CN113930624B - Method for removing fluorine and chlorine in secondary aluminum ash first-stage activity controllable dissolution process - Google Patents
Method for removing fluorine and chlorine in secondary aluminum ash first-stage activity controllable dissolution process Download PDFInfo
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Abstract
The invention relates to the technical field of aluminum clean metallurgy, and particularly discloses a method for removing fluorine and chlorine in a secondary aluminum ash first-stage active controllable dissolution process, which specifically comprises the following steps: adding aluminum ash into water containing an organic additive in batches under the condition of low solid content, controlling the temperature of a dissolution system, and stirring and dissolving to obtain dissolution slurry; extracting fluorine-containing chlorine aqueous solution from the dissolved slurry to obtain high-solid-content slurry for first-stage active dissolution; adding caustic alkali into the fluorine-containing chlorine aqueous solution, separating out coarse-grain fluoride salt and separating to obtain defluorination alkali liquor; adding a dechlorination additive into the defluorination alkali liquor for reaction, carrying out solid-liquid separation, and returning the dechlorination alkali liquor to an active dissolution process. The method efficiently and safely disposes harmful elements such as fluorine, chlorine, nitrogen, hydrogen and the like in the aluminum ash, reduces the influence of fluorine and chlorine on the production of aluminum oxide by a Bayer process or the subsequent preparation of aluminum oxide-based materials, can obviously improve the safety and the recovery rate of aluminum oxide in the comprehensive utilization of secondary aluminum ash, and is convenient for high-value utilization.
Description
Technical Field
The invention relates to the technical field of aluminum clean metallurgy, and particularly discloses a method for removing fluorine and chlorine in a secondary aluminum ash primary activity controllable dissolution process.
Background
The secondary aluminum ash is waste generated in the processes of aluminum electrolysis, aluminum casting, aluminum processing and aluminum regeneration, and is dangerous waste. The secondary aluminum ash is rich in source, complex in component and remarkable in phase content fluctuation, and can rapidly generate ammonia gas, hydrogen gas and the like along with violent heat release after being contacted with water; at the same time, chloride and fluoride enter the water, thus polluting the water, air and soil.
At present, the domestic comprehensive utilization of secondary aluminum ash is mainly concerned with the high-value utilization of aluminum, and the pretreatment of the secondary aluminum ash is provided to be used as an electrolysis raw material, corundum production, a slagging agent for metal smelting preparation, refractory material production, (poly) aluminum sulfate or (poly) aluminum chloride production, special (or sandy) alumina powder or building material production and the like; the method can recycle part (or all) of the aluminum components, but the research on safe and economic fluorine and chlorine removal methods is less, and the industrial implementation is difficult. The main defluorination and chlorination processes are summarized as follows: 1) washing with water for dechlorination and fluorine, concentrating the solution by evaporation, and crystallizing to separate out chloride salt or fluoride salt; optionally adding calcium-containing additive to generate calcium fluoride for defluorination; 2) alkali washing dechlorination and fluorine, evaporating and crystallizing to separate out chloride salt and fluoride salt; 3) treating with high temperature steam, adding sulfuric acid to precipitate out hydrogen fluoride, and removing fluoride. 4) The vacuum heating sublimation-condensation method has no pollution and short flow path for removing fluorine and chlorine (CN 104988313A). 5) High temperature calcining (CN112077124A) to volatilize fluoride salt and chloride salt, settling and dedusting, and recovering fluoride salt and chloride salt. The main disadvantages of the method are as follows: the secondary aluminum ash active substances (aluminum nitride, aluminum and silicon) have too high reaction activity, are contacted with an aqueous solution to carry out a rapid exothermic reaction, cause bumping and cannot safely remove chlorine and fluorine; the energy consumption, investment and operation cost of the chloride and fluoride separated out by evaporation and crystallization are high; the apparent solubility of the fine calcium fluoride is high, and calcium is added to remove fluorine completely; the addition of strong acid to separate out hydrogen fluoride has complex process and high cost; vacuum and high-temperature treatment, high requirements on equipment, high energy consumption and high cost. So far, the problem of safe treatment of harmful fluorine and chlorine is not economically solved, and the industrial application of various secondary aluminum ash new processes is hindered.
