 80-95 ℃, and when the activity of the fly ash is lower and the iron content is higher, a higher dissolution temperature is adopted; the intermediate product is preferably at 40 ℃ to 70 ℃, and the higher the calcination temperature and the higher the iron content in the preparation of the intermediate product, the higher the dissolution temperature is selected. The lower the pH of the acid solution used, the lower the dissolution temperature. Controlling the potential and pH value of the solution in the process of dissolution. The pH value is controlled within a range of 4 or less (preferably within a range of 0 to 4 to reduce the amount of aluminum-containing phase dissolved), and the solution potential is controlled within a range of-0.1V to 0.6V.
The dissolution time is 10 minutes to 60 minutes, and is related to the content and phase composition of iron in the raw material, the dissolution time is longer when the content of iron is high or impurities are more, and is also related to the type and dosage of a reducing agent, the dissolution time is shorter when the dosage of the reducing agent is more, the granularity is small, the reducibility is strong, and the dissolution time is longer in the opposite case. In addition, when the solution potential is controlled by the current-carrying electrode, the dissolution time required is also long.
(4) Filtering to separate, wherein pH value of the solution is not more than 4 (preferably 0-4 to reduce the dissolved amount of aluminum-containing phase), solution potential is controlled between 0V-0.3V, and then washing the solid phase material with acid solution (preferably one or more of hydrochloric acid, nitric acid, and sulfuric acid) with pH of 0-4 to ensure that aluminum-containing phase in the solid phase is not substantially dissolved and residual Fe2+Not left in the solid phase. The solid phase material can meet the requirement after 2 times of washing. The filtered liquid phase can be reused in the step (3) after iron removal treatment.
The method for adjusting and controlling the solution potential in the step (3) comprises the following steps: the addition of a metal reducing agent or the control of an electrified electrode may be used in combination of both methods.
If the method of adding the metal reducing agent is adopted independently, the addition amount is Fe3+Reduction to Fe2+By chemical reaction of (e.g. 2 Fe)3++Fe＝3Fe2+,2Fe3++Zn＝2Fe2++Zn2+The addition amount is equal to or more than all Fe in the solid-phase material3+Complete reduction to Fe2+The theoretical value required. Part of the metal reducing agent may cause hydrogen gas to be evolved from the solution, and in order to minimize the amount of hydrogen evolved, it is preferable to control the amount of hydrogen evolved in the eluted solutionThe prepared pH value and solution potential range are not contacted with H+Reducing agents for the reaction, such as iron, zinc, tin, and the like.
The invention controls the potential control range of the solution to be-0.1V-0.6V, the pH value of the solution is preferably 0-4, and the iron element in the fly ash and the intermediate product thereof is dissolved out. The acid dissolution process carried out in the range leads to the dissolution of iron-containing compounds in the fly ash or amorphous alumina intermediate product, and ferric iron is converted into ferrous ions under the control of the external potential and is dissolved in an acid solution for stable existence. Meanwhile, in the pH control range, the divalent iron ions can not be precipitated (while the trivalent iron can be precipitated in the pH range). Thus, by simultaneously controlling the potential and pH of the solution during digestion, the iron in the fly ash or intermediate will be present in the solution as ferrous ions, while the aluminum-containing phase is substantially insoluble and stable in the solid phase in this controlled region. After the iron-containing compound is dissolved out, the solid-liquid mixture is filtered and separated, and then the separation of iron and aluminum-containing phases can be realized. The invention can also be carried out with a pH of less than 0, which ensures that the ferrous ions do not precipitate, but that the aluminium-containing phase is somewhat dissolved.
The pH value of the solution is less than or equal to 4 during filtration, and the potential is controlled between 0V and 0.3V, so as to ensure that ferrous ions in the solution are not oxidized into ferric ions during filtration.
During dissolution and filtration, the lower the pH value of the solution is, the larger the upper limit of the controlled solution potential is, because the lower the pH value is, the less the precipitation of iron hydroxide is, therefore, when the pH value is lower, the potential control range of the solution can be relaxed, and the upper limit is increased; on the contrary, if the pH is higher, the solution potential range needs to be strictly controlled, and the upper limit is lowered, so as to avoid the iron from precipitating into the solid phase.
