CN113321229A - Process for producing corundum phase alumina by adopting secondary aluminum ash - Google Patents
Process for producing corundum phase alumina by adopting secondary aluminum ash Download PDFInfo
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Abstract
The invention relates to the technical field of secondary aluminum ash treatment, in particular to a process for producing corundum phase aluminum oxide by using secondary aluminum ash. The process provided by the invention comprises the following steps: mixing the secondary aluminum ash and water, adding the mixture into a reaction kettle, and performing solid-liquid separation after water leaching to obtain filtrate and filter cakes; washing the filter cake with water; adding the washed filter cake into a ball mill, and adding boric acid and acidic organic matters as mineralizers in the reaction process to obtain slurry; spray drying the slurry to obtain powder; removing iron from the powder by using a magnetic separator; calcining the powder subjected to iron removal; and crushing the calcined powder, and then washing with water to obtain corundum phase alumina. The process has the advantages of short process flow, low cost and no secondary pollution, and the secondary aluminum ash is used as a raw material to produce corundum phase aluminum oxide, so that the effect of resource application is more obvious.
Description
Technical Field
The invention relates to the technical field of secondary aluminum ash treatment, in particular to a process for producing corundum phase aluminum oxide by using secondary aluminum ash.
Background
The new solid waste law which starts to be executed in 9/1/2020 specifies: in addition to the original 'waste residue generated by the maintenance and production of an electrolytic cell in the process of electrolyzing aluminum' and 'salt slag and scum generated by electrolyzing aluminum', the scum generated on the surface of the melt in the processes of smelting and refining secondary aluminum and the salt slag and aluminum ash generated in the process of recovering the secondary aluminum are also added. The aluminum ash can be divided into electrolytic aluminum ash and regenerated aluminum ash in terms of sources, scum generated in the aluminum electrolysis process becomes the electrolytic aluminum ash, about 10-15 kg of aluminum ash is generated in 1 ton of electrolytic aluminum, and the domestic yield is about 80-100 ten thousand tons per year.
The secondary aluminum ash is analyzed, wherein the main component is alumina except partial aluminum nitride and impurity salts, the partial alumina is mainly converted into corundum phase alumina after repeated heating in the aluminum smelting and processing processes, namely commonly called alpha-alumina, the alpha-alumina is insoluble in water and acid, and the method can be used for preparing various refractory materials, grinding materials and bases of integrated circuits, and high-purity alpha-alumina is also used as a raw material for producing artificial corundum, artificial ruby and sapphire.
The treatment methods for secondary aluminum ash at home and abroad are many, and the treatment methods mainly focus on the production of building materials, water purifying agents, refractory materials and the like. From the analysis of harmless treatment of hazardous wastes, the secondary aluminum ash production building materials have certain potential safety hazards; from the perspective of reasonable utilization of resources, corundum-phase alumina is difficult to react with acid, and even though the prior art overcomes the problem, the method for changing the activity of alumina and completely converting corundum-phase alumina into active alumina with adsorption performance is not a method for reasonably utilizing resources; the production of refractory materials has certain technical difficulty, mainly because sodium salt, potassium salt and lithium salt existing in secondary aluminum ash can be transformed into low-melting substances to influence the performance of the refractory materials.
The above methods for comprehensively utilizing the secondary aluminum ash are essentially to separate and utilize the maximum amount of the most valuable components contained therein. From the perspective of comprehensive utilization of solid wastes, the method examines, judges and evaluates the solid wastes, has certain defects in aspects of capability of adapting to the market, project construction investment, economy of scale, high and low production cost, environment-friendly production line, secondary pollution generated in the disposal process, safety performance, particularly economic benefit and the like, and has various characteristics.
Disclosure of Invention
The invention aims to provide a process for producing corundum phase alumina by using secondary aluminum ash, which has the advantages of short process flow, low cost and no secondary pollution, and has more remarkable effect of resource application by using the secondary aluminum ash as a raw material to produce the corundum phase alumina.
The invention also aims to provide a process for producing corundum phase alumina by using secondary aluminum ash, which has the advantages of short process flow, low cost and no secondary pollution, and has more remarkable effect of resource application by using the secondary aluminum ash as a raw material to produce corundum phase alumina.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
On one hand, the invention provides a process for producing corundum phase alumina by adopting secondary aluminum ash, which comprises the following steps: water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:5-10, and performing solid-liquid separation after the water is leached to obtain a filtrate and a filter cake; washing: washing the filter cake with water; stirring and ball milling: adding the washed filter cake into a ball mill, and adding boric acid and acidic organic matters as mineralizers in the reaction process to obtain slurry; spray drying: spray drying the slurry to obtain powder; iron removal: removing iron from the powder by using a magnetic separator; and (3) calcining: calcining the powder material after iron removal at 1250-1600 ℃ for 1.5-3 h; and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
Further, in the water leaching process, the stirring speed in the reaction kettle is 200-500r/min, the temperature is 60-90 ℃, and the reaction time is 4-6 h.
