CN112390264B - Method for improving desilication rate of coal gangue by aluminum ash catalysis - Google Patents
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Abstract
The invention discloses a method for improving the desilication rate of coal gangue by aluminum ash catalysis, which is used for treating hazardous waste aluminum ash generated in the processes of original aluminum casting, aluminum product processing and aluminum alloy regeneration and solid waste coal gangue generated in the coal industry, can comprehensively recover aluminum elements in the aluminum ash and aluminum and silicon elements in the coal gangue, can act on aluminum-silicon components in coal gangue raw materials by adding the aluminum ash as an additive, and can obviously improve the desilication rate of the coal gangue. Meanwhile, harmful substance aluminum nitride in the aluminum ash is converted into aluminum oxide at high temperature, so that harmless and resource utilization of the aluminum ash can be realized, and the high-alumina filter residue obtained after desiliconization of the mixed material can be used as a raw material for producing aluminum oxide by a sintering method, so that the resource utilization rate is improved; the filtrate sodium silicate solution contains caustic alkali and sodium silicate which can be used as a silicon source for producing the zeolite molecular sieve, thereby realizing harmless and resource utilization of two industrial wastes.
Description
Technical Field
The invention belongs to the field of resource utilization of industrial solid wastes, and particularly relates to a method for improving the desilication rate of coal gangue by catalyzing aluminum ash.
Background
China is a big country with large reserves of coal resources, and the yield of raw coal in China is 35.5 hundred million tons in 2018, which is increased by 5.2 percent on year-by-year basis. Due to the large amount of mining of coal resources, the poor management and the inadequate protection of mining areas and various unreasonable abusive mining behaviors, various serious problems of the coal resources in China are caused. The coal gangue occupies a large amount of land resources as solid waste generated in the coal mining process, and the stockpiling amount of the coal gangue exceeds 60 hundred million tons at present. Meanwhile, China is also a large country for producing raw aluminum and consuming aluminum products, and in 2018, the yield of raw aluminum in China is 3580 million tons, which accounts for 55 percent of the total yield of raw aluminum in the whole world. Aluminum ash is generated in the processes of original aluminum casting, aluminum product processing and aluminum alloy regeneration, millions of tons of aluminum ash is produced in China every year, and serious pollution problems can be caused when the aluminum ash is not treated, stockpiled and buried. At present, the aluminum ash is listed in the national hazardous waste list, and needs to be strictly controlled and properly treated. The abandonment of the coal gangue and the aluminum ash not only occupies land resources and pollutes the environment, but also greatly wastes the resources, and the comprehensive utilization rate is low, so that the environment is polluted, and the development of high-efficiency resource utilization technologies of industrial solid/hazardous wastes is urgently needed. Aiming at the current resource situation that domestic resources are gradually deficient and the ore grade is gradually reduced, the economic resource utilization of valuable components in the massive coal gangue solid waste is of great significance. The source of limiting the utilization of the aluminum-silicon-based solid wastes lies in that the prior art cannot effectively separate silicon-containing and aluminum-containing components, and the prior art has low separation efficiency and large loss ratio of valuable components.
The desilication treatment technology aiming at the aluminum-silicon separation of the coal gangue mainly comprises the following steps:
(1) acid desilication treatment (CN 103964482A, CN 104258804A, CN 107416852A): the acid desilication treatment usually adopts hydrochloric acid or sulfuric acid to convert aluminum-containing components in the coal gangue into aluminum salts for recovery, and the silicon-containing components enter acid residues and are recovered after alkali neutralization. The method has the main defects that the silicon-containing components enter acid sludge, the impurities are more, the purity is low, and the effective utilization is difficult; meanwhile, excessive alkali is required to be added for neutralization in the recovery of silicon components in the acid residue after aluminum extraction, and the cost is high.
