CN102674422A - Method for preparing flocculant liquid polyaluminum chloride from aluminum ash - Google Patents
Method for preparing flocculant liquid polyaluminum chloride from aluminum ash Download PDFInfo
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Abstract
The invention discloses a method for preparing flocculant liquid polyaluminum chloride from aluminum ash, belonging to the technical field of solid waste treatment environment protection. The method comprises the following steps: uniformly mixing and stirring aluminum ash and water in a volume ratio of 1:(3-5), and soaking for 5-8 hours; pumping the solution into a reaction kettle, adding hydrochloric acid and water in an aluminum ash/hydrochloric acid/water volume ratio of 1:(2.5-3.0):(3.0-4.0), and reacting at 85-100 DEG C for 2-3 hours; carrying out solid-liquid separation with a plate and frame type filter-press, and adding a regulator to regulate the aluminum oxide content and basicity of the liquid, wherein if quicklime is used as the regulator, the volume ratio of the liquid to the quicklime is 1:(0.054-0.086), if aluminum dust is used as the regulator, the volume ratio of the liquid to the aluminum dust is 1:(0.023-0.04), and if solid calcium aluminate is used as the regulator, the volume ratio of the liquid to the solid calcium aluminate is 1:(0.042-0.063); and standing and aging for 48-72 while controlling the temperature at 50-60 DEG C, thereby obtaining the liquid polyaluminum chloride finished product. The invention has the advantages of simple technique, low cost and no secondary pollution, and is a good method for recycling aluminum ash.
Description
Technical field
The present invention relates to the preparation method of flocculation agent liquid aluminium polychloride, especially relate to a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride.
Background technology
In aluminum smelting technology, moulding process, can produce multiple sub product.As the main sub product of aluminium processing industry, the aluminium ash results from all aluminium generation fused operations, and aluminium content wherein accounts for 1%~12% of total losses amount in the aluminium production use.Along with the expansion day by day of metallic aluminium range of application, the generation of aluminium ash also will grow proportionately.Past people is regarded the aluminium ash as waste residue and pile up like a mountain everywhere; Soil and ecotope have been caused very big pressure, can decomposite ammonia after the aluminium nitride AlN in the aluminium ash makes moist in addition in air, breath malodor is unpleasant; And toxic, also can cause bigger pollution to atmosphere.This measure not only causes aluminium resource waste also can bring environmental problem, and the problem of environmental pollution that the aluminium ash is caused has restricted further developing of aluminium processing industry, becomes a great problem that perplexs aluminium processing enterprise for many years.Therefore, seek cost-effective method and be used and administer the aluminium ash, not only will improve the economic benefit of aluminium industry, when realizing the resources effective recycle, also will produce significant effects the Sustainable development that realizes economy, society.
The concrete composition of aluminium ash is different different because of producing the path, mainly is made up of the mixture of metallic aluminium simple substance, oxide compound and salt flux.Wherein, metallic aluminium exists under the coating of aluminum oxide and aluminium nitride AlN.Concrete content is Al:10%~30%, Al
2O
3: 20%~40%, Si, Mg, Fe oxide compound: 7%~15%, the muriate of K, Na, Ca, Mg: 15%~30% with the trace fluorochemical and residue.In fact, contain higher renewable resources in the aluminium ash, single with aluminum oxide calculating, alumina content reaches 20%~40% approximately, if can be used, and turns waste into wealth, and not only has good economic benefit, and has good environment and ecological benefits.
At present existing people attempts utilizing aluminium ash processing aluminium salt, and main method is to adopt hydrochloric acid to process aluminium chlorohydroxide.Because the aluminum oxide phase inversion becomes αYang Hualv under the high temperature, is insoluble to bronsted lowry acids and bases bronsted lowry, therefore; This method has only been utilized a spot of metallic aluminium in the aluminium ash; A large amount of aluminum oxide is not utilized well, not only cause the waste of resource, and employed hydrochloric acid also can cause secondary pollution to environment.Simultaneously, from the aluminium ash, reclaim soluble salt (like fluoride salt and NaCI, KCI etc.) and mainly be, contain a large amount of soluble salts in this aluminium ash to the two secondary aluminiums ashes (grey black or salt-cake) that reclaim through molten-salt growth method behind the metallic aluminium.Its recovery method mainly is that method such as dissolving or employing electrodialysis or control pH value makes the salt dissolving in the aluminium ash under HTHP, then through filtering purification with its recovery.The shortcoming of this method is to produce a large amount of waste liquids, and the aluminium ash that extracts behind the soluble salt also can pollute as reclaiming without additive method.