In the patent "a method for producing sandy alumina safely and efficiently by using aluminum ash" (201710096849.7), a method for producing the dechlorinated sodalite in a sodium aluminate solution is proposed, but the method is combined with a Bayer process alumina production enterprise. At present, no large-scale alumina production enterprises exist in developed eastern and western areas of China, and a new flow needs to be configured according to the defluorination and the chlorination, so that the operation cost is high; in the process of adopting the traditional small-amount multiple feeding mode, surface modification, low temperature control and specific equipment configuration are not needed, the reaction of active substances is still difficult to prevent, the system is in a higher positive pressure state, the feeding is difficult, and the operating environment is poor.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a technical scheme for washing secondary aluminum ash with water under a controllable reaction condition to economically remove chlorine and fluorine, and realize resource utilization.
In order to achieve the aim, the invention provides a method for removing fluorine and chlorine in a secondary aluminum ash primary activity controllable dissolution process, which comprises the following steps:
s1: adding aluminum ash into water containing organic additives in batches under the condition of low solid content, controlling the temperature of a dissolution system, and stirring at low speed for dissolution to obtain dissolution slurry;
s2: extracting fluorine-containing chlorine aqueous solution from the dissolved slurry to obtain high-solid-content slurry for first-stage active dissolution;
s3: adding caustic alkali into the fluorine-containing chlorine aqueous solution, separating out coarse-grain fluoride salt, and separating to obtain defluorination alkali liquor;
s4: adding a dechlorination additive into the defluorination alkali liquor for reaction and dechlorination, carrying out solid-liquid separation, and returning the dechlorination alkali liquor to the first active dissolution process.
Further, in the step S1, the organic additive is one or a mixture of two of glutathione polydentate ligands and anionic fluorocarbon surfactants, and the addition amount of the organic additive is 20-300 ppm.
Further, the aluminum ash batch adding process specifically comprises the following steps:
adding aluminum ash by times in a charging bell or nitrogen pressurization mode, wherein the adding amount is less than 60g/L each time, the adding times are more than 5 times, and the amount of the aluminum ash in the slurry is less than 400 g/L;
the pressure is more than 0.06kg/cm in the process of adding the aluminum ash by adopting a pressurizing mode 2 ；
And at least three material bells are adopted in the process of adding aluminum ash by the feeding bell.
Further, the controlling the temperature of the dissolution system and the low-speed stirring dissolution process specifically comprise:
the temperature of the system is controlled to be less than 60 ℃, and the stirring speed is less than 50 revolutions per minute.
Further, the step S3 specifically includes:
adding caustic to the slurry to a solution alkali concentration greater than 160 g/L;
adding fluoride salt seed crystal, controlling the temperature to be less than 80 ℃, obtaining coarse-grained fluoride salt crystal, and carrying out solid-liquid separation.
Further, the dechlorination additive is any one of kaolin/stone, calcined kaolin/stone or water glass.
Further, the dechlorination process is carried out for 0.5 to 4 hours at the temperature of between 70 and 120 ℃.
Further, in the step S2, the fluorine-containing chlorine aqueous solution is extracted to obtain a high solid content slurry with a solid content of 600 to 900g/L, and the extraction process may adopt nitrogen protection.
The invention combines the research result of the inventor on the reaction rule of the phase in the aluminum ash in water, and concretely discovers that:
(1) when a large amount of aluminum ash (secondary aluminum ash) is added, active components of aluminum, silicon and aluminum nitride in the aluminum ash are easy to react in water, a large amount of reaction heat is released, and dynamic synergy of high solid content and high temperature is easy to occur, so that the reaction is uncontrollable and accompanied by bumping and flash explosion;
(2) by adopting a charging bell or a pressurizing charging mode, a small quantity of multiple charging modes can be stably realized, the operating environment is good, and the reaction rate in the process of washing secondary aluminum ash by water can be controlled;
(3) the surfactant containing sulfur, nitrogen and fluorine can interact with solvated aluminum surface ions in a form similar to a coordinate bond to realize the reaction of compactly adsorbing an aluminum-containing component, carrying out surface modification and passivating active substances in water;
(4) in the process of washing the secondary aluminum ash by water, chloride is easy to leach, and fluoride leaching rate is slow; the solubility of sodium fluoride is obviously reduced along with the increase of alkali concentration, and in the fluorine-containing sodium aluminate solution, the supersaturation degree of fluorine is regulated and controlled by regulating the alkali concentration, seed crystals are added, and the agglomeration of particles is synergistically enhanced, so that coarse-grained sodium fluoride with the average grain size of more than 20 mu m can be obtained, and the economic separation is realized;
(5) the apparent solubility of the particles increases significantly as the particle size becomes smaller. When the particle size is less than 5 μm, the apparent solubility increases sharply as the particle size decreases.