Further, in the water leaching process, the reaction kettle is vacuumized by a water circulating pump, and the pressure in the reaction kettle is-0.06-0.1 Mpa.
Furthermore, the washing process adopts water washing for 5-8 times, and the solid-liquid mass ratio of each water washing is 1: 10-20.
Furthermore, the washing liquid after each washing is conveyed to the upper washing pool as washing water, and the washing water for the first time is conveyed to the reaction kettle.
Further, the solid-liquid mass ratio in the ball mill in the stirring ball-milling reaction process is 1:1-3, the rotating speed in the ball mill is 300-400r/min, and the reaction time is 1.5-2 h.
Further, citric acid or glucose can be used as the acidic organic substance.
Further, the mass of the boric acid accounts for 1-8% of the total mass of the reactants, and the mass of the acidic organic substance accounts for 0.2-0.8% of the total mass of the reactants.
Further, the speed of the peristaltic pump in the spray drying process is 35-40r/min, the air outlet temperature of the spray drying tower in the spray drying process is 105-.
On the other hand, the invention also provides a process for producing corundum phase alumina by adopting secondary aluminum ash, which is characterized by comprising the following steps: stirring and ball milling: mixing secondary aluminum ash and water, adding the mixture into a ball mill, wherein the mass ratio of the secondary aluminum ash to the water is 1:2-5, and stirring and ball milling to obtain slurry; spray drying: spray drying the slurry to obtain dried powder; washing: washing the powder by a washing tank for 5-8 times, and performing solid-liquid separation by a centrifuge after each washing to obtain washed powder; iron removal: drying the washed powder, removing iron from the powder by using a magnetic separator, adding boric acid and acidic organic matters as mineralizers, and stirring and mixing for 1.5-2.5 hours by using a mixer; and (3) calcining: calcining the powder material after iron removal at 1250-1600 ℃ for 1.5-3 h; and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
On one hand, the process for producing corundum-phase alumina by using secondary aluminum ash provided by the embodiment of the invention at least has the following advantages or beneficial effects:
in the above embodiment, the soluble salt of the secondary aluminum ash is dissolved in water during the water leaching process, and aluminum nitride reacts with water to generate aluminum hydroxide and ammonia gas, so as to remove toxicity; then washing to remove soluble salt; then boric acid and acid are added while the granularity of the secondary aluminum ash is reduced by stirring and ball millingThe organic matters are used as mineralizers to be uniformly mixed, so that subsequent reaction is facilitated, and the added boric acid can be mixed with water-insoluble minerals in the secondary aluminum ash in the calcining process, such as: nepheline (KNa)3(AlSiO4)4) Fishing island stone (NaAl)11O17) Water-soluble salts are formed by reaction, the pH value of the reaction environment can be adjusted by adding the acidic organic substance, the complex reaction of boric acid and mineral substances before calcination is facilitated, the calcination reaction is facilitated to be complete, and the acidic organic substance can be decomposed in the subsequent calcination process without influencing the product quality. Boric acid is a typical Lewis acid with an acidity constant of 5.8X 10-10Only weakly ionized to a small extent H in water+And BO3-The solution shows very weak acidity, and the hydrolysis equation is: h3BO3+H2O→ H+B(OH)4-,H+B(OH)4-The ion is tetrahedral structure, after adding acidic organic complexing agent of glucose and citric acid, B (OH) 4-reacts with polyhydroxy compound to make the balance move to the direction of ionization. Reacting to form a macromolecular chain complex, wherein the macromolecular chain complex can form inorganic salts which are easy to dissolve in water in the calcining process and then is removed by washing; the slurry after ball milling treatment is subjected to spray drying, so that the subsequent calcining reaction is more uniform and thorough; then, iron is removed through a magnetic separation iron remover, so that the subsequent reaction is prevented from being influenced, and iron can be recovered in the step, so that the resource utilization is maximized; then calcining to make boric acid and minerals such as: nepheline (KNa)3(AlSiO4)4) Fishing island stone (NaAl)11O17) And the like, forming water-soluble inorganic salts, enabling boric acid to react with the water-insoluble minerals more completely at the calcining temperature, leading to long reaction time and incomplete reaction due to too low reaction temperature and energy waste due to too high reaction temperature, and then crushing and washing to remove the water-soluble salts to obtain the corundum phase alumina with higher purity. The production process has the advantages of short flow, low cost and no secondary pollution, and the secondary aluminum ash is used as a raw material to produce corundum phase aluminum oxide, so that the effect of resource application is more obvious.
