CN106277007A - A kind of preparation method of aluminium polychlorid - Google Patents
A kind of preparation method of aluminium polychlorid Download PDFInfo
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- CN106277007A CN106277007A CN201610742808.6A CN201610742808A CN106277007A CN 106277007 A CN106277007 A CN 106277007A CN 201610742808 A CN201610742808 A CN 201610742808A CN 106277007 A CN106277007 A CN 106277007A
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
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Abstract
The invention discloses the preparation method of a kind of aluminium polychlorid.The preparation method of this aluminium polychlorid, comprises the following steps: blast furnace slag is used highly basic to impregnate by (1), obtains soaking slag；(2) described leaching slag use strong acid is carried out molten taking, obtain the mother solution containing aluminum chloride；(3) make the aluminum chloride in described mother solution carry out hydrolysis, obtain the sol solutions containing aluminium polychlorid；(4) make the aluminium polychlorid in described sol solutions occur heavy poly-, obtain aluminium polychlorid.The present invention prepares in the preparation method of aluminium polychlorid, first uses highly basic to impregnate blast furnace slag, then uses the molten acquirement of strong acid to the mother solution containing aluminum chloride dipping gained leaching slag, then hydrolyzes, finally settles, thus prepares preparation method relatively simple.It addition, with blast furnace slag as raw material, can turn waste into wealth, reduce production cost, it also avoid the discarded pollution to environment of blast furnace slag.
Description
Technical field
The present invention relates to the technical field of flocculant, particularly relate to the preparation method of a kind of aluminium polychlorid.
Background technology
Aluminium polychlorid is a kind of water-purifying material, and inorganic polymer coagulant is called again poly-aluminum for short, and english abbreviation is
PAC, the molecular weight produced due to the bridging action of hydroxide ion and the polymerization of multivalent anions is relatively big, electric charge is higher
Inorganic polymer water treatment agent.Solid and liquid two kinds can be divided into the most again.Solid is divided into again by color difference
Sepia, ecru, golden yellow and white, liquid can be rendered as water white transparency, slightly yellow, light yellow to yellowish-brown.Different
The aluminium polychlorid of color also has bigger difference in application and production technology.
In prior art, preparing the main preparation methods of aluminium polychlorid has with aluminum metal as raw material or is former with aluminium salt
Material.Preparation method with aluminum metal as raw material is to take so that the employing containing the raw material of aluminum simple substance is sour or alkali is molten, then hydrolyzes；With aluminium salt to be
The preparation method of raw material specifically, be dissolved in water and hydrolyze by aluminium salt.These preparation methoies are owing to using aluminum or aluminium salt, and it becomes to produce
Relatively costly, and production technology is the most complex.
Summary of the invention
In view of this, the present invention provides the preparation method of a kind of polyaluminium chloride, and this preparation method has higher conversion ratio.
A kind of preparation method preparing aluminium polychlorid, comprises the following steps:
1) use highly basic to impregnate blast furnace slag, obtain soaking slag；
(2) described leaching slag use strong acid is carried out molten taking, obtain the mother solution containing aluminum chloride；
(3) make the aluminum chloride in described mother solution carry out hydrolysis, obtain the sol solutions containing aluminium polychlorid；
(4) make the aluminium polychlorid in described sol solutions occur heavy poly-, obtain aluminium polychlorid.
Above-mentioned blast furnace slag refers to the refuse discharged from blast furnace during manUfaCtUre of pig iron, when furnace temperature reaches 1,400 1600 DEG C
Time, furnace charge melts, the stone-like pulse in Ore, the ash in coke and cosolvent and other can not enter impurity in the pig iron formed with
Silicate and aluminate are that master floats over the slag above molten iron.Blast furnace slag major oxide constituents is SiO2、Al2O3, CaO etc..
In step (1), the reaction equation of dipping is SiO2+2OH- =SiO3 2-+H2O.May be appreciated but, blast furnace slag
Middle SiO2Composition forms soluble silicate after being through impregnation with, and the residue after blast furnace slag is through impregnation with mainly contains Al2O3, the leaching of CaO
Slag.
Term " highly basic " refers to the alkali that can all ionize.Highly basic can use highly basic well known in the art, both can be nothing
Machine highly basic, such as Strong oxdiative sodium, Strong oxdiative potassium, it is also possible to for organic alkali, such as Sodium ethylate, potassium ethoxide etc..Preferably divide for quality
Number be 20～40wt% sodium hydroxide or potassium hydroxide, such as its mass fraction can be 20wt%, 22wt%, 25wt%, 30wt%,
35wt%, 38wt% or 40wt% etc..
