CN110902706A - Method for preparing polyaluminum chloride from aluminum ash - Google Patents
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Abstract
The invention relates to a method for preparing polyaluminium chloride by using aluminum ash, which comprises the steps of mixing the aluminum ash with coke and preparing pellets with the diameter of 5-20 mm; adding the pellets into a moving bed reactor from the top end, introducing chlorine gas with the concentration of 35-100% from the bottom to perform chlorination reaction, and respectively obtaining a gas-phase product taking aluminum chloride as a main component and a solid-phase product taking magnesium chloride as a main component after chlorination; mixing an aluminum chloride product obtained after the temperature of the gas-phase product is reduced with water to obtain an aluminum chloride solution with the concentration of 300-600 g/L, adjusting the pH value to 3-4 by using ammonia gas, curing at room temperature for 10-20 h, and drying a cured liquid-phase product to obtain a polyaluminum chloride product; the solid phase product can be directly used as a raw material for preparing the snow-melting agent. The method realizes the high-efficiency recovery of aluminum in the aluminum ash and the harmless utilization of the tailings by the processes of pellet preparation, chlorination and aluminum chloride solution polymerization, and is a green and environment-friendly comprehensive utilization process of the aluminum ash.
Description
The technical field is as follows:
the invention belongs to the technical field of aluminum ash utilization, and particularly relates to a method for preparing polyaluminum chloride from aluminum ash.
Background art:
aluminum is a prop industry in the nonferrous metallurgy industry in China, and the capacity of the raw aluminum in China reaches more than 3000 million tons and is listed as the first world by 2018. The aluminum ash is one of the main wastes in the aluminum smelting process, 180-290 kg of aluminum ash slag is generated when one ton of raw aluminum/aluminum material is produced, and millions of tons of aluminum ash slag are discharged every year. The aluminum ash is listed in the name of dangerous waste due to the content of nitride, fluorine, chlorine and the like.
In recent years, China's aluminum industry has carried out a lot of research works aiming at the efficient and high-valued utilization of aluminum ash, such as the method for recovering and recycling aluminum ash slag proposed by Lihu, and the disclosure number is: the main steps of CN 109970456A' are: s1, rolling and grinding the aluminum ash, separating iron impurities by a magnetic separation method, and separating metal aluminum by a screening method to obtain secondary aluminum ash; s2, carrying out water washing operation on the secondary aluminum ash, and decomposing aluminum nitride and salts in the secondary aluminum ash; s3, adding kaolin, bentonite and talc in a certain proportion into the alumina-containing filter residue obtained after washing to obtain wet-milled slurry, and further adding a stabilizer of ammonium polyacrylate, a surfactant of carboxymethyl cellulose and hot silica sol to prepare slurry; s4, dipping the slurry obtained in the step S3 by adopting organic foam, and obtaining a biscuit through slurry coating and drying for multiple times; and S5, carrying out glue discharging and sintering on the biscuit obtained in the step S4 to obtain the foamed ceramic.
"a method for comprehensively utilizing waste aluminum ash and an aluminum ash forming block, which are provided by Zhu 28557 and the like, and have the following publication numbers: the main steps of CN109402672A "include: (1) mixing and stirring the aluminum ash with a binder and water to ensure that the aluminum ash has binding property; (2) extruding and molding the stirred aluminum ash in a mold; (3) separating the extruded and formed aluminum ash forming block from the mold for drying treatment; (4) mounting the dried aluminum ash forming block on a new anode and putting the aluminum ash forming block into a tank for use; (5) after the aluminum ash slag forming block is used for 28 days, the anode is consumed, the aluminum ash slag forming block and materials in the tank are mixed into a crusting block, and the consumed anode and the crusting block on the consumed anode are taken out; (6) crushing the crusting blocks to enable the particle size of the crusting blocks to be smaller than 44 micrometers and account for 18-30%; (7) and covering the crusting blocks meeting the granularity on a new anode to be used as an antioxidant and heat-insulating material.