On the other hand, the process for producing corundum-phase alumina by using secondary aluminum ash provided by the embodiment of the invention at least has the following advantages or beneficial effects:
in the above embodiment, the soluble salt of the secondary aluminum ash is dissolved in water during the stirring and ball milling process, the aluminum nitride reacts with the water to generate aluminum hydroxide and ammonia gas, so as to remove toxicity, and simultaneously reduce the particle size of the secondary aluminum ash, thereby facilitating the subsequent chemical reaction of water-insoluble minerals; then, drying the slurry subjected to ball milling treatment by spray drying, so that the subsequent calcining reaction is more uniform and thorough; then washing to remove soluble salt, and performing solid-liquid separation by using a centrifugal machine to ensure that the solid-liquid separation efficiency is better; then the deironing is in deironing through the magnetic separation deironing machine, avoids influencing subsequent reaction, and can retrieve iron at this step for the resource utilization maximize, add boric acid and acid organic matter and mix as mineralizer misce bene, the subsequent reaction of being convenient for, add boric acid can be in the calcination in-process with the secondary aluminium ash in the water-insoluble mineral substance like: nepheline (KNa)3(AlSiO4)4) Fishing island stone (NaAl)11O17) The reaction forms water-soluble inorganic salt, and the pH value of the reaction environment can be adjusted by adding acidic organic matters, so that the complex reaction of boric acid and mineral substances before calcination is facilitated, and the calcination reaction is facilitated to be complete. Boric acid is a typical Lewis acid with an acidity constant of 5.8X 10-10Only weakly ionized to a small extent H in water+And BO3-The solution shows very weak acidity, and the hydrolysis equation is: h3BO3+H2O→H+B(OH)4-,H+B(OH)4-The ions are tetrahedral, after adding acidic organic complexing agents of glucose and citric acid, B (OH)4-Reacts with the polyol to shift the equilibrium in the direction of ionization. Reacting to form a macromolecular chain complex, wherein the macromolecular chain complex can be removed in the calcining process; then calcining to make boric acid react with water-insoluble impurities in the secondary aluminum ash to form water-soluble minerals, and making the boric acid react with the water-insoluble minerals more completely at such calcining temperatureThe reaction time is long due to the low temperature, the reaction is incomplete, and the energy waste is caused due to the high reaction temperature; then crushing and washing to remove water-soluble salt to obtain the corundum phase alumina with excellent purity. The production process has the advantages of short flow, low cost and no secondary pollution, and the secondary aluminum ash is used as a raw material to produce corundum phase aluminum oxide, so that the effect of resource application is more obvious.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an XRD pattern of corundum phase alumina prepared according to examples 1-3 of the present invention;
FIG. 2 is an XRD pattern of the sample without boric acid added for impurity removal;
FIG. 3 is an XRD (X-ray diffraction) diagram of the content of precipitated salt after flash evaporation treatment of 10 times of washing water in the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.
The embodiment of the application provides a process for producing corundum phase alumina by adopting secondary aluminum ash, which comprises the following steps: water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:5-10, and performing solid-liquid separation after the water is leached to obtain a filtrate and a filter cake; washing: washing the filter cake with water; stirring and ball milling: adding the washed filter cake into a ball mill, and adding boric acid and acidic organic matters as mineralizers in the reaction process to obtain slurry; spray drying: spray drying the slurry to obtain powder; iron removal: removing iron from the powder by using a magnetic separator; and (3) calcining: calcining the powder material after iron removal at 1250-1600 ℃ for 1.5-3 h; and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
In the above embodiment, the soluble salt of the secondary aluminum ash is dissolved in water during the water leaching process, and aluminum nitride reacts with water to generate aluminum hydroxide and ammonia gas, so as to remove toxicity; then washed to remove soluble salts.
Then, while the granularity of the secondary aluminum ash is reduced by stirring and ball milling, adding boric acid and acidic organic matters as mineralizers to be uniformly mixed, so as to facilitate subsequent reaction, wherein the added boric acid can react with water-insoluble minerals in the secondary aluminum ash in the calcining process to form water-soluble minerals, such as: nepheline (KNa)3(AlSiO4)4) Fishing island stone (NaAl)11O17) Referring to fig. 1 and 2, it can be seen that the addition of boric acid has a good impurity removal effect, and the purity of corundum phase alumina produced by adding secondary aluminum ash is effectively improved.
The pH value of the reaction environment can be adjusted by adding acidic organic matters, the reaction of boric acid and other impurities is facilitated, the boric acid is a typical Lewis acid, the acidity constant is 5.8 multiplied by 10 < -10 >, and only a small amount of H can be weakly ionized in water+And BO3-The solution shows very weak acidity, and the hydrolysis equation is: h3BO3+H2O →H+B(OH)4-,H+B(OH)4-The ions are tetrahedral, after adding acidic organic complexing agents of glucose and citric acid, B (OH)4-Reacting with polyhydroxy compound to make equilibrium move toward ionization direction, reacting to form macromolecular chain complex, and removing the macromolecular chain complex in the course of calcining.