In addition, the method with aluminium ash synthesizing aluminate (being mainly sodium aluminate and calcium aluminate) is that the aluminium ash behind the removal soluble salt is dissolved in NaOH, metallic aluminium in the aluminium ash and Al
2O
3Generate sodium aluminate with the NaOH reaction, filtering then purifies just can obtain the sodium aluminate product together.With the synthetic calcium aluminate of aluminium ash then is that aluminium ash and CaO are passed through high-temperature calcination together, finally obtains calcium aluminate.Its shortcoming is that the production technique power consumption is big, is prone to produce secondary pollution.
Also have the people from the aluminium ash, to reclaim aluminum oxide, in its production process during adding acid-respons controlled temperature about 90 ℃, sulfuric acid concentration 30%, the amount of dissolving in aluminium ash be 10% o'clock can stripping aluminium ash in 88% aluminum oxide.Though this method can reduce manufacturing cost of aluminum oxide, technology is complicated, can produce obnoxious flavoures such as ammonia, methane during washing, and produce a large amount of waste liquids, as not dealing carefully with environment is caused serious threat.
In addition, the somebody is a raw material synthetic water purification agent Tai-Ace S 150 with aluminium ash (mainly referring to two secondary aluminiums ash).Tai-Ace S 150 can remove impurity such as phosphoric acid salt in anhydrating, zinc, chromium, but and degerming, the color and the smell of control water.Its method is before aluminium ash and sulfuric acid reaction, to remove the soluble salt in the aluminium ash earlier, and the sour concentration of control is 50%, 90 ℃ of following stirring and dissolving 1 hour, and can be with 95% Al in the aluminium ash
2O
3Stripping.Its shortcoming is that the aluminium ash can produce obnoxious flavoures such as ammonia, hydrogen, methane with sulfuric acid reaction the time.
At last, also have the researchist to utilize aluminium ash synthetic fire resistive material and material of construction, as produce brown corundum, preparation fused corundom or magnesium aluminate spinel compoud, synthetic Sialon composite ceramics, produce ceramic gaged brick, be used for refractory castable and prefabricated section etc.Can also be used to pave the way etc.
In a word, contain the material that many meetings directly or indirectly work the mischief to environment in the aluminium ash, directly abandon and to cause environmental pollution.Simultaneously, the aluminium ash is again a kind of renewable resources with comprehensive utilization value, therefrom can reclaim aluminium, salt, and aluminum oxide also can synthesize water purification agent, can also be used for aspects such as refractory materials, road usefulness and material of construction, steel desulfurization agent.The recoverying and utilizing method of aluminium ash is a lot, should be according to practical situation comprehensive treating process as far as possible, and according to high-recovery, higher economic benefit with do not cause the principle of secondary pollution to select.Realize the comprehensive utilization of aluminium ash, can turn waste into wealth, protect environment, can reduce production cost of products again, demonstrate fully the theory of environmental protection.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride; Not only can effectively utilize aluminium ash preparation flocculation agent liquid aluminium polychloride; Can also eliminate of the pollution of aluminium ash effectively, and avoid in the course of processing, environment being caused secondary pollution environment.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, and it may further comprise the steps: 1. the aluminium ash is carried out mixing and stirring with water 1: 3 by volume~5, soaked 5~8 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in 1: 2.5~3.0: 3.0~4.0 the aluminium ashes after washing, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 85~100 ℃, reacts 2~3 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank; Add regulator and regulate liquid alumina content and basicity, as adopting unslaked lime, liquid: it is 1: 0.054~0.086 that unslaked lime adds volume ratio; If adopt the aluminium bits; Liquid: it is 1: 0.023~0.04 that the aluminium bits add volume ratio, if adopt the solid calcium aluminate, liquid: it is 1: 0.042~0.063 that the solid calcium aluminate adds volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 50~60 ℃, and the curing time is 48~72 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
1. aluminium ash and water 1: 3 by volume~5 are carried out mixing and stirring in step in, soaked 5~8 hours.
3. be the ash of aluminium by volume in step: hydrochloric acid: water is 1: 2.5~3.0: 3.0~4.0 in reaction kettle, to add hydrochloric acid and water, and the formation mixed solution stirs.