The invention relates to a method for preparing polyaluminium chloride and coproducing refractory material by using aluminum ash, such as Lixipeng, and the like, and the publication number is as follows: CN 110040756A' uses waste aluminum ash and hydrochloric acid as raw materials, firstly screens the aluminum ash to recover simple substance aluminum, then pre-purifies the undersize, then mixes the pre-purified aluminum ash with hydrochloric acid to carry out leaching reaction, and carries out solid-liquid separation and washing to obtain filtrate and filter cake; the filter cake is dried, mixed, molded, dried and sintered to prepare a refractory material, and the filtrate is polymerized to prepare the polyaluminium chloride water purifying agent.
The method mainly aims at harmless treatment of aluminum ash, and although a part of patents (such as a method for preparing polyaluminium chloride and a refractory material by using aluminum ash) can also obtain high-value products of aluminum chloride, the method also has the problems of high treatment difficulty of acid leaching residues obtained after hydrochloric acid leaching and the like.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provide a method for preparing polyaluminium chloride by utilizing aluminium ash, based on the advantages of short flow, easy separation of products, easy comprehensive utilization of tailings and the like of the chlorine metallurgy technology, and the harmless utilization of valuable components in the aluminium ash is realized by utilizing the procedures of pellet preparation, chlorination, aluminium chloride solution polymerization and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing polyaluminium chloride by using aluminium ash comprises the following steps:
(1) mixing aluminum ash and coke according to a weight ratio of 1: (0.05-0.3), mixing to form a mixed solid phase, and adding a binder into the mixed solid phase, wherein the binder is added in an amount of, by mass: 10 parts of binder: (1-2) preparing pellets of 5-20 mm;
(2) adding pellets from the top end of a moving bed reactor, adding chlorine gas with the volume concentration of 35-100% from the bottom of the moving bed reactor, reacting the pellets and the chlorine gas in the reactor for 5-60 min at the reaction temperature of 700-1100 ℃, and obtaining a chlorination product, wherein the chlorination product comprises a solid phase and a gas phase, and the chlorine gas and aluminum in the aluminum ash are in a molar ratio of (1.5-3): 1, adding;
(3) and cooling the gas-phase product to obtain aluminum chloride, absorbing the aluminum chloride by clear water to obtain an aluminum chloride solution with the concentration of 300-600 g/L, adjusting the pH value of the aluminum chloride solution to 3-4 by using ammonia gas, curing the aluminum chloride solution at room temperature for 10-20 h, and drying the cured liquid-phase product to obtain the polyaluminum chloride product.
(4) The solid phase product is directly used as a raw material for preparing the snow-melting agent.
In the step (1), the aluminum ash comprises the following components in percentage by mass: 58.4% of Al, 8.88% of MgO, 0.502% of Cl0.5% of F, 0.28% of K, 11.4% of N, SiO20.58 percent, and the balance of oxygen and other impurities.
In the step (1), the binder is prepared from polyvinyl alcohol and water according to a volume ratio of (3-5) to 1.
In the step (2), the reaction of aluminum nitride, aluminum metal and aluminum oxide in the aluminum ash and chlorine gas in the chlorination process is as follows:
2AlN+3Cl2＝2AlCl3+N2(1)
Al2O3+1.5C+3Cl2＝2AlCl3+1.5CO2(2)
2Al+3Cl2＝2AlCl3(3)
in the step (2), a magnesium-containing phase (represented by a MgO form) in the aluminum ash reacts with chlorine gas in the chlorination process as follows:
MgO+0.5C+Cl2＝MgCl2+0.5CO2(4)
in the step (2), aluminum chloride, nitrogen and unreacted chlorine generated in the chlorination process enter a gas phase, the main component of the solid phase is magnesium chloride, wherein the gas phase product is directly absorbed by clear water, and the chlorine is returned to the step (1) for reuse.