(2) Alkaline desiliconization treatment (CN 107285341A, CN 107758713A, CN 108658088A): the alkali desiliconization treatment is usually carried out by mixing sodium carbonate or sodium bicarbonate with coal gangue according to a certain proportion, calcining at high temperature, dissolving calcined material out by water or dilute alkali liquor, and carrying out solid-liquid separation to obtain sodium silicate solution and residue containing aluminum components. The method has the main defects that the amount of the added sodium carbonate or sodium bicarbonate is too high in the high-temperature calcination process, and is usually 1-3 times of the mass of the coal gangue, so that the desilication cost of the coal gangue is greatly increased; meanwhile, the desilication rate of the coal gangue is only 40-50%, and the low desilication rate can cause low concentration of the sodium silicate solution and high silicon content in the slag.
At present, in the treatment technology of aluminum ash (CN 107555447A, CN 109127654A, CN 109052445A, and CN 108275708A), a wet method is mostly adopted to leach the aluminum ash in an aqueous solution, wherein harmful aluminum nitride is hydrolyzed and removed, and the leachate is evaporated to recover salts. The main disadvantages of the method are that harmful gas ammonia gas is released in the hydrolysis process of the harmful substance aluminum nitride in the aluminum ash, the environment is polluted, a large amount of alkaline waste water is generated, the evaporation cost of the leaching solution is high, and the economy is poor. Some patents directly add untreated aluminum ash into the electrolytic cell, but aluminum nitride in the aluminum ash has poor solubility in electrolyte, which can seriously affect various indexes of electrolysis.
Disclosure of Invention
The invention provides a method for improving the desilication rate of coal gangue by catalyzing aluminum ash, aiming at solving the problems of difficult separation of aluminum and silicon components in the coal gangue and low desilication rate, and the method comprises the following steps:
s1: mixing aluminum ash and coal gangue to form a mixed material, and calcining the mixed material in a calcining device to obtain a calcined product;
s2: grinding and soaking the calcined product in alkali liquor to obtain soaking slurry;
s3: and filtering the dipping slurry to obtain filter residue and filtrate.
The source of the aluminum ash and the coal gangue is not limited, and the aluminum ash and the coal gangue can be selected conventionally in the field, for example, the aluminum ash can be fine aluminum ash obtained after metal aluminum is extracted from molten salt dross generated in the processes of original aluminum casting, aluminum product processing and aluminum alloy regeneration; the coal gangue raw material can be a black grey rock which has lower carbon content and is harder than coal and is associated with a coal bed in a coal washing or coal forming process.
As an embodiment of the present invention, in step S1, the aluminum ash contains 40-50 wt% of Al2O325-30 wt% of AlN, 1-3 wt% of Al; the coal gangue contains 35-45 wt% of Al2O330-40% by weight of SiO21-3% by weight of Fe2O3(ii) a The ratio of aluminum to silicon of the coal gangue is 0.8-1.5.
The aluminum-silicon ratio is the ratio of the aluminum content to the silicon content in the coal gangue material based on the weight of the aluminum oxide and the silicon oxide.
The invention has no limitation on other components and contents in the aluminum ash and coal gangue, and can be selected conventionally in the field, and in one embodiment, the aluminum ash contains Al2O3AlN and Al, and may contain a small amount of fluoride and chloride; the coal gangue contains Al2O3、SiO2And Fe2O3Besides, CaO and MgO may be contained.
In step S1, the aluminum ash is used in an amount of 0.3 to 15 parts by weight based on 100 parts by weight of the coal gangue in the mixture.
As an embodiment of the present invention, in step S1, the calcining apparatus is a circulating fluidized bed calcining furnace; the conditions of the calcination treatment include: the temperature is 1000-1200 ℃, and the time is 30-120 min.
As an embodiment of the present invention, in step S2, the lye impregnation comprises: putting the ground calcined product into a sodium hydroxide and/or sodium carbonate solution, and soaking for 30-120min at 80-100 ℃;
the concentration of the sodium hydroxide and/or sodium carbonate solution is 90-120g/L, and the solid-to-liquid ratio of the impregnation is 200-400 g/L.
As an embodiment of the present invention, in step S3, the conditions of the filtering process include: the temperature is 80-90 deg.C, and the time is 5-10 min.
As an embodiment of the present invention, the method further comprises: and (5) leading the filtrate obtained in the step (S3) out of the system, and drying the filter residue.
As an embodiment of the invention, SiO is present in the filtrate2The concentration of (A) is 80-100g/L, Na2The concentration of O is 60-80g/L, Al2O3The concentration of (A) is 1-3 g/L.