Then, the slurry after ball milling treatment is dried through spray drying, so that the subsequent calcining reaction is more uniform and thorough; then the iron is removed through a magnetic separation iron remover, so that the subsequent reaction is prevented from being influenced, and the iron can be recovered in the step, so that the resource utilization is maximized.
And then calcining to enable boric acid to react with impurities insoluble in water in the secondary aluminum ash to form water-soluble minerals, wherein the calcining temperature enables the boric acid to react with the water-insoluble minerals more completely, the reaction time is long due to the low reaction temperature, the reaction is incomplete, the mineralizer is ineffective due to the high reaction temperature, the reaction rate is reduced, and the boric acid and the water-insoluble minerals are incomplete in reaction.
Then crushing and washing to remove water-soluble salt to obtain the corundum phase alumina with excellent purity. The production process has the advantages of short flow, low cost and no secondary pollution, and the secondary aluminum ash is used as a raw material to produce corundum phase aluminum oxide, so that the effect of resource application is more obvious.
Further, in the water leaching process, the stirring speed in the reaction kettle is 200-500r/min, the temperature is 60-90 ℃, and the reaction time is 4-6 h. In the above embodiment, adopt such parameter can make the soluble salt in the secondary aluminium ash dissolve in aqueous fast, the rotational speed of crossing low can reduce the efficiency of reaction and ball-milling, too high rotational speed can accelerate equipment wearing and tearing and can reduce the efficiency of reaction and ball-milling equally, calcination temperature crosses low can influence the completeness of edulcoration reaction, too high temperature can cause and cause the energy waste, the reaction time short excessively can lead to the reaction incomplete, dissolve thoroughly, the reaction time overlength can influence the time of process flow, and the process cost is improved.
Further, in the water leaching process, the reaction kettle is vacuumized by a water circulating pump, and the pressure in the reaction kettle is-0.06-0.1 Mpa.
In the above embodiment, adopt water circulating pump to above-mentioned reation kettle evacuation, because aluminium nitride in the secondary aluminium ash reacts with water and forms aluminium hydroxide and ammonia, adopt water circulating pump can make the ammonia in the reation kettle absorb by the water in the water circulating pump and obtain the aqueous ammonia, so not only can realize gaseous recovery separation in the course of the technology, can also improve the efficiency of reaction in the whole course of the technology.
The above-mentioned embodiment adopts water circulating pump to the evacuation of above-mentioned reation kettle, and 8% -12% aqueous ammonia can be prepared to the aqueous ammonia that obtains, and this type of aqueous ammonia can directly get into the SOx/NOx control technology of electrolytic aluminum enterprise power plant, improves the output value in the production corundum phase aluminium oxide in-process of secondary aluminium ash, realizes zero release, green among the whole technological process.
Furthermore, the washing process adopts water washing for 5-8 times, and the solid-liquid mass ratio of each water washing is 1: 10-20. In the embodiment, the filter cake is washed by water for 5-8 times, and the solid-liquid mass ratio is 1:10-20, so that almost all soluble salts contained in the filter cake can be removed, only water-insoluble minerals are left, the subsequent reaction is facilitated, and the purity of the corundum phase alumina can be further ensured.
Furthermore, the washing liquid after each washing is conveyed to the upper washing pool as washing water, and the washing water for the first time is conveyed to the reaction kettle. In the above embodiment, the washing liquid after each washing is sent to the last washing tank as the washing water, the first washing water is sent to the reaction kettle, the production cost can be reduced without affecting the washing effect, the salt content in the washing water after 5 times of washing is tested as shown in table 1 below, the ion concentration in the washing water after being recycled for many times is tested as shown in table 2 below, and the fluorine and chlorine ion concentration in the washing water is tested as shown in table 3 below:
TABLE 1
TABLE 2
TABLE 3
| Ion(s) | F-(mg/L) | Cl-(mg/L) |
| Recycling 5 times of first washing water | 895.9 | 905.1 |
| |
1808.5 | 2653.4 |
| |
774.6 | 636.2 |
As can be seen from tables 1, 2 and 3, the recycled washing water can reduce the production cost without affecting the washing effect.
The recycled washing water can be subjected to flash evaporation treatment, and as can be seen from fig. 3, the impurity salts of the washing water subjected to flash evaporation treatment for 10 times of washing treatment are mainly chlorine salt and fluorine salt, and the separated salt after treatment can be used as electrolyte for an electrolytic aluminum enterprise and supplemented into an electrolytic cell as electrolyte, and the mass ratio of the separated salt to newly added electrolyte is controlled to be 3-5%; the water vapor obtained after treatment can be directly supplemented into the leaching and washing processes after condensation, and can be recycled, so that the whole process is more green and environment-friendly due to recycling.