Step 4. in temperature of reaction kettle be set to 85~100 ℃, reacted 2~3 hours.
5. the gas that produces in reaction process in step adopts the absorption tower to absorb, and spray liquid adopts clear water, continues reaction in the absorption liquid back flow reaction still.
6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution in step in, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry.
7. be extraction isolated liquid to equalizing tank in step; Add regulator and regulate liquid alumina content and basicity, as adopting unslaked lime, liquid: it is 1: 0.054~0.086 that unslaked lime adds volume ratio; If adopt the aluminium bits; Liquid: it is 1: 0.023~0.04 that the aluminium bits add volume ratio, if adopt the solid calcium aluminate, liquid: it is 1: 0.042~0.063 that the solid calcium aluminate adds volume ratio.
8. will place plastic containers to leave standstill in step through the solution after regulating in, temperature be controlled at 50~60 ℃, and the curing time is 48~72 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
Compared with prior art; The invention has the advantages that and use a step acid pasting to extract the aluminium in the aluminium ash; Make aluminum oxide and pure aluminum and hydrochloric acid soln in the aluminium ash in self thermopositive reaction and generate aluminum chloride; Mixed solution with aluminum chloride carries out solid-liquid separation then, can prepare the inorganic polymer flocculant liquid aluminium polychloride through overregulating slaking.Not only method is simple, and is easy and simple to handle, and with respect to the existing working method of alum clay for feedstock production flocculant poly aluminum chloride of utilizing; Need not pulverize alum clay, with low cost, the whole aluminium compositions in the aluminium ash all can be extracted; Not only renewable resource can be made full use of, also secondary pollution can be do not produced.And the waste residue that solid-liquid separation obtains can be used as manufacture of cement addition material or brick-making raw material after air-dry, and back to nature can not cause any pollution to environment; What produce in the employing cold water spray absorption reaction process is the gas of major ingredient with HCl, and carries out continuing in the absorption liquid back flow reaction still reaction, effectively reuse, thus avoid process gas that environment is caused secondary pollution.Simultaneously, the liquid flocculant poly aluminum chloride that this process method is produced, traditional relatively solid polyaluminium chloride; Can be widely used in the industrial sewages processing such as papermaking, printing and dyeing, chemical industry, and need not prepare, promptly throw and promptly use; Flexibility is strong, uses conveniently, and technology is easier; Production cost is lower, and application prospect is wider.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing; Through instance the present invention is done further explain: present embodiment is being to implement under the prerequisite with technical scheme of the present invention; Provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment one: a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, and it may further comprise the steps: 1. the aluminium ash was carried out mixing and stirring in 1: 3 by volume with water, soaked 8 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in the aluminium ash after washing at 1: 2.5: 3.0, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 85 ℃, reacts 2.5 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank, add regulator and regulate liquid alumina content and basicity, adopt unslaked lime, liquid: it is 1: 0.062 that unslaked lime adds volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 50 ℃, and the curing time is 72 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
Embodiment two: a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, and it may further comprise the steps: 1. the aluminium ash was carried out mixing and stirring in 1: 4 by volume with water, soaked 7 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in the aluminium ash after washing at 1: 3.0: 4.0, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 90 ℃, reacts 3 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank, add regulator and regulate liquid alumina content and basicity, adopt the aluminium bits, liquid: it is 1: 0.04 that the aluminium bits add volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 60 ℃, and the curing time is 48 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
Embodiment three: a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, and it may further comprise the steps: 1. the aluminium ash was carried out mixing and stirring in 1: 5 by volume with water, soaked 5 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in the aluminium ash after washing at 1: 2.5: 3.5, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 100 ℃, reacts 2 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank, add regulator and regulate liquid alumina content and basicity, adopt the solid calcium aluminate, liquid: it is 1: 0.053 that the solid calcium aluminate adds volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 55 ℃, and the curing time is 60 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
Embodiment four: a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, and it may further comprise the steps: 1. the aluminium ash was carried out mixing and stirring in 1: 3.5 by volume with water, soaked 7.5 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in the aluminium ash after washing at 1: 2.8: 3.5, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 90 ℃, reacts 2.7 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank, add regulator and regulate liquid alumina content and basicity, adopt unslaked lime, liquid: it is 1: 0.076 that unslaked lime adds volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 50 ℃, and the curing time is 72 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