The conditions of the drying treatment include: the temperature is 105-115 ℃, and the time is 60-120 min.
As an embodiment of the present invention, the method further comprises: the filter residue is used for producing alumina by a sintering method;
the filter residue is an aluminum-containing material, and the silicon-aluminum ratio of the aluminum-containing material can be 2.3-2.7.
As an embodiment of the present invention, the conditions of the sintering method include: the temperature is 1100 ℃ and 1200 ℃, and the time is 30-75 min.
As an embodiment of the present invention, the method further comprises: using the filtrate for the production of zeolite molecular sieves or for sale as a product; the filtrate is sodium silicate solution.
The technical scheme provided by the invention has the beneficial effects that at least:
the method is used for treating the hazardous waste aluminum ash generated in the processes of casting the raw aluminum, processing the aluminum product and regenerating the aluminum alloy and the solid waste coal gangue generated in the coal industry, can comprehensively recover the aluminum element in the aluminum ash and the aluminum and silicon elements in the coal gangue, can act on the aluminum-silicon component in the coal gangue raw material by adding the aluminum ash as an additive, and can obviously improve the desilication rate of the coal gangue. Meanwhile, harmful substance aluminum nitride in the aluminum ash is converted into aluminum oxide at high temperature, so that the aluminum ash can be harmlessly utilized and recycled, and the desiliconized filter residue of the mixed material can be used as a raw material for producing aluminum oxide by a sintering method, so that the resource utilization rate is improved; the filtrate sodium silicate solution contains caustic alkali and sodium silicate which can be used as a silicon source for producing the zeolite molecular sieve, thereby realizing harmless and resource utilization of two industrial wastes.
The technology simultaneously realizes the synergistic and efficient resource utilization of the aluminum ash and the coal gangue, and solves the problem of low desilication rate of the coal gangue. The method provided by the invention innovatively solves the major common problem of high-efficiency separation of aluminum and silicon components in the coal gangue and environmental pollution caused by hazardous waste of aluminum ash, and the material with the improved aluminum-silicon ratio can replace part of low-grade bauxite, so that the method has a wide industrial application prospect.
Compared with the traditional process, the process is simple, the addition of auxiliary materials such as sodium carbonate and the like is greatly reduced, the harmful substance aluminum nitride in the aluminum ash is converted into aluminum oxide by utilizing the self heat value of the coal gangue in the high-temperature calcination process, the harmless and resource utilization of the aluminum ash is realized, the used raw materials are industrial waste materials, the cost is low, and the obtained products such as sodium silicate and high aluminum-silicon ratio materials are high-value products. The whole treatment process of the invention has no discharge of harmful waste residues, waste liquid and waste gas, and realizes the high-efficiency utilization of silicon and aluminum components in industrial waste, thereby being a green and clean resource utilization technology for treating aluminum ash and coal gangue.
Drawings
FIG. 1 is a process flow diagram of the method for improving the desilication rate of coal gangue by using aluminum ash as a catalyst.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
As shown in FIG. 1, the aluminum ash used in the following examples was from a raw aluminum fusion casting process and had a composition of 46.2 wt.% Al2O328.7% by weight of AlN, 2.8% by weight of Al, 5.8% by weight of SiO22.6% by weight of Fe2O34.8% by weight of NaF, 3.8% by weight of CaF23.5% by weight of NaCl, 1.8% by weight of KCl; the coal gangue comes from coal washing process.
[ example 1 ]
Coal gangue (composition of 35.2 wt% Al) with Al/Si ratio of 0.91 was prepared by the method shown in FIG. 12O338.7% by weight of SiO22.1% by weight of Fe2O31.3 weight percent of CaO, 0.6 weight percent of MgO, and 22.1 weight percent of loss on ignition) and aluminum ash are uniformly mixed according to a certain proportion, wherein the aluminum ash and the aluminum ash are mixedThe mass ratio of the coal gangue is 1: 100; adding the mixed material into a circulating fluidized roasting furnace, carrying out high-temperature roasting at 1050 ℃, crushing the roasted mixed material, carrying out desiliconization treatment on the crushed mixed material under the conditions that the concentration of alkali liquor is 90g/L, the solid-liquid ratio is 350g/L, the desiliconization temperature is 85 ℃, the desiliconization time is 60 minutes, filtering to obtain a filtrate which is a sodium silicate solution, the ratio of aluminum to silicon of filter residues after desiliconization is 2.38, and the desiliconization rate is 61.8 weight percent.