Further, the solid-liquid mass ratio in the ball mill in the stirring ball-milling reaction process is 1:1-3, the rotating speed in the ball mill is 300-400r/min, and the reaction time is 1.5-2 h.
In the above examples, such parameters are used to make the water insoluble minerals in the secondary aluminum ash uniform with the boric acid and acidic organics.
Further, the acidic organic substance is citric acid or glucose.
In the above examples, the use of citric acid or glucose allows the reaction environment to better adjust the Ph, providing an optimal reaction environment for the boric acid to react with minerals.
Further, the mass of the boric acid accounts for 1-8% of the total mass of the reactants, and the mass of the acidic organic substance accounts for 0.2-0.8% of the total mass of the reactants.
In the above embodiment, the boric acid and the acidic organic substance in such proportions can fully react the minerals in the secondary aluminum ash, and the incomplete reaction caused by too low amount of the boric acid and the acidic organic substance can not increase the process cost caused by too high amount of the boric acid and the acidic organic substance.
Further, the speed of the peristaltic pump in the spray drying process is 35-40r/min, the air outlet temperature of the spray drying tower in the spray drying process is 105-.
In the above examples, the dry powder particle size of the water-insoluble mineral in the secondary aluminum ash can be controlled to be 40-60 μm by using such parameters, which is beneficial to the reaction in the subsequent calcination process.
On the other hand, the embodiment of the application provides a process for producing corundum-phase alumina by using secondary aluminum ash, which is characterized by comprising the following steps: stirring and ball milling: mixing secondary aluminum ash and water, adding the mixture into a ball mill, wherein the mass ratio of the secondary aluminum ash to the water is 1:2-5, and stirring and ball milling to obtain slurry; spray drying: spray drying the slurry to obtain dried powder; washing: washing the powder by a washing tank for 5-8 times, and performing solid-liquid separation by a centrifuge after each washing to obtain washed powder; iron removal: drying the washed powder, removing iron from the powder by using a magnetic separator, adding boric acid and acidic organic matters as mineralizers, and stirring and mixing for 1.5-2.5 hours by using a mixer; and (3) calcining: calcining the powder material after iron removal at 1250-1600 ℃ for 1.5-3 h; and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
In the above embodiment, the soluble salt of the secondary aluminum ash is dissolved in water during the stirring and ball milling process, the aluminum nitride reacts with the water to generate aluminum hydroxide and ammonia gas, so as to remove toxicity, and simultaneously reduce the particle size of the secondary aluminum ash, thereby facilitating the subsequent chemical reaction of water-insoluble minerals; then, drying the slurry subjected to ball milling treatment by spray drying, so that the subsequent calcining reaction is more uniform and thorough; then washing to remove soluble salt, and performing solid-liquid separation by using a centrifugal machine to ensure that the solid-liquid separation efficiency is better; then the deironing is being passed through the magnetic separation deironing machine deironing, avoids influencing subsequent reaction, and can retrieve iron at this step for the resource utilization maximize, add boric acid and acid organic matter and mix as mineralizer misce bene, the subsequent reaction of being convenient for, add boric acid and can react with the water-insoluble mineral substance in the secondary aluminum ash in the calcination process and form the mineral substance that can dissolve in water, for example: nepheline (KNa3(AlSiO4)4), fishing island stone (NaAl11O17) and the like, please refer to fig. 1 and fig. 2, which show that the addition of boric acid has good impurity removal effect and effectively improves the purity of corundum phase alumina produced by adding secondary aluminum ash; the pH value of the reaction environment can be adjusted by adding an acidic organic substance, the reaction of boric acid and other impurities is facilitated, the boric acid is a typical Lewis acid, the acidity constant is 5.8 multiplied by 10 < -10 >, only a small amount of H < + > and BO3 < - > can be weakly ionized in water, the solution has extremely weak acidity, and the hydrolysis equation is as follows: h3BO3+ H2O → H + B (OH)4-, H + B (OH) 4-ions are tetrahedral, and after adding acidic organic complexing agents of glucose and citric acid, B (OH) 4-reacts with polyhydroxy compounds to move the equilibrium in the direction of ionization. Reacting to form a macromolecular chain complex, wherein the macromolecular chain complex can be removed in the calcining process; then calcining to enable boric acid to react with impurities insoluble in water in the secondary aluminum ash to form water-soluble minerals, wherein the boric acid and the water-insoluble minerals react more completely at the calcining temperature, the reaction time is long due to the fact that the reaction temperature is too low, the reaction is incomplete, the mineralizer is ineffective due to the fact that the reaction temperature is too high, the reaction rate is reduced, and the boric acid and the water-insoluble minerals do not completely react; then crushing and washing to remove water-soluble salt to obtain the corundum phase alumina with excellent purity. The production process has the advantages of short flow, low cost and no secondary pollution, and the secondary aluminum ash is used as a raw material to produce corundum phase aluminum oxide, so that the effect of resource application is more obvious.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a process for producing corundum phase alumina by using secondary aluminum ash, which comprises the following steps:
water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:5, the stirring speed in the reaction kettle is 200r/min, the temperature is 90 ℃, the reaction time is 4 hours, a water circulating pump is adopted to vacuumize the reaction kettle in the reaction process, the pressure in the reaction kettle is-0.06 Mpa, and after water leaching is finished, solid-liquid separation is carried out to obtain filtrate and filter cakes.