(6) The chlorine is easy to be embedded into zeolite (Na) in sodium aluminate solution 6 Al 6 Si 6 O 24 ) In (b), by producing sodalite (Na) 8 Al 6 Si 6 O 24 Cl 2 ) Removing chlorine. And kaolin/stone and baked kaolin/stone can be converted into sodalite through dissolution in the reaction with alkali, so that the dechlorination efficiency is high.
Compared with the prior art, the invention has the following beneficial effects:
(1) controlling the reaction of active components, safely removing fluorine and chlorine: the invention provides a multi-factor coupling inhibition aluminum ash reaction, which can remarkably inhibit the reaction of active components and water, reduce the reaction rate and the reaction rate, strengthen the water-washing removal of chlorine and fluorine, build a safe bottom line, optimize the operation environment and ensure the controllable proceeding of the reaction by adding an organic matter additive into water for surface passivation, adding aluminum ash in batches, controlling mass transfer (low-speed stirring) and controlling the reaction temperature (low temperature) for coupling.
(2) Economically separating fluorine and chlorine containing solutions: the chlorine and fluorine-containing solution is taken out by the pressure formed by a small amount of generated gas through the self-pressure of the material taking pipe, so that the amount of the chlorine and fluorine-containing solution can be conveniently and economically regulated and controlled, and the operation cost is low.
(3) The fluoride salt is recycled and efficiently utilized: when the sodium fluoride is precipitated by traditional evaporation or in concentrated alkali, the product has small particle size, very large apparent solubility, more attached liquid, more washing water and incomplete defluorination; according to the invention, the supersaturation degree of sodium fluoride is regulated, and a proper amount of seed crystals are added to promote agglomeration of fine-particle sodium fluoride, so that coarse-particle sodium fluoride is obtained, the precipitation rate of sodium (potassium) fluoride is improved, impurity adsorption is reduced, and the purity of sodium fluoride is improved, thereby improving the economy of sodium (potassium) fluoride recovery.
(4) Short-process dechlorination: the silicon-containing substances in the sodium aluminate solution are used for reaction to generate zeolite which is embedded to generate sodalite, so that chlorine can be removed in a short process, impurities are not introduced, the alkali liquor can be conveniently recycled, the operation cost can be reduced, the consumption can be reduced, and the industrialization is facilitated.
(5) Be convenient for improve secondary aluminium ash treatment effeciency: based on the controllable reaction water slurry mixing with low solid content and the participation of the slurry with high solid content in the first active dissolving process, the subsequent process can be continuously carried out with high concentration on the premise of removing fluorine and chlorine in advance, and the amount of water entering the process is reduced.
(6) Promoting the industrialization of the technology. If the method is cooperated with alumina enterprises, the influence of chlorine and fluorine on alumina by a Bayer process can be reduced by the method for removing fluorine and chlorine; if no alumina enterprise is cooperative, the early-stage fluorine and chlorine removal is beneficial to the later-stage alumina material preparation or alumina production flow optimization, and the product quality is improved. All of them promote the industrialization of the comprehensive utilization technology of the secondary aluminum ash.
Drawings
FIG. 1 is a process flow chart of a method for removing fluorine and chlorine in a secondary aluminum ash primary activity controlled dissolution process provided by the embodiment of the invention.
Detailed Description
The present invention will be described in detail with reference to the drawings and examples, but the present invention is not limited thereto. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention.
Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art; all reagents used in the examples are commercially available unless otherwise specified.
The percentage "%" referred to in the present invention means mass% unless otherwise specified; but the percentage of the solution, unless otherwise specified, refers to the grams of solute contained in 100ml of the solution.
The weight parts in the invention can be the weight units known in the art such as mu g, mg, g, kg, and the like, and can also be multiples thereof, such as 1/10, 1/100, 10, 100, and the like.
