CN101817580A - Method for preparing silicoferrite-containing Al13 by utilizing aluminum ash slag - Google Patents

Method for preparing silicoferrite-containing Al13 by utilizing aluminum ash slag Download PDF

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CN101817580A
CN101817580A CN201010161274A CN201010161274A CN101817580A CN 101817580 A CN101817580 A CN 101817580A CN 201010161274 A CN201010161274 A CN 201010161274A CN 201010161274 A CN201010161274 A CN 201010161274A CN 101817580 A CN101817580 A CN 101817580A
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aluminium
solution
ash
polymerization
ferrosilicon
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李小忠
苏晓梅
刘兴
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Zhejiang Normal University CJNU
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Zhejiang Normal University CJNU
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Abstract

The invention relates to a method for preparing silicoferrite-containing Al13 by utilizing aluminum ash slag, which belongs to the technical field of harmless and resourceful treatment of wastes. The method is completed as follows: the method for preparing the silicoferrite-containing Al13 by utilizing the aluminum ash slag comprises the following steps: (1) uniformly mixing aluminum ash with Na2CO3, then placing in a furnace for calcination, and obtaining off-white powder; (2) placing the off-white powder into a container, and then adding hydrochloric acid for carrying out acid leaching reaction; (3) carrying out solid-liquid separation on acid-leached products, and obtaining sediments and solution containing Fe3+ and AlCl3; (4) adding alkaline solution into the obtained sediments for carrying out reaction, carrying out the solid-liquid separation and obtaining the sediments and Na2SiO3 solution; and (5) adding the Na2SiO3 solution into the AlCl3 solution, uniformly mixing, regulating the pH of the solution and obtaining the silicoferrite-containing Al13. The method has the advantages of simple process, less residue, low cost and less pollution.