In order to obtain higher by and the leaching rate of silicon dioxide (leaching rate is for leaching aluminium composition and theoretical aluminum content
Ratio), the consumption of highly basic is advisable with 4～6, is in terms of 1 by the quality of blast furnace slag, such as its consumption can be 4,4.2,4.5,5,
5.5,5.8,6 etc..
The temperature of dipping is preferably 30～50 DEG C, such as 30 DEG C, 32 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 48 DEG C, 49 or 50 DEG C
Deng.
In step (2), the molten reaction equation that takes of strong acid is used to be:；
。
Above-mentioned strong acid can be both mineral acid, such as dilute hydrochloric acid, dilute sulfuric acid, dust technology；Can also be organic acid, such as benzene sulphur
Acid, trifluoroacetic acid etc..In order to avoid introducing the removal trouble that new impurity is brought, strong acid can use hydrochloric acid.Herein, hydrochloric acid
Concentration can be with 15～25wt%(mass fractions) be advisable, such as 15wt%, 16wt%, 18wt%, 20wt%, 21wt%, 22wt%,
23wt%, 24wt%, 24.5wt% or 25wt% etc..
The consumption of strong acid, it is preferred that can be 20～40ml, counts with the quality of blast furnace slag for 1g.The consumption of such as strong acid
Can be 20ml, 21ml, 22ml, 23ml, 25ml, 30ml, 35ml, 37ml, 38ml, 39ml or 40ml etc..
In order to obtain the preferable aluminum ions molten rate that takes, the molten temperature taken of strong acid is preferably 90～100 DEG C, such as 90 DEG C,
91 DEG C, 93 DEG C, 95 DEG C, 97 DEG C, 98 DEG C, 99 DEG C or 100 DEG C etc..
On the basis of this molten temperature taken, the molten time taken is advisable with 1～2h, such as 1h, 1h 20min, 1.5h,
1.75,2h etc..If the time exceedes this scope, the raising of leaching rate can not be brought significantly.
Dipping can be carried out under an increased pressure, pressure can be 0.1～0.2MPa, such as 0.1 MPa, 0.12MPa,
0.15MPa, 0.18MPa, 0.19MPa or 0.20MPa etc..
Can carry out under conditions of stirring it should be noted that above-mentioned highly basic dipping is molten with acid, the rotating speed of stirring is to this
Bright effect does not results in impact.Its rotating speed can adjust according to actual needs.
In above-mentioned steps (3), hydrolysis generates the process of aluminium polychlorid is that aluminum particulate hydrolysis generates Liu's hydrated aluminum and joins
Position ion, i.e..When pH value in solution raises, join in complex ion
Position water hydrolyzes, thus causes proton migration process, two OH mono-between monomer produce bridge formations and Step Condensation be dimer,
Trimer, therefore, the amount adding alkali increases, and aggregate rate can be made to increase.But when being aggregated to a certain degree, because of aluminium ion increasingly
Few, polymerization machine can reduce.
Said hydrolyzed reaction temperature be preferred with 20～40 DEG C, such as 20 DEG C, 21 DEG C, 22 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 38
DEG C, 39 DEG C or 40 DEG C etc..At a temperature of this hydrolysis, the time of hydrolysis preferably 2～4h, as 2h, 2.25h,
2.5h, 3h, 3.5h, 3.75h or 4h etc..
The pH of hydrolysis is advisable with 6.8～7.5, and such as 6.8,6.9,7,7.2,7.5 etc., preferably 7.2 etc..
In above-mentioned steps (4), owing to the aluminium polychlorid in sol solutions is dispersed in water with the form of colloidal sol.So can adopt
The mode settled with colloid well-known to those skilled in the art implements the present invention.Such as can add a small amount of electrolyte (such as salt
Acid), then stand, lower floor's solid phase is aluminium polychlorid.Then the supernatant (can siphonage) on upper strata is being removed.Or ground, for
Obtain effect of settling faster, centrifugation can be used, first centrifugal the most solid to separate out with 3000～5000rpm rotating speeds
Phase, is removing supernatant.
After step (4), also the aluminium polychlorid that sedimentation obtains can be dried, such as vacuum lyophilization.
Term " vacuum lyophilization " is called for short lyophilizing, is in relatively low temperature (-10 DEG C～-50 by wet stock or solution
DEG C) under be frozen into solid-state, then make moisture therein be directly sublimed into gaseous state without liquid under vacuum (1.3～13 handkerchief),
Make the dry technology of material dewatering eventually.
Roasting can also be included before the step (1), be the referring to property of temperature of roasting 600～800 DEG C, as 600 DEG C,
620 DEG C, 650 DEG C, 700 DEG C, 750 DEG C, 780 DEG C or 800 DEG C etc..The purpose of roasting is so that blast furnace slag activates, it is simple to follow-up
Impregnating.