Example 1
40g of secondary aluminum ash (total Al) was taken 2 O 3 81.37％,SiO 2 3.5％,AlN 10.42％,MgO 2.56％,Fe 2 O 3 1.05％,TiO 2 0.56％,Na 2 O4.91%, Cl 5.32% and F4.9%) was added into 120mL of glutathione solution containing 300ppm by nitrogen pressurization in 7 portions, the stirring speed was 20 rpm, and the temperature was controlled to be less than 30 ℃. After the addition, the pressure of the reaction system was 0.09kg/cm 2 Filtering and pumping 55mL of chlorine-containing and fluorine-containing aqueous solution by utilizing self pressure, and transferring the remaining high-concentration (740 g/L) slurry to a first active dissolution procedure; adding 13g of sodium hydroxide into 50mL of solution containing chlorine and fluorine for 5 times, adding 5g of sodium fluoride with the average particle size of 15 mu m as seed crystal at one time, and separating out coarse sodium fluoride by using the seed crystal at the temperature of 40 ℃, wherein the average particle size is 35 mu m, and the fluorine removal rate is 60%; adding 3g of kaolinite into the solution for removing fluorine, and dechlorinating for 4h at 100 ℃, wherein the dechlorinating rate is 70%. Returning the dechlorinated alkali liquor to the first active stage of dissolution process.
Example 2
Taking 50g of the secondary aluminum ash, adding 120mL of water containing 50ppm of anionic fluorocarbon surfactant in a nitrogen pressurization mode for 10 times, stirring at the speed of 30 r/min, and controlling the temperature to be less than 35 ℃. After the addition, the pressure of the reaction system was 0.07kg/cm 2 Filtering and pumping 60mL of chlorine-containing and fluorine-containing aqueous solution by utilizing self pressure, and transferring the remaining high-concentration (830 g/L) slurry to a first active dissolution procedure; adding 15g of sodium hydroxide into 50mL of solution containing chlorine and fluorine for 5 times, adding 4g of sodium fluoride with the average particle size of 30 mu m as seed crystal at one time, and separating out coarse sodium fluoride at the temperature of 35 ℃ by using the seed crystal, wherein the average particle size is 52 mu m, and the fluorine removal rate is 70%; adding 3g of roasted kaolinite into the solution for removing fluorine, and dechlorinating for 4h at 70 ℃, wherein the dechlorinating rate is 71%. Returning the dechlorinated alkali liquor to the first active stage of dissolution process.
Example 3
Taking 50g of the secondary aluminum ash, adding 120mL of water containing 100ppm of glutathione and anionic fluorocarbon surfactant for 10 times by adopting a nitrogen pressurization mode, stirring at the speed of 40 r/min, and controlling the temperature to be less than 45 ℃. After the addition, the pressure of the reaction system was 0.05kg/cm 2 In the above step, 55mL of an aqueous solution containing chlorine and fluorine was filtered and extracted by the use of the autogenous pressure, and the remaining slurry having a high concentration (. about.910 g/L) was transferred to the first active digestion step; adding 15g of sodium hydroxide into about 55mL of chlorine and fluorine-containing solution for 3 times, adding 4g of sodium fluoride with the average particle size of 30 mu m as seed crystal at one time, and separating out coarse sodium fluoride from the seed crystal at the temperature of 35 ℃, wherein the average particle size is 52 mu m, and the fluorine removal rate is 70%; 7mL of 30% water glass is added into the solution for removing fluorine, dechlorination is carried out for 3h at 100 ℃, and the dechlorination rate is 64%. Returning the dechlorinated alkali liquor to the first active stage of dissolution process.
Example 4
30g of the secondary aluminum ash is taken for 6 times, 120mL of water containing 300ppm of glutathione and anionic fluorocarbon surfactant is added in a charging clock mode, the stirring speed is 10 r/min, and the temperature is controlled to be less than 35 ℃. After the addition, the pressure of the reaction system was 0.03kg/cm 2 Filtering and extracting 50mL of chlorine-containing and fluorine-containing aqueous solution by utilizing self pressure and extraction, and transferring the remaining high-concentration (about 620g/L) slurry to a first active dissolution procedure; adding 13g of sodium hydroxide into 50mL of chlorine-containing and fluorine-containing solution for 2 times, adding 4g of sodium fluoride with the average particle size of 15 mu m as seed crystals at one time, and separating out coarse sodium fluoride by using the seed crystals at the temperature of 60 ℃, wherein the average particle size is 32 mu m, and the fluorine removal rate is 66%; 1g of roasted kaolinite (earth) is added into the solution for removing fluorine, and dechlorination is carried out for 0.5h at 120 ℃, wherein the dechlorination rate is 53 percent. Returning the dechlorinated alkali liquor to the first active stage of dissolution process.