Description

Utilize the preparation of aluminium lime-ash to contain the method for ferrosilicon polymerization 13 aluminium
Technical field
The present invention relates to the technical field of the innoxious and resource utilization of refuse, is a kind of method of utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium.
Technical background
Flocculant of polymeric aluminium chloride development and exploitation start from the Japan in the later stage sixties 20th century, after this, many research workers of states such as Europe, the U.S. and USSR (Union of Soviet Socialist Republics) have carried out a large amount of research and developments to its synthesis and preparation process, existing a large amount of both at home and abroad patents and bibliographical information the preparation technology of tens of kinds of polymerize aluminum chlorides and method commonly used have following several:
One, be the production method of raw material with aluminium, active aluminium sesquioxide or aluminium ash
With aluminium, active aluminium sesquioxide or aluminium ash is that the production technique of raw material has acid-soluble one-step, alkali solution technique and neutralisation.Wherein the product polymerize aluminum chloride content that makes of alkali solution technique and neutralisation is all lower, is difficult to apply, and the product polymerize aluminum chloride content that acid-soluble one-step makes is high slightly.Its principle is for to be dissolved in hydrochloric acid with a certain amount of aluminium or active aluminium sesquioxide, and along with the carrying out of reaction, the pH value of system raises gradually, and impels Al (H at a certain temperature 2O) 6 3+Hydrolysis and polyreaction take place, the polymeric aluminum chlorides solution that makes.But the polymerization degree of this method sintetics is generally below 40%, and SiO 2Reach the Al that is wrapped up by glass microballon 2O 3, Fe 2O 3Be not used effectively the discarded further contaminate environment of a large amount of residues Deng owing to be insoluble in acid.
Two, be the method for raw material with sodium aluminate or aluminium hydroxide.(day clear and 45-38121 of disclosure special permission; Clear and 53-1240)
Sodium aluminate or aluminium hydroxide and hydrochloric acid are reacted the generation polymerize aluminum chloride by a certain percentage in reactor.The working condition that this method is produced polymerize aluminum chloride requires High Temperature High Pressure, and cost is higher, and the Al in the product quality indicator 13Content can only reach 40～50%.
Three, with the aluminum chloride be the production method of raw material.Common method mainly contains following five kinds:
1, neutralisation
In aluminum trichloride solution, add alkaline matters such as sodium hydroxide, lime, Wingdale, yellow soda ash, improve the concentration of hydroxide ion, promoting the hydrolysis of aluminum chloride, different add alkali number and can obtain different basicity products.The actual production of this method is wayward, can not realize the stoichiometric(al) of suitable basicity and effective aluminium component, and quality product is stable inadequately, Al 13Content is lower.
2, thermal decomposition method
With the crystal aluminum chloride is raw material, also can adopt the boiling pyrolysis method to make solid PAC, crystal aluminum chloride is pyrolysis at a certain temperature, decomposite hydrogenchloride and water, polymerization becomes powdered product, and promptly PAC (grog) adds certain water gaging with grog and stirs, be solidified into the resinousness product within a short period of time, drying, pulverize get final product solid PAC product.This method investment of production equipment is big, and decomposition efficiency is lower, and easily produces aluminium sesquioxide, and the polymerization degree of product is generally below 50%.
3, electroosmose process
This method is to be electrolytic solution with the aluminum chloride, constitutes reaction chamber with two anion-exchange membranes (out-phase), and graphite cake is an anode, and monolithic porous is a negative electrode, and logical certain hour direct current promptly makes the PAC liquid product.Though this technology is advanced, the place one's entire reliance upon quality of ion-exchange membrane of this method complex process, the quality product of manufacturing exists easy generation film and pollute this thorny difficult problem, and the more expensive cost of PAC that causes of the price of film is higher.
4, resolvability aluminum anode electrolytic process
The Chinese Academy of Sciences has developed at ecological center a kind of technology of preparing of high-quality polymerize aluminum chloride, this technology is electrolytic solution with the aluminum chloride, and aluminium sheet is an anode, and iron plate is a negative electrode, lead to the low voltage of certain hour, the direct current of big electric current, can make the liquid product of polymerize aluminum chloride.Though its basicity is higher, its composition Al that effectively flocculates 13Massfraction is about 70%.But this method is to be anode with the aluminium sheet, most of aluminium is from the dissolving of anode aluminium sheet in the polymerize aluminum chloride of preparation, cause the production cost of this method higher relatively, can't satisfy the needs of scale operation, and wherein still have 20%～40% aluminium to exist with aluminum ion and aluminium hydroxide form.