In the step (3), the polyaluminium chloride product contains 26.4-31% of alumina, has the basicity of 52-71% and is earthy yellow.
In the step (4), the content of magnesium chloride in the solid-phase product is 91.23-94.15%.
In the method, the recovery rate of aluminum in the aluminum ash is 91.02-94.17%.
The invention has the beneficial effects that:
(1) the method adopts a chlorination mode to directly realize the high-efficiency separation of the three components of aluminum, magnesium and nitrogen in the aluminum ash, the magnesium directly enters a slag phase, the aluminum chloride and the nitrogen enter a gas phase, and the nitrogen and the aluminum chloride products can be respectively obtained after the temperature is reduced, thereby belonging to a short-flow utilization process;
(2) the aluminum chloride product obtained by the method can be directly used for preparing polyaluminum chloride products, so that high-value utilization is realized;
(3) the main component of the tailings generated by the method is magnesium chloride, and the tailings can be directly used as a raw material for preparing the snow-melting agent, so that harmless utilization is realized.
Description of the drawings:
FIG. 1 is a process flow diagram of a method for preparing polyaluminum chloride from aluminum ash according to an embodiment of the present invention.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
The aluminum ash adopted by the embodiment of the invention comprises the main components of Al-58.4%, MgO-8.88%, Cl-0.502%, F-0.5%, K-0.28%, N-11.4%, and SiO2-0.58% and the balance oxygen and other impurities;
the embodiment of the invention adopts coke with main components of fixed carbon of-59.52 percent, volatile component of-33.6 percent, ash content of-4.9 percent and other impurities as the rest components.
The raw materials adopted in the embodiment of the invention are aluminum ash, the production method of the invention is not limited to the adoption of the raw materials, and any raw material taking aluminum as a main component can be produced by adopting the technology.
In the embodiment of the invention, coke is added in the carbonization process, the production method is not limited to the adoption of the raw materials, and any additive taking carbon as a main component can be used as the additive of the technology.
A method for preparing polyaluminium chloride by using aluminium ash comprises the following steps:
(1) mixing aluminum ash and coke according to a weight ratio of 1: (0.05-0.3), mixing to form a mixed solid phase, and adding a binder into the mixed solid phase, wherein the binder is added in an amount of, by mass: 10 parts of binder: (1-2) preparing pellets of 5-20 mm;
(2) adding pellets from the top end of a moving bed reactor, adding chlorine gas with the volume concentration of 35-100% from the bottom of the moving bed reactor, reacting the pellets and the chlorine gas in the reactor for 5-60 min at the reaction temperature of 700-1100 ℃, and obtaining a chlorination product, wherein the chlorination product comprises a solid phase and a gas phase, and the chlorine gas and aluminum in the aluminum ash are in a molar ratio of (1.5-3): 1, adding;
(3) and cooling the gas-phase product to obtain aluminum chloride, absorbing the aluminum chloride by clear water to obtain an aluminum chloride solution with the concentration of 300-600 g/L, adjusting the pH value of the aluminum chloride solution to 3-4 by using ammonia gas, curing the aluminum chloride solution at room temperature for 10-20 h, and drying the cured liquid-phase product to obtain the polyaluminum chloride product.
(4) The solid phase product is directly used as a raw material for preparing the snow-melting agent.
In the step (1), the aluminum ash comprises the following components in percentage by mass: 58.4% of Al, 8.88% of MgO, 0.502% of Cl0.5% of F, 0.28% of K, 11.4% of N, SiO20.58 percent, and the balance of oxygen and other impurities.
In the step (1), the binder is prepared from polyvinyl alcohol and water according to a volume ratio of (3-5) to 1.