Example 5
And (3) taking 40g of the secondary aluminum ash for 8 times, adding 100mL of water containing 20ppm of anionic fluorocarbon surfactant in a charging clock mode, stirring at the speed of 90 r/min, and controlling the temperature to be lower than 35 ℃. After the addition, the pressure of the reaction system was 0.07kg/cm 2 Filtering and pumping 45mL of chlorine-containing and fluorine-containing aqueous solution by utilizing self pressure, and transferring the remaining high-concentration (670 g/L) slurry to a first active dissolution process; in about 45mL of a solution containing chlorofluoroAdding 13g of sodium hydroxide for 2 times, adding 4g of sodium fluoride with the average grain diameter of 15 mu m as seed crystal for one time, and separating out coarse-grain sodium fluoride at the temperature of 70 ℃ by using the seed crystal, wherein the average grain diameter is 25 mu m, and the fluorine removal rate is 45%; 6g of roasted kaolinite (clay) is added into the solution for removing fluorine, and dechlorination is carried out for 4 hours at 120 ℃, wherein the dechlorination rate is 92%. Returning the dechlorinated alkali liquor to the first active stage of dissolution process.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (6)
1. A method for removing fluorine and chlorine in a secondary aluminum ash first-stage active controllable dissolution process is characterized by comprising the following steps:
s1: under the condition of low solid content, adding aluminum ash into water containing organic additives in batches, controlling the temperature of a dissolution system, and stirring at low speed to dissolve out to obtain dissolution slurry containing fluorine and chlorine;
s2: extracting fluorine-containing chlorine aqueous solution from the dissolved slurry to obtain high-solid-content slurry for first-stage active dissolution;
s3: adding caustic alkali into the fluorine-containing chlorine aqueous solution, separating out coarse-grain fluoride salt, and separating to obtain defluorination alkali liquor;
s4: adding a dechlorinating additive into the defluorination alkali liquor for reaction and dechlorination, carrying out solid-liquid separation, and returning the dechlorination alkali liquor to a section of active dissolution process;
in the step S1, the organic additive is one or a mixture of two of glutathione polydentate ligands and anionic fluorocarbon surfactants, and the addition amount of the organic additive is 20-300 ppm;
the dechlorination additive is any one of kaolin, roasted kaolin or water glass.
2. The method for removing fluorine and chlorine in the secondary aluminum ash primary activity controlled dissolution process according to claim 1, wherein the aluminum ash batch adding process specifically comprises the following steps:
adding aluminum ash by times in a charging bell or nitrogen pressurization mode, wherein the adding amount is less than 60g/L each time, the adding times are more than 5 times, and the amount of the aluminum ash in the slurry is less than 400 g/L;
the pressure in the process of adding the aluminum ash by adopting a nitrogen pressurization mode is more than 0.06kg/cm 2 ;
And at least three material bells are adopted in the process of adding aluminum ash by the feeding bell.
3. The method for removing fluorine and chlorine in the secondary aluminum ash primary activity controllable digestion process according to claim 1, wherein the digestion system temperature control and low-speed stirring digestion process specifically comprises:
the temperature of the system is controlled to be less than 60 ℃, and the stirring speed is less than 100 revolutions per minute.
4. The method for removing fluorine and chlorine in the secondary aluminum ash first-stage activity controlled dissolution process according to claim 1, wherein the step S3 specifically comprises:
adding caustic to the slurry to a solution alkali concentration greater than 160 g/L;
adding fluoride salt seed crystal, controlling the temperature to be less than 80 ℃, obtaining coarse fluoride salt crystal, and carrying out solid-liquid separation.
5. The method for removing fluorine and chlorine in the secondary aluminum ash primary activity controlled dissolution process according to claim 1, wherein the chlorine removal process is a reaction at 70-120 ℃ for 0.5-4 h.
6. The method for removing fluorine and chlorine in the secondary aluminum ash primary activity controllable dissolution process according to claim 1, wherein the fluorine and chlorine containing aqueous solution is extracted in the step S2 to obtain slurry with a solid content of 600-900 g/L, and the extraction process can be protected by nitrogen.
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