CN112340759A - Method for preparing polyaluminum chloride and recovering silicon simple substance by using secondary aluminum ash - Google Patents
Method for preparing polyaluminum chloride and recovering silicon simple substance by using secondary aluminum ash Download PDFInfo
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- CN112340759A CN112340759A CN202011134792.3A CN202011134792A CN112340759A CN 112340759 A CN112340759 A CN 112340759A CN 202011134792 A CN202011134792 A CN 202011134792A CN 112340759 A CN112340759 A CN 112340759A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 87
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 38
- 239000000126 substance Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 28
- 239000010703 silicon Substances 0.000 title claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 229910000676 Si alloy Inorganic materials 0.000 claims abstract description 15
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000002386 leaching Methods 0.000 claims abstract description 9
- 230000009615 deamination Effects 0.000 claims abstract description 8
- 238000006481 deamination reaction Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010612 desalination reaction Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 abstract description 14
- 239000002699 waste material Substances 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 5
- 238000005266 casting Methods 0.000 abstract description 4
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- GCSPEDBBNOCYOD-UHFFFAOYSA-M aluminum;oxygen(2-);chloride Chemical compound [O-2].[Al+3].[Cl-] GCSPEDBBNOCYOD-UHFFFAOYSA-M 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to the field of waste resource recycling in the aluminum-silicon alloy casting industry, and particularly relates to a method for preparing polyaluminium chloride by using secondary aluminum ash and recycling a silicon simple substance, which comprises the following steps: s1, carrying out ball milling and screening on secondary aluminum ash of the aluminum-silicon alloy, wherein oversize products are used for recovering simple aluminum, and undersize products are used as raw materials; s2, dispersing the undersize obtained in the step S1 in water for alkali catalytic deamination and desalination treatment to obtain pretreated aluminum ash; s3, reacting the pretreated aluminum ash obtained in the step S2 with hydrochloric acid, and then carrying out solid-liquid separation to obtain polyaluminum chloride and filter residues; s4, dispersing the filter residue obtained in the step S3 in a hydrochloric acid solution again for high-pressure acid leaching, then carrying out solid-liquid separation, and washing and drying the filter residue to obtain the silicon simple substance. The method realizes the resource treatment of the filter residue of the polyaluminium chloride prepared from the secondary aluminium ash under the low temperature condition, and has remarkable social and economic benefits.
Description
Technical Field
The invention belongs to the field of waste resource recycling in the aluminum-silicon alloy casting industry, and particularly relates to a method for preparing polyaluminium chloride and recycling a silicon simple substance by utilizing aluminum-silicon alloy aluminum ash.
Background
The aluminum ash is a solid substance containing metallic aluminum and other components generated in the processes of electrolytic aluminum production and casting of aluminum alloy, waste aluminum recovery and regeneration and the like. Because the aluminum ash contains toxic and harmful substances to the environment, the aluminum ash is listed as non-ferrous metal smelting waste (HW48) in the national hazardous waste list, and the hazardous property is toxicity (T). According to the different content of metal aluminum in the aluminum ash, the aluminum ash is divided into primary aluminum ash and secondary aluminum ash. The primary aluminum ash contains high simple substance aluminum content, the content of metal aluminum is generally 50-70%, and the primary aluminum ash is also called lime. The production waste manufacturer can treat the primary aluminum ash to recover the simple substance aluminum, and the waste after the simple substance aluminum is extracted is the secondary aluminum ash. The components of the aluminum ash have certain differences due to different generation raw materials and production processes.
The aluminum-silicon alloy is an important member in the aluminum alloy industry, has the advantages of light specific gravity, small expansion coefficient, good wear resistance, strong corrosion resistance and the like, and is widely applied to the fields of aerospace, automobiles and the like. A large amount of aluminum ash is also generated in the production and casting processes of the aluminum-silicon alloy, and the generated aluminum ash is treated by processes such as ash frying and the like to obtain secondary aluminum ash. The secondary aluminum ash contains simple substance aluminum, aluminum oxide, aluminum nitride, salts and fluoride, and also contains simple substance silicon, wherein the simple substance aluminum, the aluminum oxide, the aluminum nitride and the simple substance silicon have important economic value.
The preparation of the polyaluminium chloride by using the secondary aluminium ash is the most widely used method of the secondary aluminium ash:
chinese patent CN109534466A discloses a method for preparing a water purifying agent containing polyaluminium chloride from aluminium ash, wherein the aluminium ash is firstly ball-milled and uniformly mixed with calcium carbonate or calcium oxide, then the mixture is roasted at 850-1200 ℃ in an oxidizing atmosphere to obtain calcium aluminate, and the calcium aluminate reacts with hydrochloric acid to obtain the polyaluminium chloride. The patent solves the problems of flammability and explosiveness of hydrogen discharged by hydrolysis or acidolysis of metal aluminum and the problem of activation of alpha-alumina. However, the patent requires high-temperature roasting in an oxidizing atmosphere to obtain calcium aluminate, and the investment and operation costs are high.