5, dimensional stable anode electrolytic process
Teachers such as the Qu Jiuhui of Ecological Envionment Research Centre, Chinese Academy of Sciences go out Al with the dimensional stable anode electrolytic preparation 13Account for the polymerize aluminum chloride of total aluminium more than 60%.But electrolysis time is longer, generally more than 10 hours, and Al 13Easily the deposition cathode surface causes electrode passivation, and electrolytic efficiency is lower, and Al 13Content remains further to be improved.
Summary of the invention
The objective of the invention is higher at existing complex process in the existing preparation polymerize aluminum chloride method, cost, easily cause the weak point of secondary pollution, provide that a kind of what have advantages such as technology is simple, level of residue is few, cost is low, pollution is few is the method that feedstock production contains ferrosilicon polymerization 13 aluminium with the aluminium ash.
The technical scheme that method adopted that the present invention utilizes the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium is finished in the following way: the method for utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium may further comprise the steps:
(1) with aluminium ash and Na 2CO 3Put into the stove calcining behind the mixing and obtain pale powder;
(2) above-mentioned pale powder is put into container after, add hydrochloric acid and carry out acid-leaching reaction;
(3) above-mentioned acidleach product is carried out solid-liquid separation, obtain throw out and contain Fe 3+AlCl 3Solution;
(4) in the above-mentioned throw out that obtains, add alkaline solution and react, obtain throw out and Na through solid-liquid separation 2SiO 3Solution;
(5) at AlCl 3Add Na in the solution 2SiO 3Solution, through mix and the potential of hydrogen of regulator solution after promptly obtain containing ferrosilicon polymerization 13 aluminium.
Utilize the preparation of aluminium lime-ash to contain in the method for ferrosilicon polymerization 13 aluminium aluminium ash and Na above-mentioned 2CO 3The quality proportioning be: aluminium ash 10 parts, Na 2CO 35～8 parts.
Utilize the preparation of aluminium lime-ash to contain in the method for ferrosilicon polymerization 13 aluminium calcining aluminium ash and Na above-mentioned 2CO 3The temperature of mixture is 650 ℃～950 ℃, and calcination time is 0.5～1.5h.
Utilize the preparation of aluminium lime-ash to contain in the method for ferrosilicon polymerization 13 aluminium aluminium ash and Na above-mentioned 2CO 3The hydrochloric acid that is added after the pale powder that calcining obtains is put into container is the hydrochloric acid of massfraction 3%～12%, and the acid-leaching reaction time of being carried out is 2～7h.
Utilize the preparation of aluminium lime-ash to contain in the method for ferrosilicon polymerization 13 aluminium above-mentioned, added alkaline solution is a NaOH solution in step (4), the mass ratio of throw out and NaOH solution is 1: 0.4～1.2, and temperature of reaction is 80 ℃～90 ℃, and the reaction times is 0.5～1.5h.
Utilize aluminium lime-ash preparation to contain in the method for ferrosilicon polymerization 13 aluminium above-mentioned, in step (5) to AlCl 3Add Na in the solution 2SiO 3The mode of solution is for dripping, and the potential of hydrogen of institute's regulator solution is a pH value 3.0～5.5.
Utilize the preparation of aluminium lime-ash to contain in the method for ferrosilicon polymerization 13 aluminium above-mentioned, the partial reaction principle is as follows:,
Calcination reaction: 3Al 2O 32SiO 2(c)+Na 2CO 3(s)=2NaAlSiO 4(c)+2Al 2O 3(s)+CO 2(gas) ↑
Al 2O 3(excessive glass)+Na 2CO 3(s)=2NaAlO 2(s)+CO 2(gas) ↑
Acid-leaching reaction: NaAlSiO 4+ 4H +=Al 3++ Na ++ H 2O+H 2SiO 3↓
NaAlQ 2+4H +＝Al 3++Na ++2H 2O
H 2SiO 3＝(1-n)H 2O+SiO 2.nH 2O
The molten reaction of alkali: SiO 2.nH 2O+2NaOH=Na 2SiO 3+ (n+1) H 2O
The present invention not only makes the Al that exists with crystalline form in the aluminium ash by the molten reaction of high-temperature calcination, acidleach and alkali 2O 3With the maximized stripping of the aluminium that is wrapped up by glass microballon, overcome because of problems such as the low wasting of resources that causes of aluminium ash solubility rate, environmental pollutions; And preparation contain ferrosilicon polymerization 13 aluminium products, performance is superior than traditional flocculant.
The present invention compares with existing preparation polymerize aluminum chloride method, has following characteristics:
1, the solubility rate height of aluminium ash, the starting temperature of reaction is low, has reduced cost.
2, the amount height of the stripping aluminium of aluminium ash has reduced the environmental pollution that discarded aluminium ash is caused thus.
3, owing to contain ferrosilicon impurity, Al in the aluminium ash 13Coupled action easily takes place in the poly-silicic acid interionic of ion and iron, and the polymerization degree that contains ferrosilicon polymerization 13 aluminium of generation is enlarged markedly, and its flocculating effect and stability are all obviously improved, simultaneously, use this product treatment sewage, the aluminium less residue in the water quality, the aluminium residual quantity has only 1.3～2.1 μ g/L.
Embodiment
Below by embodiment the present invention is made further and to specify.
Example 1