In the step (2), the reaction of aluminum nitride, aluminum metal and aluminum oxide in the aluminum ash and chlorine gas in the chlorination process is as follows:
2AlN+3Cl2＝2AlCl3+N2(1)
Al2O3+1.5C+3Cl2＝2AlCl3+1.5CO2(2)
2Al+3Cl2＝2AlCl3(3)
in the step (2), a magnesium-containing phase (represented by a MgO form) in the aluminum ash reacts with chlorine gas in the chlorination process as follows:
MgO+0.5C+Cl2＝MgCl2+0.5CO2(4)
in the step (2), aluminum chloride, nitrogen and unreacted chlorine generated in the chlorination process enter a gas phase, the main component of the solid phase is magnesium chloride, wherein the gas phase product is directly absorbed by clear water, and the chlorine is returned to the step (1) for reuse.
In the step (3), the polyaluminium chloride product contains 26.4-31% of alumina, has the basicity of 52-71% and is earthy yellow.
In the step (4), the content of magnesium chloride in the solid-phase product is 91.23-94.15%.
In the method, the recovery rate of aluminum in the aluminum ash is 91.02-94.17%.
Example 1
A method for preparing polyaluminium chloride by using aluminium ash is shown in a process flow diagram in figure 1 and comprises the following steps:
mixing aluminum ash and coke according to a weight ratio of 1: 0.3, adding a binder into the mixed solid phase, wherein the binder is prepared from polyvinyl alcohol and water in a volume ratio of 4:1, the adding amount of the binder is 200g per kilogram of the mixed solid phase, and preparing pellets with the diameter of 20mm by using pellet grade. Adding the pellets into the top of a moving bed reactor, adding chlorine gas with the volume concentration of 100% from the bottom, reacting the pellets and the chlorine gas in the reactor for 60min at the reaction temperature of 700 ℃, wherein the mol ratio of the chlorine gas to aluminum in the aluminum ash is 1.5: 1 is added. After chlorination, the main component of the gas-phase product is aluminum chloride, the aluminum chloride product obtained after cooling is mixed with water to obtain an aluminum chloride solution with the concentration of 600g/L, the pH value is adjusted to 4 by ammonia gas, the mixture is aged for 10 hours at room temperature, the aged liquid-phase product is dried to obtain a polyaluminum chloride product, the content of alumina in the polyaluminum chloride product is 28.87%, the basicity is 68%, and the polyaluminum chloride product is earthy yellow. After treatment, the recovery rate of aluminum in the aluminum ash is 92.31 percent, the content of magnesium chloride in the solid-phase product is 94.15 percent, and the aluminum ash can be directly used as a raw material for preparing the snow-melting agent.
Example 2
A method for preparing polyaluminium chloride by using aluminium ash is shown in a process flow diagram in figure 1 and comprises the following steps:
mixing aluminum ash and coke according to a weight ratio of 1: 0.05, adding a binder into the mixed solid phase, wherein the binder is prepared from polyvinyl alcohol and water in a volume ratio of 4:1, the adding amount of the binder is 100g per kilogram of the mixed solid phase, and preparing 5mm pellets by using a pellet grade. Adding the pellets into the top of a moving bed reactor, adding chlorine gas (the rest components are oxygen) with the volume concentration of 35% from the bottom, reacting the pellets and the chlorine gas in the reactor for 5min at the reaction temperature of 1100 ℃, wherein the mol ratio of the chlorine gas to aluminum in the aluminum ash is 3: 1 is added. After chlorination, the main component of the gas-phase product is aluminum chloride, the aluminum chloride product obtained after cooling is mixed with water to obtain an aluminum chloride solution with the concentration of 300g/L, the pH value is adjusted to 3 by ammonia gas, the mixture is aged at room temperature for 20 hours, and the aged liquid-phase product is dried to obtain a polyaluminum chloride product, wherein the content of aluminum oxide in the polyaluminum chloride product is 26.8 percent, the basicity is 52 percent, and the polyaluminum chloride product is earthy yellow. After treatment, the recovery rate of aluminum in the aluminum ash is 91.02%, the content of magnesium chloride in the solid-phase product is 91.23%, and the aluminum ash can be directly used as a raw material for preparing a snow-melting agent.