Chinese patent CN110040756A discloses a method for preparing polyaluminium chloride and a refractory material by using aluminium ash, wherein an aluminium-containing solution and high-purity powder are prepared by primary purification and deep purification, and the polyaluminium chloride and the refractory material are respectively prepared, so that resource utilization of the aluminium ash is realized. But 1300-1700 ℃ is needed for preparing refractory bricks, and the investment and operation cost is high.
Chinese patent CN110194474A discloses a process for producing polyaluminium chloride and calcium aluminate by using aluminium ash, which comprises the steps of carrying out deamination and F removal treatment on the aluminium ash, then carrying out a reaction with acid to obtain polyaluminium chloride, mixing the obtained filter residue with calcium-based auxiliary materials, drying and carrying out a high-temperature reaction to obtain the calcium aluminate. The high temperature reaction of calcium aluminate also has the problem of high investment and cost operation cost.
Chinese patent CN110467209A discloses a process for preparing high-purity calcium aluminate and polyaluminium chloride, which uses industrial waste hydrochloric acid and secondary aluminium ash as raw materials to produce calcium aluminate and polyaluminium chloride, and solves the problems of acid waste liquid discharge and aluminium ash pollution. However, the filter residue obtained in the production of the polyaluminium chloride in the patent can be reacted at the high temperature of 1100-1700 ℃ to obtain the calcium aluminate powder, and the investment and operation cost is high.
The method for preparing polyaluminium chloride by using secondary aluminium ash containing aluminium ash in the prior art has the following main defects:
1. the filter residue is used for preparing refractory bricks, the high temperature of 1300-1700 ℃ is required, and the equipment investment and the operation cost are high;
2. the calcium aluminate material obtained by mixing the filter residue or the aluminum ash with calcium-based materials such as calcium oxide, calcium carbonate and the like through high-temperature reaction also needs the high temperature of 850 ℃ and 1700 ℃, and the equipment investment and the operation cost are high.
Disclosure of Invention
In view of the above, the invention provides a method for treating filter residue of polyaluminium chloride from aluminum ash by using a low-temperature wet process at 130-160 ℃ to remove insoluble alpha-Al at normal temperature from the filter residue, aiming at the problems of high equipment investment and high energy consumption in the prior art of high-temperature pyrogenic process for treating the filter residue of polyaluminium chloride from aluminum ash2O3And converting the spinel into polyaluminium chloride and recovering the simple substance silicon in the aluminum-silicon alloy aluminum ash. The simple substance silicon can be directly sold as a product, and the product value is high. The low-temperature wet process at 130-160 ℃ has low equipment investment and operation cost, and has good economic and social benefits.
The technical scheme of the invention is as follows:
a method for preparing polyaluminium chloride by using secondary aluminum ash and recovering a silicon simple substance is characterized by comprising the following steps:
s1, carrying out ball milling and screening on secondary aluminum ash of the aluminum-silicon alloy, wherein oversize products are used for recovering simple aluminum, and undersize products are used as raw materials;
s2, dispersing the undersize obtained in the step S1 in water for alkali catalytic deamination and desalination treatment to obtain pretreated aluminum ash;
s3, reacting the pretreated aluminum ash obtained in the step S2 with hydrochloric acid, and then carrying out solid-liquid separation to obtain polyaluminum chloride and filter residues;
s4, dispersing the filter residue obtained in the step S3 in a hydrochloric acid solution again for high-pressure acid leaching, then carrying out solid-liquid separation, and washing and drying the filter residue to obtain the silicon simple substance.
Further, in the step S4, the filtrate and washing liquid obtained by the treatment are returned to the step S3 for adjusting the acid.
Further, in the step S1, the mesh number of the screen used is 100-200 meshes.
Further, in the step S2, the concentration of the alkali used for alkali catalysis is 0.5-1.5%, the liquid-solid ratio is 5-10:1, the temperature is 70-90 ℃ during treatment, and the time is 2-6 h.
Further, in the step S3, the liquid-solid ratio of the reaction is 5-10:1, the concentration of hydrochloric acid is 15% -25%, the temperature is 60-90 ℃, and the reaction time is 1-3 h.
Further, in the step S4, the liquid-solid ratio of the reaction is 3-5:1, the hydrochloric acid concentration is 15% -20%, and the temperature is 130-.