Washing: and (3) washing the filter cake with water for 5 times in the washing process, wherein the solid-liquid mass ratio of each washing is 1:20, the washing liquid after each washing is conveyed to the upper washing tank to be used as washing water, and the first washing water is conveyed to the reaction kettle.
Stirring and ball milling: adding the washed filter cake into a ball mill, wherein a grinding ball of the ball mill is made of corundum materials in the stirring and ball milling reaction process, the diameter of the grinding ball is 1mm, boric acid and acidic organic matters are added in the reaction process as mineralizers, the mass of the boric acid is 1% of the total mass of reactants, the mass of the acidic organic matters is 0.8% of the total mass of the reactants, the acidic organic matters are citric acid, the solid-liquid mass ratio in the ball mill in the stirring and ball milling reaction process is 1:1, the rotating speed in the ball mill is 300r/min, and the reaction time is 2h, so that slurry is obtained;
spray drying: spray drying the slurry, wherein the speed of a peristaltic pump in the spray drying process is 40r, the air outlet temperature of a spray drying tower in the spray drying process is 105 ℃, the air inlet temperature of the spray drying tower in the spray drying process is 240 ℃, and the rotating speed of a centrifugal turntable in the spray drying process is 35r/min to obtain powder;
iron removal: removing iron from the powder by using a magnetic separator;
and (3) calcining: calcining the powder subjected to iron removal at 1250 ℃ for 3 h;
and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
Example 2
The embodiment provides a process for producing corundum phase alumina by using secondary aluminum ash, which comprises the following steps:
water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:10, the stirring speed in the reaction kettle is 500r/min, the temperature is 90 ℃, the reaction time is 4 hours, a water circulating pump is adopted to vacuumize the reaction kettle in the reaction process, the pressure in the reaction kettle is 0.1Mpa, and after water leaching is finished, solid-liquid separation is carried out to obtain filtrate and filter cakes.
Washing: and (3) washing the filter cake with water for 8 times in the washing process, wherein the solid-liquid mass ratio of each time of washing is 1:10, the washing liquid after each time of washing is conveyed to the upper washing tank to be used as washing water, and the washing water for the first time is conveyed to the reaction kettle.
Stirring and ball milling: adding the washed filter cake into a ball mill, wherein a grinding ball of the ball mill is made of corundum materials in the stirring and ball milling reaction process, the diameter of the grinding ball is 3mm, boric acid and acidic organic matters are added in the reaction process as mineralizers, the mass of the boric acid is 8% of the total mass of reactants, the mass of the acidic organic matters is 0.8% of the total mass of the reactants, the acidic organic matters are citric acid or glucose, the solid-liquid mass ratio in the ball mill in the stirring and ball milling reaction process is 1:3, the rotating speed in the ball mill is 400r/min, and the reaction time is 1.5h, so that slurry is obtained;
spray drying: spray drying the slurry, wherein the speed of a peristaltic pump in the spray drying process is 40r, the air outlet temperature of a spray drying tower in the spray drying process is 110 ℃, the air inlet temperature of the spray drying tower in the spray drying process is 260 ℃, and the rotating speed of a centrifugal turntable in the spray drying process is 40r/min to obtain powder;
iron removal: removing iron from the powder by using a magnetic separator;
and (3) calcining: calcining the powder subjected to iron removal at 1600 ℃ for 1.5 h;
and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
Example 3
The embodiment provides a process for producing corundum phase alumina by using secondary aluminum ash, which comprises the following steps:
water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:8, the stirring speed in the reaction kettle is 400r/min, the temperature is 80 ℃, the reaction time is 5 hours, a water circulating pump is adopted to vacuumize the reaction kettle in the reaction process, the pressure in the reaction kettle is 0.06MPa, and after water leaching is finished, solid-liquid separation is carried out to obtain filtrate and filter cakes.