A kind of method of utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium, its preparation process is: (1) is with Na 2CO 3Press 1: 1.5 mixing of mass ratio with the aluminium ash; (2) mixture is placed retort furnace, at 650 ℃ of following roast 1h; (3) HCl with product of roasting and massfraction 3% carries out acid-leaching reaction in reactor, and extraction time is 6h; (4) the acidleach product is carried out solid-liquid separation through filter, throw out and NaOH after separating are pressed 1: 0.4 mixing of mass ratio,, carry out solid-liquid separation then, obtain Na at 82 ℃ of following heated and stirred 1.5h 2SiO 3Supernatant liquor is standby; (5) with pickling liquor AlCl 3Be raw material, to wherein dripping alkali immersion liquid Na 2SiO 3, the potential of hydrogen of regulator solution, the pH that makes solution is 3.0, contains ferrosilicon polymerization 13 aluminium product, wherein Al thereby prepare 13The ratio that accounts for total aluminium is 90.3%, and basicity is 80%, the throw out oven dry with alkali after molten, weighs that to calculate the residual residue rate be 9.5%.
Example 2
A kind of method of utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium.Its preparation process is: (1) is with Na 2CO 3Press 1: 1.6 mixing of mass ratio with the aluminium ash; (2) mixture is placed retort furnace, at 750 ℃ of following roast 0.5h; (3) HCl with product of roasting and massfraction 5% carries out acid-leaching reaction in reactor, and extraction time is 4h; (4) the acidleach product is carried out solid-liquid separation through filter, throw out and NaOH after separating are pressed 1: 0.8 mixing of mass ratio,, carry out solid-liquid separation then, obtain Na at 87 ℃ of following heated and stirred 1h 2SiO 3Supernatant liquor is standby; (5) with pickling liquor AlCl 3Be raw material, to wherein dripping alkali immersion liquid Na 2SiO 3, the potential of hydrogen of regulator solution, the pH that makes solution is 4.0, contains ferrosilicon polymerization 13 aluminium product, wherein Al thereby prepare 13The ratio that accounts for total aluminium is 91.6%, and basicity is 82%, the throw out oven dry with alkali after molten, weighs that to calculate the residual residue rate be 8.7%.
Example 3
A kind of method of utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium.Its preparation process is: (1) is with Na 2CO 3Press 1: 1.8 mixing of mass ratio with the aluminium ash; (2) mixture is placed retort furnace, at 850 ℃ of following roast 1.5h; (3) HCl with product of roasting and massfraction 8% carries out acid-leaching reaction in reactor, and extraction time is 7h; (4) the acidleach product is carried out solid-liquid separation through filter, throw out and NaOH after separating are pressed 1: 1.0 mixing of mass ratio,, carry out solid-liquid separation then, obtain Na at 85 ℃ of following heated and stirred 0.5h 2SiO 3Supernatant liquor is standby; (5) with pickling liquor AlCl 3Be raw material, to wherein dripping alkali immersion liquid Na 2SiO 3, the potential of hydrogen of regulator solution, the pH that makes solution is 5.0, contains ferrosilicon polymerization 13 aluminium product, wherein Al thereby prepare 13The ratio that accounts for total aluminium is 92.5%, and basicity is 85%, the throw out oven dry with alkali after molten, weighs that to calculate the residual residue rate be 5.8%.
Example 4
A kind of method of utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium.Its preparation process is: (1) is with Na 2CO 3Press 1: 2.0 mixing of mass ratio with the aluminium ash; (2) mixture is placed retort furnace, at 950 ℃ of following roast 1.0h; (3) HCl with product of roasting and massfraction 12% carries out acid-leaching reaction in reactor, and extraction time is 5h; (4) the acidleach product is carried out solid-liquid separation through filter, throw out and NaOH after separating are pressed 1: 1.2 mixing of mass ratio,, carry out solid-liquid separation then, obtain Na at 80 ℃ of following heated and stirred 1.5h 2SiO 3Supernatant liquor is standby; (5) with pickling liquor AlCl 3Be raw material, to wherein dripping alkali immersion liquid Na 2SiO 3, the potential of hydrogen of regulator solution, the pH that makes solution is 5.5, contains ferrosilicon polymerization 13 aluminium product, wherein Al thereby prepare 13The ratio that accounts for total aluminium is 92.6%, and basicity is 83%, the throw out oven dry with alkali after molten, weighs that to calculate the residual residue rate be 5.0%.
Example 5
A kind of method of utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium.Its preparation process is: (1) is with Na 2CO 3Press 1: 1.7 mixing of mass ratio with the aluminium ash; (2) mixture is placed retort furnace, at 730 ℃ of following roast 1.5h; (3) HCl with product of roasting and massfraction 10% carries out acid-leaching reaction in reactor, and extraction time is 6h; (4) the acidleach product is carried out solid-liquid separation through filter, throw out and NaOH after separating are pressed 1: 0.9 mixing of mass ratio,, carry out solid-liquid separation then, obtain Na at 90 ℃ of following heated and stirred 1.0h 2SiO 3Supernatant liquor is standby; (5) with pickling liquor AlCl 3Be raw material, to wherein dripping alkali immersion liquid Na 2SiO 3, the potential of hydrogen of regulator solution, the pH that makes solution is 5.2, contains ferrosilicon polymerization 13 aluminium product, wherein Al thereby prepare 13The ratio that accounts for total aluminium is 92.8%, and basicity is 85.2%, the throw out oven dry with alkali after molten, weighs that to calculate the residual residue rate be 4.8%.