Further, in the step S4, the reaction pressure is 0.3-0.5MPa, and the reaction time is 2-4 h.
In the invention, the simple substance aluminum has the characteristic of good ductility, and the secondary aluminum ash has poor ductility of aluminum oxide, aluminum nitride, salt and the like, and most of the simple substance aluminum in the secondary aluminum ash can be recycled by utilizing the characteristic through a ball milling and screening method. The aluminum nitride contained in the ball-milled undersize reacts with water to generate ammonia gas and aluminum hydroxide, the ammonia gas generated under the alkaline condition is easy to remove, and the sieveSalts such as sodium chloride, potassium chloride and the like contained in the waste are very easy to dissolve in water, and ammonia and salts in the secondary aluminum ash can be removed by using a method of alkali-catalyzed water immersion by utilizing the characteristics; the secondary aluminum ash after deaminizing and desalting contains simple substance aluminum, aluminum hydroxide and aluminum oxide which are easily dissolved in acid, and most of the aluminum ash can be leached by utilizing a normal-pressure acid leaching mode. And the substances which are difficult to leach by atmospheric acid leaching: such as alpha-Al2O3Spinel, etc. under a certain acidity of hydrochloric acid, temperature and pressure, it is easy to leach out to obtain aluminium chloride. The silicon simple substance contained in the aluminum ash alloy has poor chemical activity and cannot react with hydrochloric acid at normal temperature, normal pressure, high temperature and high pressure, so that the silicon simple substance can be recovered by using a low-temperature wet process.
The invention utilizes the conventional acid dissolution and low-temperature wet process technology of 160 ℃ at 130 ℃ to treat the secondary aluminum ash of the aluminum-silicon alloy, prepare the polyaluminum chloride and recover the silicon simple substance. The secondary aluminum ash of the aluminum-silicon alloy is subjected to ball milling and screening, catalytic water leaching and normal-pressure acid leaching to obtain polyaluminum chloride, and filter residues are subjected to high-pressure acid leaching to obtain simple substance silicon, so that the resource utilization of the secondary aluminum ash of the aluminum-silicon alloy is realized.
The invention has the beneficial effects that:
the method provided by the invention has the advantages that simple substance aluminum is recycled by ball milling and screening, the obtained screen underflow is subjected to deamination and desalination through alkali catalysis pretreatment, the pretreated aluminum ash reacts with hydrochloric acid to obtain polyaluminium chloride, and then the simple substance silicon is recycled through a high-pressure acid leaching mode, so that the recycling treatment of the filter residue of the polyaluminium chloride prepared from secondary aluminum ash under a low-temperature condition is realized, and the method has remarkable social and economic benefits.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A method for preparing polyaluminium chloride by using secondary aluminum ash and recovering a silicon simple substance is characterized by comprising the following steps:
ball-milling secondary aluminum ash of the aluminum-silicon alloy, then sieving by using a 100-mesh sieve, dispersing undersize products in 1% aqueous alkali with the liquid-solid ratio of 5:1, reacting for 4 hours at 70 ℃, performing deamination and desalination treatment, and then performing solid-liquid separation; dissolving the filter residue in 15% hydrochloric acid with a liquid-solid ratio of 10:1, stirring at 60 ℃ for reaction for 3h, then carrying out solid-liquid separation, carrying out polymerization regulation on the filtrate to obtain polyaluminum chloride, dissolving the filter residue in 15% hydrochloric acid, stirring in a high-pressure reaction kettle at a liquid-solid ratio of 5:1 and a temperature of 130 ℃ and a pressure of 0.3MPa for reaction for 4h, then carrying out solid-liquid separation, and washing and drying the filter residue to obtain the simple substance silicon. The content of the obtained polyaluminium chloride-aluminum oxide is 9.22 percent, and the basicity is 51 percent.
Example 2
A method for preparing polyaluminium chloride by using secondary aluminum ash and recovering a silicon simple substance is characterized by comprising the following steps:
ball-milling secondary aluminum ash of the aluminum-silicon alloy, sieving by using a 150-mesh sieve, dispersing undersize products in 1.5% aqueous alkali with the liquid-solid ratio of 8:1, reacting for 3 hours at 80 ℃, performing deamination and desalination treatment, and then performing solid-liquid separation; dissolving the filter residue in 20% hydrochloric acid with a liquid-solid ratio of 8:1, stirring at 70 ℃ for reaction for 2h, then carrying out solid-liquid separation, carrying out polymerization regulation on the filtrate to obtain polyaluminum chloride, dissolving the filter residue in 18% hydrochloric acid, stirring in a high-pressure reaction kettle at a liquid-solid ratio of 3:1 and 150 ℃ and a pressure of 0.4MPa for reaction for 3h, then carrying out solid-liquid separation, and washing and drying the filter residue to obtain the simple substance silicon. The content of the obtained polyaluminium chloride-aluminum oxide is 10.53 percent, and the basicity is 60 percent.