Example 3
A method for preparing polyaluminium chloride by using aluminium ash is shown in a process flow diagram in figure 1 and comprises the following steps:
mixing aluminum ash and coke according to a weight ratio of 1: 0.1, adding a binder into the mixed solid phase, wherein the binder is prepared from polyvinyl alcohol and water in a volume ratio of 4:1, the adding amount of the binder is 150g per kilogram of the mixed solid phase, and preparing 10mm pellets by using pellet grade. Adding the pellets into the top of a moving bed reactor, adding chlorine gas (the rest components are oxygen) with the volume concentration of 65% from the bottom, reacting the pellets and the chlorine gas in the reactor for 30min at the reaction temperature of 1000 ℃, wherein the mol ratio of the chlorine gas to aluminum in the aluminum ash is 2: 1 is added. After chlorination, the main component of the gas-phase product is aluminum chloride, the aluminum chloride product obtained after cooling is mixed with water to obtain an aluminum chloride solution with the concentration of 400g/L, the pH value is adjusted to 3.5 by ammonia gas, the mixture is aged for 15 hours at room temperature, and the aged liquid-phase product is dried to obtain a polyaluminum chloride product, wherein the content of aluminum oxide in the polyaluminum chloride product is 28.55 percent, the basicity is 67 percent, and the polyaluminum chloride product is earthy yellow. After treatment, the recovery rate of aluminum in the aluminum ash is 92.11 percent, the content of magnesium chloride in the solid-phase product is 91.58 percent, and the aluminum ash can be directly used as a raw material for preparing the snow-melting agent.
Example 4
A method for preparing polyaluminium chloride by using aluminium ash is shown in a process flow diagram in figure 1 and comprises the following steps:
mixing aluminum ash and coke according to a weight ratio of 1: 0.2, adding a binder into the mixed solid phase, wherein the binder is prepared from polyvinyl alcohol and water in a volume ratio of 4:1, the adding amount of the binder is 200g per kilogram of the mixed solid phase, and preparing pellets with the diameter of 15mm by using pellet grade. Adding the pellets into the top of a moving bed reactor, adding chlorine gas (the rest is oxygen) with the volume concentration of 85% from the bottom, reacting the pellets and the chlorine gas in the reactor for 45min at the reaction temperature of 950 ℃, wherein the mol ratio of the chlorine gas to aluminum in the aluminum ash is 2.5: 1 is added. After chlorination, the main component of the gas-phase product is aluminum chloride, the aluminum chloride product obtained after cooling is mixed with water to obtain an aluminum chloride solution with the concentration of 500g/L, the pH value is adjusted to 4 by ammonia gas, the mixture is aged for 18h at room temperature, and the aged liquid-phase product is dried to obtain a polyaluminum chloride product, wherein the content of aluminum oxide in the polyaluminum chloride product is 30.9 percent, the basicity is 71 percent, and the polyaluminum chloride product is earthy yellow. After treatment, the recovery rate of aluminum in the aluminum ash is 94.17 percent, and the content of magnesium chloride in the solid-phase product is 93.61 percent, so that the aluminum ash can be directly used as a raw material for preparing the snow-melting agent.