Claims (6)

1. one kind is utilized the aluminium lime-ash to prepare the method that contains ferrosilicon polymerization 13 aluminium, it is characterized in that the method for utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium may further comprise the steps:
(1) with aluminium ash and Na 2CO 3Put into the stove calcining behind the mixing and obtain pale powder;
(2) above-mentioned pale powder is put into container after, add hydrochloric acid and carry out acid-leaching reaction;
(3) above-mentioned acidleach product is carried out solid-liquid separation, obtain throw out and contain Fe 3+AlCl 3Solution;
(4) in the above-mentioned throw out that obtains, add alkaline solution and react, obtain throw out and Na through solid-liquid separation 2SiO 3Solution;
(5) at AlCl 3Add Na in the solution 2SiO 3Solution, through mix and the potential of hydrogen of regulator solution after promptly obtain containing ferrosilicon polymerization 13 aluminium.
2. the method for utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium according to claim 1 is characterized in that aluminium ash and Na 2CO 3The quality proportioning be: aluminium ash 10 parts, Na 2CO 35～8 parts.
3. the method for utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium according to claim 1 is characterized in that calcining aluminium ash and Na 2CO 3The temperature of mixture is 650 ℃～950 ℃, and calcination time is 0.5～1.5h.
4. the method for utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium according to claim 1 is characterized in that aluminium ash and Na 2CO 3The hydrochloric acid that is added after the pale powder that calcining obtains is put into container is the hydrochloric acid of massfraction 3%～12%, and the acid-leaching reaction time of being carried out is 2～7h.
5. the method for utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium according to claim 1, it is characterized in that added alkaline solution is a NaOH solution in the step (4) in claim 1, the mass ratio of throw out and NaOH solution is 1: 0.4～1.2, temperature of reaction is 80 ℃～90 ℃, and the reaction times is 0.5～1.5h.
6. the method for utilizing the preparation of aluminium lime-ash to contain ferrosilicon polymerization 13 aluminium according to claim 1 is characterized in that in the step (5) in claim 1 to AlCl 3Add Na in the solution 2SiO 3The mode of solution is for dripping, and the potential of hydrogen of institute's regulator solution is a pH value 3.0～5.5.
CN201010161274A 2010-04-30 2010-04-30 Method for preparing silicoferrite-containing Al13 by utilizing aluminum ash slag Pending CN101817580A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114425556A (en) * 2022-02-07 2022-05-03 浙江美臣新材料科技有限公司 Aluminum ash recycling treatment method
CN114735737A (en) * 2022-04-01 2022-07-12 武汉鸿劲金属铝业有限公司 Method for preparing polyaluminum chloride co-production baking-free environment-friendly brick from aluminum ash

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张寿通等: "新型聚硅酸氯化铝铁絮凝剂制备与性能", 《大连交通大学学报》 *
王丽华: "利用高铝粉煤灰制备聚合氯化铝的实验研究", 《中国优秀博硕士学位论文全文数据库（博士） 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114425556A (en) * 2022-02-07 2022-05-03 浙江美臣新材料科技有限公司 Aluminum ash recycling treatment method
CN114735737A (en) * 2022-04-01 2022-07-12 武汉鸿劲金属铝业有限公司 Method for preparing polyaluminum chloride co-production baking-free environment-friendly brick from aluminum ash

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Application publication date: 20100901