[ example 2 ] A method for producing a polycarbonate
Coal gangue (30.2 wt% Al) with Al/Si ratio of 0.82 was mixed by the method shown in FIG. 12O336.8% by weight of SiO21.6% by weight of Fe2O30.7 weight percent of CaO, 1.1 weight percent of MgO, and 29.6 weight percent of loss on ignition) and aluminum ash are uniformly mixed according to a certain proportion, wherein the mass ratio of the aluminum ash to the coal gangue is 5: 100; adding the mixed material into a circulating fluidized roasting furnace, carrying out high-temperature roasting at 1100 ℃, crushing the calcined mixed material, carrying out desiliconization treatment on the crushed mixed material under the conditions that the concentration of alkali liquor is 100g/L, the solid-liquid ratio is 300g/L, the desiliconization temperature is 90 ℃, the desiliconization time is 90 minutes, filtering to obtain a filtrate which is a sodium silicate solution, the ratio of aluminum to silicon of filter residues after desiliconization is 2.57, and the desiliconization rate is 62.8 weight percent.
[ example 3 ]
Coal gangue (38.3 wt% Al) with Al/Si ratio of 1.07 is prepared by the method shown in FIG. 12O335.8% by weight of SiO21.8% by weight of Fe2O31.3 weight percent of CaO, 1.0 weight percent of MgO, and 21.8 weight percent of loss on ignition) and aluminum ash are uniformly mixed according to a certain proportion, wherein the mass ratio of the aluminum ash to the coal gangue is 10: 100; adding the mixed material into a circulating fluidized roasting furnace, carrying out high-temperature roasting at 1150 ℃, crushing the calcined mixed material, carrying out desiliconization treatment on the crushed mixed material under the conditions that the concentration of alkali liquor is 120g/L, the solid-liquid ratio is 250g/L, the desiliconization temperature is 95 ℃, the desiliconization time is 120 minutes, filtering to obtain a filtrate which is a sodium silicate solution, the ratio of aluminum to silicon of filter residues after desiliconization is 2.71, and the desiliconization rate is 60.5 weight percent.
[ example 4 ] A method for producing a polycarbonate
Coal Using the procedure of example 1The gangue desilication is different only in that: coal gangue (composition of 28.6 wt% Al)2O346.9% by weight of SiO21.1% by weight of Fe2O3CaO 0.5 wt%, MgO 0.3 wt%, loss on ignition 22.6 wt%) was 0.61. The ratio of aluminum to silicon of the filter residue after desiliconization is 1.32, and the desiliconization rate is 53.8 weight percent.
[ example 5 ]
The coal gangue desilication is carried out by adopting the method of the embodiment 1, and the difference is that: the mass ratio of the aluminum ash to the coal gangue is 20: 100. The ratio of aluminum to silicon of the filter residue after desiliconization is 1.65, and the desiliconization rate is 44.8 weight percent.
[ example 6 ]
The coal gangue desilication is carried out by adopting the method of the embodiment 1, and the difference is that: and adding the mixed material into a circulating fluidized roaster to carry out high-temperature calcination at 850 ℃. The ratio of aluminum to silicon of the filter residue after desiliconization is 1.59, and the desiliconization rate is 42.8 percent by weight.
[ example 7 ]
The coal gangue desilication is carried out by adopting the method of the embodiment 1, and the difference is that: and crushing the calcined mixture, and then carrying out desiliconization treatment on the mixture under the conditions that the concentration of alkali liquor is 70g/L, the solid-liquid ratio is 500g/L, the desiliconization temperature is 70 ℃, the desiliconization time is 30 minutes, the ratio of aluminum to silicon of filter residue after desiliconization is 1.55, and the desiliconization rate is 41.3 weight percent.