Example 5
A method for preparing polyaluminium chloride by using aluminium ash is shown in a process flow diagram in figure 1 and comprises the following steps:
mixing aluminum ash and coke according to a weight ratio of 1: 0.3, adding a binder into the mixed solid phase, wherein the binder is prepared from polyvinyl alcohol and water in a volume ratio of 4:1, the adding amount of the binder is 100g per kilogram of the mixed solid phase, and preparing 5mm pellets by using a pellet grade. Adding the pellets into the top of a moving bed reactor, adding chlorine gas (the rest components are oxygen gas) with the volume concentration of 90% from the bottom, reacting the pellets and the chlorine gas in the reactor for 60min at the reaction temperature of 900 ℃, wherein the mol ratio of the chlorine gas to aluminum in the aluminum ash is 1.8: 1 is added. After chlorination, the main component of the gas-phase product is aluminum chloride, the aluminum chloride product obtained after cooling is mixed with water to obtain an aluminum chloride solution with the concentration of 500g/L, the pH value is adjusted to 4 by ammonia gas, the mixture is aged for 15 hours at room temperature, and the aged liquid-phase product is dried to obtain a polyaluminum chloride product, wherein the content of aluminum oxide in the polyaluminum chloride product is 28.11 percent, the basicity is 65 percent, and the polyaluminum chloride product is earthy yellow. After treatment, the recovery rate of aluminum in the aluminum ash is 92.08 percent, the content of magnesium chloride in the solid-phase product is 92.42 percent, and the aluminum ash can be directly used as a raw material for preparing the snow-melting agent.
Claims (7)
1. A method for preparing polyaluminium chloride by using aluminium ash is characterized by comprising the following steps:
(1) mixing aluminum ash and coke according to a weight ratio of 1: (0.05-0.3), mixing to form a mixed solid phase, and adding a binder into the mixed solid phase, wherein the binder is added in an amount of, by mass: 10 parts of binder: (1-2) preparing pellets of 5-20 mm;
(2) adding pellets from the top end of a moving bed reactor, adding chlorine gas with the volume concentration of 35-100% from the bottom of the moving bed reactor, reacting the pellets and the chlorine gas in the reactor for 5-60 min at the reaction temperature of 700-1100 ℃, and obtaining a chlorination product, wherein the chlorination product comprises a solid phase and a gas phase, and the chlorine gas and aluminum in the aluminum ash are in a molar ratio of (1.5-3): 1, adding;
(3) cooling the gas-phase product to obtain aluminum chloride, absorbing the aluminum chloride by clear water to obtain an aluminum chloride solution with the concentration of 300-600 g/L, adjusting the pH value of the aluminum chloride solution to 3-4 by using ammonia gas, curing the aluminum chloride solution at room temperature for 10-20 h, and drying the cured liquid-phase product to obtain a polyaluminum chloride product;
(4) the solid phase product is directly used as a raw material for preparing the snow-melting agent.
2. The method for preparing polyaluminum chloride from aluminum ash according to claim 1, wherein in the step (1), the aluminum ash comprises the following components in percentage by mass: 58.4 percent of Al, 8.88 percent of MgO, 0.502 percent of Cl, 0.5 percent of F, 0.28 percent of K, 11.4 percent of N, and SiO20.58 percent, and the balance of oxygen and other impurities.
3. The method for preparing polyaluminum chloride from aluminum ash as claimed in claim 1, wherein in the step (1), the binder is prepared from polyvinyl alcohol and water in a volume ratio of (3-5): 1.
4. The method for preparing polyaluminum chloride from aluminum ash as claimed in claim 1, wherein in step (2), aluminum chloride, nitrogen and unreacted chlorine generated in the chlorination process enter into gas phase, the solid phase component is magnesium chloride, and the chlorine is returned to step (1) for reuse.
5. The method for preparing polyaluminum chloride from aluminum ash as claimed in claim 1, wherein in step (3), the polyaluminum chloride product has an alumina content of 26.4-31%, a basicity of 52-71%, and an earthy yellow color.
6. The method for preparing polyaluminum chloride from aluminum ash as claimed in claim 4, wherein in the step (4), the content of magnesium chloride in the solid-phase product is 91.23-94.15%.
7. The method for preparing polyaluminum chloride from aluminum ash according to claim 1, wherein the recovery rate of aluminum in the aluminum ash is 91.02-94.17%.
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| CN115504494A (en) * | 2022-09-14 | 2022-12-23 | 江苏柏环环境科技有限公司 | Salt-containing solid waste resource recovery method |
| CN115672931A (en) * | 2022-09-14 | 2023-02-03 | 江苏柏环环境科技有限公司 | Recycling method of aluminum-containing solid waste |
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