The invention has the beneficial effects that: by implementing the technical scheme of the invention, the impurity iron in the fly ash and the intermediate product can be effectively removed at low cost, the method can be used for aluminum electrolysis production, has great economic effect, and simultaneously utilizes solid wastes, thereby having great social benefit.
The invention has the following advantages: as for the technology for preparing the aluminum-silicon alloy by electrolyzing the fly ash extract, the iron impurities in the fly ash and the aluminum chloride raw material produced by the fly ash hydrochloric acid method can be removed to the level of 0.3 percent with lower cost. The obtained aluminum chloride with low iron content or aluminum oxide products obtained by further processing the aluminum chloride can meet the requirements of aluminum electrolysis raw materials. Meanwhile, by adopting the method to remove iron, the dissolution loss rate of aluminum in the aluminum chloride raw material is less than 5 percent and is lower than the loss rate of nearly 20 percent in the prior art. For the intermediate product, the iron removal cost of the existing ion exchange method is high, and the technology can reduce the iron removal cost by more than 50 percent, and has obvious cost advantage.
Detailed Description
The fly ash (containing 2.73% of iron) adopted by the embodiment comes from a certain power generation enterprise in inner Mongolia, and AlCl3·6H2The O crystal (containing 0.63 percent of iron) comes from a product produced by treating the high-alumina fly ash by a hydrochloric acid method by another enterprise.
Example 1
500 g of the fly ash is taken and sieved by an abrasive for standby. Preparing a 1mol/L concentration acid solution by using industrial hydrochloric acid for later use according to a liquid-solid ratio of 3:1, the dissolution equipment adopts a self-made reactor, the dissolution temperature is 95 ℃, 20 g of iron particles (with the diameter of 2mm) are weighed and mixed with the materials, the mixture is added into an acid solution, the mixture is stirred at a low speed for 30 minutes, a pH value probe is adopted to monitor the pH value of the solution on line, a potentiometer is adopted to monitor the potential of the solution, the pH value is about 0, and the potential is between 0.1 and 0.2V. Then solid-liquid separation is carried out on a filter press, the residual iron particles are separated out, the solid-phase filter cake is washed twice by dilute hydrochloric acid with the pH value of 0.5, and the iron content in the solid obtained by drying is 0.0192%. The dissolution loss of aluminum was 4.82%.
Example 2
1000 g of the fly ash is taken and sieved by an abrasive for standby. Preparing 0.5mol/L concentration acid solution by using industrial nitric acid for later use according to a liquid-solid ratio of 5:1, the dissolution equipment adopts a self-made reactor, the dissolution temperature is 75 ℃, 40 g of iron particles (with the diameter of 2mm) are weighed and mixed with the materials, the mixture is added into an acid solution, the mixture is stirred at a low speed for 20 minutes, a pH value probe is adopted to monitor the pH value of the solution on line, a potentiometer is adopted to monitor the potential of the solution, the pH value is about 0.5, and the potential is between 0.1 and 0.4V. And then performing solid-liquid separation on a filter press, separating out the residual iron particles, washing the solid-phase filter cake twice by using dilute nitric acid with the pH value of 1, and drying to obtain a solid with the iron content of 0.0273%. The dissolution loss of aluminum was 3.57%.
Example 3
1000 g of the fly ash is taken and sieved by an abrasive for standby. Preparing 0.05mol/L acid solution by using industrial sulfuric acid for later use according to a liquid-solid ratio of 3:1, the dissolution equipment adopts a self-made reactor, the dissolution temperature is 90 ℃, 20 g of zinc particles and materials are weighed and mixed to be added into an acid solution, the stirring is carried out at a low speed for 40 minutes, a pH value probe is adopted to monitor the pH value of the solution on line, a potentiometer is adopted to monitor the potential of the solution, the pH value is about 1, and the potential is between-0.10V and 0.15V. Then, solid-liquid separation was performed on a filter press, the solid-phase filter cake was washed twice with a dilute sulfuric acid having a pH of 2, and the iron content in the dried solid was 0.0239%. The dissolution loss of aluminum was 4.12%.