Washing: and (3) washing the filter cake with water for 7 times in the washing process, wherein the solid-liquid mass ratio of each washing is 1:15, the washing liquid after each washing is conveyed to the upper washing tank to be used as washing water, and the first washing water is conveyed to the reaction kettle.
Stirring and ball milling: adding the washed filter cake into a ball mill, wherein a grinding ball of the ball mill is made of corundum materials in the stirring and ball milling reaction process, the diameter of the grinding ball is 2mm, boric acid and acidic organic matters are added in the reaction process as mineralizers, the mass of the boric acid is 5% of the total mass of reactants, the mass of the acidic organic matters is 0.3% of the total mass of the reactants, the acidic organic matters are citric acid or glucose, the solid-liquid mass ratio in the ball mill in the stirring and ball milling reaction process is 1:2, the rotating speed in the ball mill is 350r/min, and the reaction time is 2 hours, so that slurry is obtained;
spray drying: spray drying the slurry, wherein the speed of a peristaltic pump in the spray drying process is 38r, the air outlet temperature of a spray drying tower in the spray drying process is 108 ℃, the air inlet temperature of the spray drying tower in the spray drying process is 250 ℃, and the rotating speed of a centrifugal turntable in the spray drying process is 38r/min to obtain powder;
iron removal: removing iron from the powder by using a magnetic separator;
and (3) calcining: calcining the powder subjected to iron removal at 1500 ℃ for 2 h;
and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
Example 4
The embodiment provides a process for producing corundum phase alumina by using secondary aluminum ash, which comprises the following steps:
water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:6, the stirring speed in the reaction kettle is 300r/min, the temperature is 65 ℃, the reaction time is 5.5 hours, a water circulating pump is adopted to vacuumize the reaction kettle in the reaction process, the pressure in the reaction kettle is-0.01 Mpa, and after water leaching, solid-liquid separation is carried out to obtain filtrate and filter cakes.
Washing: and (3) washing the filter cake with water for 6 times in the washing process, wherein the solid-liquid mass ratio of each washing is 1:12, the washing liquid after each washing is conveyed to the upper washing tank to be used as washing water, and the first washing water is conveyed to the reaction kettle.
Stirring and ball milling: adding the washed filter cake into a ball mill, wherein a grinding ball of the ball mill is made of corundum materials in the stirring and ball milling reaction process, the diameter of the grinding ball is 2mm, boric acid and acidic organic matters are added in the reaction process as mineralizers, the mass of the boric acid is 4% of the total mass of reactants, the mass of the acidic organic matters is 0.4% of the total mass of the reactants, the acidic organic matters are citric acid or glucose, the solid-liquid mass ratio in the ball mill in the stirring and ball milling reaction process is 1:2, the rotating speed in the ball mill is 325r/min, and the reaction time is 1.8h, so as to obtain slurry;
spray drying: spray-drying the slurry, wherein the speed of a peristaltic pump in the spray-drying process is 37r, the air outlet temperature of a spray-drying tower in the spray-drying process is 102 ℃, the air inlet temperature of the spray-drying tower in the spray-drying process is 245 ℃, and the rotating speed of a centrifugal turntable in the spray-drying process is 39r/min to obtain powder;
iron removal: removing iron from the powder by using a magnetic separator;
and (3) calcining: calcining the powder subjected to iron removal at 1300 ℃ for 2.5 h;
and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
Example 5
The embodiment provides a process for producing corundum phase alumina by using secondary aluminum ash, which comprises the following steps:
water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:9, the stirring speed in the reaction kettle is 450r/min, the temperature is 75 ℃, the reaction time is 4.5h, a water circulating pump is adopted to vacuumize the reaction kettle in the reaction process, the pressure in the reaction kettle is 0.03MPa, and after water leaching is finished, solid-liquid separation is carried out to obtain filtrate and filter cakes.
Washing: and (3) washing the filter cake with water for 6 times in the washing process, wherein the solid-liquid mass ratio of each washing is 1:16, the washing liquid after each washing is conveyed to the upper washing tank to be used as washing water, and the first washing water is conveyed to the reaction kettle.