[ COMPARATIVE EXAMPLES ]
The coal gangue in the embodiment 1 is subjected to desilication treatment by adopting the prior art, specifically: coal gangue (composition of 35.2 wt% Al) with Al/Si ratio of 0.912O338.7% by weight of SiO22.1% by weight of Fe2O31.3 weight percent of CaO, 0.6 weight percent of MgO and 22.1 weight percent of loss on ignition) without adding any additive, calcining the mixture in a circulating fluidized roaster at 850 ℃, crushing the calcined mixture, and then carrying out desiliconization treatment under the conditions that the alkali liquor concentration is 60g/L, the solid-liquid ratio is 400g/L, the desiliconization temperature is 80 ℃ and the desiliconization time is 30 minutes, wherein the aluminum-silicon ratio of filter residue after desiliconization is 1.52, and the desiliconization rate is only 40.1 weight percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A method for improving the desilication rate of coal gangue by using aluminum ash as a catalyst is characterized by comprising the following steps:
s1: mixing aluminum ash and coal gangue to form a mixed material, and calcining the mixed material in a calcining device to obtain a calcined product;
s2: grinding and soaking the calcined product in alkali liquor to obtain soaking slurry;
s3: filtering the dipping slurry to obtain filter residue and filtrate;
in step S1, the aluminum ash contains 40-50 wt% of Al2O325-30 wt% of AlN, 1-3 wt% of Al; in the mixed material, the using amount of the aluminum ash is 0.3-15 parts by weight relative to 100 parts by weight of the coal gangue.
2. The method as claimed in claim 1, wherein in step S1, the coal refuse contains 35-45 wt% Al2O330-40% by weight of SiO21-3% by weight of Fe2O3(ii) a The ratio of aluminum to silicon of the coal gangue is 0.8-1.5.
3. The method of claim 1, wherein in step S1, the calcining apparatus is a circulating fluidized roaster; the conditions of the calcination treatment include: the temperature is 1000-1200 ℃, and the time is 30-120 min.
4. The method of claim 1, wherein in step S2, the lye impregnation comprises: putting the ground calcined product into a sodium hydroxide and/or sodium carbonate solution, and soaking for 30-120min at 80-100 ℃;
the concentration of the sodium hydroxide and/or sodium carbonate solution is 90-120g/L, and the solid-to-liquid ratio of the impregnation is 200-400 g/L.
5. The method according to claim 1, wherein in step S3, the conditions of the filtering process include: the temperature is 80-90 deg.C, and the time is 5-10 min.
6. The method of claim 1, further comprising: and (5) leading the filtrate obtained in the step (S3) out of the system, and drying the filter residue.
7. The method of claim 6, wherein the filtrate is SiO2The concentration of (A) is 80-100g/L, Na2The concentration of O is 60-80g/L, Al2O3The concentration of (A) is 1-3 g/L;
the conditions of the drying treatment include: the temperature is 105-115 ℃, and the time is 60-120 min.
8. The method of claim 1, further comprising: the filter residue is used for producing alumina by a sintering method;
the filter residue is an aluminum-containing material, and the silicon-aluminum ratio of the aluminum-containing material is 2.3-2.7; the conditions of the sintering process include: the temperature is 1100-1200 ℃, and the time is 30-75 min.
9. The method of claim 1, further comprising: using the filtrate for the production of zeolite molecular sieves or for sale as a product;
the filtrate is sodium silicate solution.
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| CN100572572C (en) * | 2008-04-17 | 2009-12-23 | 上海交通大学 | The method of utilizing aluminium ash and coal gangue composite wastes to produce aluminum silicon alloy |
| CN101734698B (en) * | 2009-09-08 | 2013-01-09 | 东北大学 | Method for preparing aluminum oxide from aluminiferous material |
| CN101759209B (en) * | 2010-01-20 | 2012-07-25 | 潘爱芳 | Method for extracting high purity alumina and silica gel from coal gangue |
| CN104445312B (en) * | 2014-10-30 | 2016-03-02 | 北京矿冶研究总院 | Method for extracting aluminum oxide by synergistic treatment of fly ash and coal gangue |
| WO2018166221A1 (en) * | 2017-03-17 | 2018-09-20 | 山东大学 | System and method for co-treating organic wastewater and industrial solid waste |
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