Example 4
Taking the AlCl3·6H21000 g of O crystals were hydrolyzed at 450 ℃ for 5 hours under an air atmosphere to obtain 252 g of an alumina intermediate. Preparing 0.1mol/L acid solution by using industrial hydrochloric acid for later use according to a liquid-solid ratio of 5:1, the dissolution equipment adopts a self-made reactor, the dissolution temperature is 55 ℃, 20 g of iron particles (with the diameter of 2mm) are weighed and mixed with the materials, the mixture is added into an acid solution, the mixture is stirred at a low speed for 20 minutes, a pH value probe is adopted to monitor the pH value of the solution on line, a potentiometer is adopted to monitor the potential of the solution, the pH value is about 1, and the potential is between 0.1 and 0.2V. Then solid-liquid separation is carried out on a filter press, the residual iron particles are separated out, the solid-phase filter cake is washed twice by dilute hydrochloric acid with the pH value of 3, and the iron content in the solid obtained by drying is 0.0139%. The dissolution loss of aluminum was 1.52%.
Example 5
Taking the AlCl3·6H21000 g of O crystals were hydrolyzed at 450 ℃ for 5 hours under an air atmosphere to obtain 252 g of an alumina intermediate. Preparing 0.01mol/L concentration acid solution by using industrial nitric acidLiquid is reserved, and the ratio of liquid to solid is 5:1, the dissolution equipment adopts a self-made reactor, the dissolution temperature is 45 ℃, 20 g of iron particles (with the diameter of 2mm) are weighed and mixed with the materials, the mixture is added into an acid solution, the mixture is stirred at a low speed for 20 minutes, a pH value probe is adopted to monitor the pH value of the solution on line, a potentiometer is adopted to monitor the potential of the solution, the pH value is about 2, and the potential is between 0.1 and 0.4V. Then, solid-liquid separation was performed on a filter press, the remaining iron particles were separated, the solid-phase cake was washed twice with a dilute hydrochloric acid having a pH of 4, and the iron content in the dried solid was 0.0252%. The dissolution loss of aluminum was 0.88%.
Example 6
Taking the AlCl3·6H21000 g of O crystals were hydrolyzed at 450 ℃ for 5 hours under an air atmosphere to obtain 252 g of an alumina intermediate. Preparing an acid solution with pH of 4 by using industrial sulfuric acid for later use, wherein the pH value is as follows according to a liquid-solid ratio of 3:1, taking out, wherein a self-made reactor is adopted as a dissolving-out device, the dissolving-out temperature is 80 ℃, 15 g of zinc particles and materials are weighed and mixed to be added into an acid solution, stirring is carried out at a low speed for 30 minutes, a pH value probe is adopted to monitor the pH value of the solution on line, a potentiometer is adopted to monitor the potential of the solution, the pH value is about 4, and the potential is between-0.05V and 0.15V. Then solid-liquid separation is carried out on a filter press, the solid-phase filter cake is washed twice by dilute sulphuric acid with pH 4, and the iron content in the solid obtained by drying is 0.0132%. The dissolution loss of aluminum was 1.31%.
Example 7
Taking the AlCl3·6H21000 g of O crystals were hydrolyzed at 450 ℃ for 5 hours under an air atmosphere to obtain 252 g of an alumina intermediate. Preparing 0.1mol/L acid solution by using industrial hydrochloric acid for later use according to a liquid-solid ratio of 5:1, the dissolution is carried out by adopting a self-made reactor, the dissolution temperature is 50 ℃, two steel plate electrodes are placed in the solution, a fast graphite electrode is inserted between the steel plate electrodes, the periphery of the graphite electrode is isolated and sealed by a cation membrane, the steel plate is used as a cathode, the graphite electrode is used as an anode, and the electrolysis is carried out by electrifying, so that the potential of the cathode steel plate can be controllably adjusted between-0.1V and 0.6V. The time is 60 minutes, the pH value of the solution is monitored on line by a pH value probe, and the pH value is changed between 0 and 1. Then solid-liquid separation is carried out on a filter press, and the residue is leftSeparating out the rest iron particles, washing the solid-phase filter cake twice with dilute hydrochloric acid with pH 4, and drying to obtain solid with iron content of 0.0108%. The dissolution loss of aluminum was 0.67%.