Stirring and ball milling: adding the washed filter cake into a ball mill, wherein a grinding ball of the ball mill is made of corundum materials in the stirring and ball milling reaction process, the diameter of the grinding ball is 3mm, boric acid and acidic organic matters are added in the reaction process as mineralizers, the mass of the boric acid is 6% of the total mass of reactants, the mass of the acidic organic matters is 0.6% of the total mass of the reactants, the acidic organic matters are citric acid or glucose, the solid-liquid mass ratio in the ball mill in the stirring and ball milling reaction process is 1:3, the rotating speed in the ball mill is 380r/min, and the reaction time is 1.92h, so as to obtain slurry;
spray drying: spray drying the slurry, wherein the speed of a peristaltic pump in the spray drying process is 39r, the air outlet temperature of a spray drying tower in the spray drying process is 109 ℃, the air inlet temperature of the spray drying tower in the spray drying process is 255 ℃, and the rotating speed of a centrifugal turntable in the spray drying process is 40r/min to obtain powder;
iron removal: removing iron from the powder by using a magnetic separator;
and (3) calcining: calcining the powder subjected to iron removal at 1550 ℃ for 1.8 h;
and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
Experimental example 1
The corundum phase alumina prepared in examples 1 to 3 was subjected to ICP measurement, and the corundum phase alumina did not react under these conditions and thus was not dissolved into the solution system, and the ion content was shown in table 4 by ICP measurement.
TABLE 4
Experimental example 2
The corundum phase alumina prepared in examples 1-3 was XRF tested and subjected to XRF testing with the respective ion contents shown in table 5.
Experimental example 3
The corundum phase alumina prepared in examples 1 to 3 was XRD-tested and subjected to XRD-testing, and the respective ion contents were as shown in FIG. 1.
It can be seen from the above experimental examples that the total content of corundum-phase alumina in the preparation of examples 1 to 3 is greater than 99.5%, wherein the content of corundum-phase alumina is greater than 98%, and the content of low-melting matters is less than 0.4%, so that the corundum-phase alumina is produced by using secondary aluminum ash as a raw material by adopting the process, and the effect of resource utilization is more remarkable.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A process for producing corundum phase alumina by using secondary aluminum ash is characterized by comprising the following steps:
water leaching: mixing secondary aluminum ash and water, adding the mixture into a reaction kettle, wherein the mass ratio of the secondary aluminum ash to the water is 1:5-10, and performing solid-liquid separation after the water leaching is finished to obtain a filtrate and a filter cake;
washing: washing the filter cake with water;
stirring and ball milling: adding the washed filter cake into a ball mill, and adding boric acid and acidic organic matters as mineralizers in the reaction process to obtain slurry;
spray drying: spray drying the slurry to obtain powder;
iron removal: removing iron from the powder by using a magnetic separator;
and (3) calcining: calcining the powder material after iron removal at 1250-1600 ℃ for 1.5-3 h;
and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
2. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 1, is characterized in that: in the water leaching process, the stirring speed in the reaction kettle is 200-500r/min, the temperature is 60-90 ℃, and the reaction time is 4-6 h.
3. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 1 or 2, is characterized in that: in the water leaching process, a water circulating pump is adopted to vacuumize the reaction kettle, and the pressure in the reaction kettle is-0.06-0.1 Mpa.
4. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 1, is characterized in that: the washing process adopts water washing for 5-8 times, and the solid-liquid mass ratio of each time of water washing is 1: 10-20.
5. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 4, is characterized in that: and conveying the washing liquid after each washing to the upper washing tank as washing water, and conveying the washing water for the first time to the reaction kettle.
6. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 1, is characterized in that: the solid-liquid mass ratio in the ball mill in the stirring ball-milling reaction process is 1:1-3, the rotating speed in the ball mill is 300-400r/min, and the reaction time is 1.5-2 h.
7. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 1, is characterized in that: the acidic organic substance can be citric acid or glucose.
8. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 1, is characterized in that: the mass of the boric acid is 1-8% of the total mass of the reactants, and the mass of the acidic organic matter is 0.2-0.8% of the total mass of the reactants.
9. The process for producing corundum phase alumina by using secondary aluminum ash according to claim 1, is characterized in that: the speed of the peristaltic pump in the spray drying process is 35-40r/min, the air outlet temperature of the spray drying tower in the spray drying process is 105-110 ℃, the air inlet temperature of the spray drying tower in the spray drying process is 240-260 ℃, and the rotating speed of the centrifugal turntable in the spray drying process is 35-40 r/min.
10. A process for producing corundum phase alumina by using secondary aluminum ash is characterized by comprising the following steps:
stirring and ball milling: mixing secondary aluminum ash and water, adding the mixture into a ball mill, wherein the mass ratio of the secondary aluminum ash to the water is 1:2-5, and stirring and ball milling to obtain slurry;
spray drying: spray drying the slurry to obtain dried powder;
washing: washing the powder by a washing tank for 5-8 times, and performing solid-liquid separation by a centrifuge after each washing to obtain washed powder;
iron removal: drying the washed powder, removing iron from the powder by using a magnetic separator, adding boric acid and acidic organic matters as mineralizers, and stirring and mixing for 1.5-2.5 hours by using a mixer;
and (3) calcining: calcining the powder material after iron removal at 1250-1600 ℃ for 1.5-3 h;
and (3) washing again: and crushing the calcined powder, and then washing with water to obtain corundum phase alumina.
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