Embodiment five: a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, and it may further comprise the steps: 1. the aluminium ash was carried out mixing and stirring in 1: 4.5 by volume with water, soaked 6.5 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in the aluminium ash after washing at 1: 2.6: 3.2, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 100 ℃, reacts 2.5 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank, add regulator and regulate liquid alumina content and basicity, adopt the aluminium bits, liquid: it is 1: 0.035 that the aluminium bits add volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 60 ℃, and the curing time is 64 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
Embodiment six: a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, and it may further comprise the steps: 1. the aluminium ash was carried out mixing and stirring in 1: 5 by volume with water, soaked 5 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in the aluminium ash after washing at 1: 2.7: 3.8, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 85 ℃, reacts 2.9 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank, add regulator and regulate liquid alumina content and basicity, adopt the solid calcium aluminate, liquid: it is 1: 0.057 that the solid calcium aluminate adds volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 60 ℃, and the curing time is 48 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
Claims (8)
1. a method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride is characterized in that it may further comprise the steps: 1. the aluminium ash is carried out mixing and stirring with water 1: 3 by volume~5, soaked 5~8 hours; 2. extract supernatant liquid to settling tank, handle the back reuse, the remaining aluminium ash after washing is extracted to reaction kettle with pump; 3. aluminium ash by volume: hydrochloric acid: water is to add hydrochloric acid and water in 1: 2.5~3.0: 3.0~4.0 the aluminium ashes after washing, and the formation mixed solution stirs; 4. temperature of reaction kettle is set to 85~100 ℃, reacts 2~3 hours; 5. the gas that produces in the reaction process adopts the absorption tower to spray absorption, and spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle; 6. adopt plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution, can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry; 7. extract isolated liquid to equalizing tank; Add regulator and regulate liquid alumina content and basicity, as adopting unslaked lime, liquid: it is 1: 0.054~0.086 that unslaked lime adds volume ratio; If adopt the aluminium bits; Liquid: it is 1: 0.023~0.04 that the aluminium bits add volume ratio, if adopt the solid calcium aluminate, liquid: it is 1: 0.042~0.063 that the solid calcium aluminate adds volume ratio; 8. will place plastic containers to leave standstill through the solution after regulating, temperature be controlled at 50~60 ℃, and the curing time is 48~72 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
2. according to claims 1 described a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride, it is characterized in that during step 1. the aluminium ash being carried out mixing and stirring with water 1: 3 by volume~5, soaked 5~8 hours.
3. according to claims 1 described a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride; It is characterized in that 3. step is the ash of aluminium by volume: hydrochloric acid: water is 1: 2.5~3.0: 3.0~4.0 in reaction kettle, to add hydrochloric acid and water, and the formation mixed solution stirs.
4. according to the described a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride of claims 1, it is characterized in that temperature of reaction kettle is set to 85~100 ℃ during step is 4., reacted 2~3 hours.
5. according to claims 1 described a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride; It is characterized in that adopting the absorption tower to spray absorption the gas that produces in the reaction process during step 5.; Spray liquid adopts clear water, and absorption liquid is back to and continues reaction in the reaction kettle.
6. according to claims 1 described a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride; It is characterized in that adopting plate and frame(type)filter press to carry out solid-liquid separation reacted mixed solution during step 6., can be used as manufacture of cement addition material or brick-making raw material after waste residue is air-dry.
7. according to claims 1 described a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride; It is characterized in that step is 7. for extracting isolated liquid to equalizing tank; Add regulator and regulate liquid alumina content and basicity, as adopting unslaked lime, liquid: it is 1: 0.054~0.086 that unslaked lime adds volume ratio; If adopt the aluminium bits; Liquid: it is 1: 0.023~0.04 that the aluminium bits add volume ratio, if adopt the solid calcium aluminate, liquid: it is 1: 0.042~0.063 that the solid calcium aluminate adds volume ratio.
8. according to claims 1 described a kind of method of utilizing the aluminium ash to prepare the flocculation agent liquid aluminium polychloride; It is characterized in that to place plastic containers to leave standstill through the solution after regulating during step 8.; Temperature is controlled at 50~60 ℃; Curing time is 48~72 hours, promptly gets flocculation agent liquid aluminium polychloride finished product.
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