Claims (10)
1. A method for removing iron impurities in fly ash and an intermediate product thereof is characterized in that the intermediate product is an amorphous alumina intermediate product obtained by low-temperature hydrolysis of an iron-containing aluminum chloride product produced from fly ash, and the method comprises the following steps:
(1) screening the fly ash or the intermediate product by using an abrasive material to obtain a solid material, wherein the particle size of the solid material is less than 0.1 mm;
(2) preparing an acid solution with the pH value less than or equal to 4;
(3) putting an acid solution into a dissolution tank, adding the solid material according to a liquid-solid ratio of 3:1-5:1, and dissolving out iron element in the solid material at a temperature of 20-100 ℃, wherein the standard electrode potential of the solution is controlled to be-0.1V-0.6V, the pH value of the solution is controlled to be less than or equal to 4, and the dissolution time is 10-60 min;
(4) filtering and separating, wherein the pH value of the solution is controlled to be less than or equal to 4 during filtering, and the standard electrode potential of the solution is controlled to be between 0V and 0.3V; washing the solid phase substance after filtration with acid solution with pH value of 0-4.
2. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 1, wherein the pH value of the acid solution in the step (2) is 0-4; controlling the pH value of the solution in the step (3) to be in the range of 0-4; and (4) controlling the pH value of the solution to be 0-4 during filtering in the step (4).
3. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 1 or 2, wherein the acid solution in the step (2) is one or more of hydrochloric acid solution, sulfuric acid solution and nitric acid solution; and (3) the acid solution for washing in the step (4) is one or more of a hydrochloric acid solution, a sulfuric acid solution and a nitric acid solution.
4. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 1 or 2, wherein when the solid material added in the step (3) is fly ash, the dissolution temperature is 80-95 ℃; when the solid material added in the step (3) is the intermediate product, the dissolution temperature is 40-70 ℃.
5. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 1 or 2, wherein the leaching in step (3) and the filtering in step (4) are performed in such a way that the lower the pH value of the solution, the larger the upper limit of the standard electrode potential control range of the solution.
6. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 1 or 2, wherein the method for controlling the solution potential in step (3) is one of or both of adding a powered electrode control and adding a metal reducing agent control.
7. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 6, wherein the metal reducing agent is one or more of Fe, Zn and Sn.
8. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 6 or 7, wherein when the method for controlling the solution potential in the step (3) is controlled by adding the metal reducing agent, the amount of the metal reducing agent is more than or equal to the amount of all Fe in the solid material3+Complete reduction to Fe2+The theoretical value required.
9. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 8, wherein when the method for controlling the solution potential in the step (3) is the addition of the metal reducing agent, the amount of the metal reducing agent is controlled so as to remove all Fe in the solid material3+Complete reduction to Fe2+The theoretical value required.
10. The method for removing iron impurities in fly ash and intermediate products thereof as claimed in claim 1 or 2, wherein the liquid obtained after filtering in step (4) is subjected to iron removal treatment and then is repeatedly used in step (3).
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| CN114455618A (en) * | 2022-03-15 | 2022-05-10 | 吉林大学 | Method for preparing low-sodium low-iron superfine alpha-alumina and large-pore-volume pseudo-boehmite |
| CN114477256A (en) * | 2022-03-15 | 2022-05-13 | 吉林大学 | Method for producing low-sodium low-iron composite gamma-alumina and co-producing ammonium chloride |
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| CN114455618A (en) * | 2022-03-15 | 2022-05-10 | 吉林大学 | Method for preparing low-sodium low-iron superfine alpha-alumina and large-pore-volume pseudo-boehmite |
| CN114477256A (en) * | 2022-03-15 | 2022-05-13 | 吉林大学 | Method for producing low-sodium low-iron composite gamma-alumina and co-producing ammonium chloride |
| CN114477257A (en) * | 2022-03-15 | 2022-05-13 | 吉林大学 | Method for preparing low-sodium low-iron aluminum hydroxide flame retardant and co-producing ammonium chloride by using circulating fluidized bed fly ash |
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