Example 3
A method for preparing polyaluminium chloride by using secondary aluminum ash and recovering a silicon simple substance is characterized by comprising the following steps:
ball-milling secondary aluminum ash of the aluminum-silicon alloy, then sieving by using a 200-mesh sieve, dispersing undersize products in 0.5% aqueous alkali with the liquid-solid ratio of 10:1, reacting for 2h at 90 ℃, performing deamination and desalination treatment, and then performing solid-liquid separation; dissolving filter residues in 25% hydrochloric acid with the liquid-solid ratio of 5:1, stirring and reacting at 80 ℃ for 1h, then carrying out solid-liquid separation, carrying out polymerization regulation on the filtrate to obtain polyaluminum chloride, dissolving the filter residues in 20% hydrochloric acid, stirring and reacting in a high-pressure reaction kettle for 2h with the liquid-solid ratio of 3:1 and the pressure of 0.5MPa at 160 ℃, then carrying out solid-liquid separation, and washing and drying the filter residues to obtain the simple substance silicon. The content of the obtained polyaluminium chloride-aluminum oxide is 11.03 percent, and the basicity is 59 percent.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art. It should be noted that the technical features not described in detail in the present invention can be implemented by any prior art in the field.
Claims (7)
1. A method for preparing polyaluminium chloride by using secondary aluminum ash and recovering a silicon simple substance is characterized by comprising the following steps:
s1, carrying out ball milling and screening on secondary aluminum ash of the aluminum-silicon alloy, wherein oversize products are used for recovering simple aluminum, and undersize products are used as raw materials;
s2, dispersing the undersize obtained in the step S1 in water for alkali catalytic deamination and desalination treatment to obtain pretreated aluminum ash;
s3, reacting the pretreated aluminum ash obtained in the step S2 with hydrochloric acid, and then carrying out solid-liquid separation to obtain polyaluminum chloride and filter residues;
s4, dispersing the filter residue obtained in the step S3 in a hydrochloric acid solution again for high-pressure acid leaching, then carrying out solid-liquid separation, and washing and drying the filter residue to obtain the silicon simple substance.
2. The method for preparing polyaluminum chloride and recovering elemental silicon from secondary aluminum ash as claimed in claim 1, wherein in step S4, the filtrate and washing liquid obtained from the treatment are returned to step S3 for adjusting acid.
3. The method as claimed in claim 1, wherein in the step S1, the mesh size of the screen is 100-200 meshes.
4. The method for preparing polyaluminum chloride and recovering elemental silicon from secondary aluminum ash as claimed in claim 1, wherein in step S2, the concentration of alkali used for alkali catalysis is 0.5-1.5%, the liquid-solid ratio is 5-10:1, the temperature during treatment is 70-90 ℃ and the time is 2-6 h.
5. The method for preparing polyaluminum chloride and recovering elemental silicon from secondary aluminum ash as claimed in claim 1, wherein in step S3, the liquid-solid ratio of the reaction is 5-10:1, the concentration of hydrochloric acid is 15% -25%, the temperature is 60-90 ℃, and the reaction time is 1-3 h.
6. The method as claimed in claim 1, wherein the liquid-solid ratio of the reaction in step S4 is 3-5:1, the hydrochloric acid concentration is 15% -20%, and the temperature is 130-160 ℃.
7. The method for preparing polyaluminum chloride and recovering elemental silicon from secondary aluminum ash as claimed in claim 6, wherein in step S4, the reaction pressure is 0.3-0.5MPa and the reaction time is 2-4 h.
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| CN202011134792.3A CN112340759A (en) | 2020-10-21 | 2020-10-21 | Method for preparing polyaluminum chloride and recovering silicon simple substance by using secondary aluminum ash |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114655973A (en) * | 2022-04-27 | 2022-06-24 | 河南爱尔福克化学股份有限公司 | Method and device for recovering filter residue in polyaluminium chloride production |
| CN114772623A (en) * | 2022-03-30 | 2022-07-22 | 同济大学 | Method for continuously producing polyaluminum chloride by using aluminum ash |
| CN115159553A (en) * | 2022-07-20 | 2022-10-11 | 山东绿然环保科技有限公司 | Production process for preparing polyaluminum chloride by using secondary aluminum ash |
| CN115821057A (en) * | 2022-06-30 | 2023-03-21 | 湖南锐异资环科技有限公司 | Resourceful treatment method for cryolite-containing secondary aluminum ash |
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