Above-mentioned do not address part, it is adaptable to prior art.
As used herein, above-mentioned term:
" mass parts " refers to represent the basic measurement unit of the mass ratio relation of multiple component, and 1 part can represent arbitrary unit matter
Amount, as being expressed as 1g, it is possible to represents 2.689g etc..If we say that the mass parts of component A is a part, the mass parts of B component
For b part, then it represents that the quality of component A and mass ratio a:b of B component.Or ground, represents that the quality of component A is aK, B component
Quality be bK(K be Arbitrary Digit, represent multiplying factor).Can not misread, unlike mass fraction, all components
Mass parts sum is not limited to the restriction of 100 parts.
" one ", " a kind of " and " described " are used interchangeably and refer to one or more.
"and/or" for represent the one or both of illustrated situation all it may happen that, such as, A and/or B includes (A
And B) and (A or B).
It addition, all numerical value that the scope stated by end points herein is comprised in the range of including this (such as, 1 to 10 bag
Include 1.4,1.9,2.33,5.75,9.98 etc.).
It addition, the statement of " at least one " herein include one and above all numbers (such as, at least 2, at least
4, at least 6, at least 8, at least 10, at least 25, at least 50, at least 100 etc.).
The present invention prepares in the preparation method of aluminium polychlorid, first uses highly basic to impregnate blast furnace slag, then will leaching
Stain gained leaching slag uses the molten acquirement of strong acid to the mother solution containing aluminum chloride, then hydrolyzes, finally settles, thus prepares preparation side
Method is relatively simple.It addition, with blast furnace slag as raw material, can turn waste into wealth, reduce production cost, it also avoid the discarded of blast furnace slag
Pollution to environment.
Detailed description of the invention
Technical scheme is further illustrated below in conjunction with embodiment.
Embodiment 1
Step one, blast furnace slag is crushed to below 80 mesh.
Step 2, the blast furnace slag through step one is inserted chamber type electric resistance furnace roasting 10h at 600 DEG C.
Step 3, it is 20wt% sodium hydroxide to be inserted 78-1 type magnetic force stir by blast furnace slag and the mass fraction through step 2
Mixing in device, wherein the consumption of sodium hydroxide is 4, is in terms of 1 by the quality of blast furnace slag, impregnates 5h, filters, retain leaching at 30 DEG C
Slag.
Step 4, it is 15wt% hydrochloric acid to be inserted in above-mentioned magnetic stirring apparatus by above-mentioned leaching slag and mass fraction, wherein hydrochloric acid
Consumption be 50ml, count with the quality of blast furnace slag for 1g, at 90 DEG C impregnate 2h, obtain the mother solution containing aluminum chloride.
Step 5, by above-mentioned mother solution add sodium hydroxide to regulate pH to 6.8, at 40 DEG C, the time of described hydrolysis
For 2h, obtain the sol solutions containing aluminium polychlorid.
Step 6, above-mentioned sol solutions is centrifugal so that its layering at 3000～5000rpm rotating speeds, suck supernatant with siphon
Liquid, collects the gel of aluminium polychlorid.
Step 7, the gel of above-mentioned aluminium polychlorid is used vacuum freeze-drying, obtain polyaluminium aluminium powder.
Embodiment 2
Step one, blast furnace slag is crushed to below 80 mesh.
Step 2, the blast furnace slag through step one is inserted chamber type electric resistance furnace roasting 6h at 800 DEG C.
Step 3, it is 40wt% sodium hydroxide to be inserted 78-1 type magnetic force stir by blast furnace slag and the mass fraction through step 2
Mixing in device, wherein the consumption of sodium hydroxide is 4, is in terms of 1 by the quality of blast furnace slag, impregnates 3h, filters, retain leaching at 50 DEG C
Slag.
Step 4, it is 25wt% hydrochloric acid to be inserted in 78-1 type magnetic stirring apparatus by above-mentioned leaching slag and mass fraction, wherein salt
The consumption of acid is 30ml, counts with the quality of blast furnace slag for 1g, impregnates 1h, obtain the mother solution containing aluminum chloride at 100 DEG C.
Step 5, by above-mentioned mother solution add sodium hydroxide to regulate pH to 6.8, at 20 DEG C, the time of described hydrolysis
For 4h, obtain the sol solutions containing aluminium polychlorid.
Step 6, above-mentioned sol solutions is centrifugal so that its layering at 3000～5000rpm rotating speeds, suck supernatant with siphon
Liquid, collects the gel of aluminium polychlorid.
Step 7, the gel of above-mentioned aluminium polychlorid is used vacuum freeze-drying, obtain polyaluminium aluminium powder.
Embodiment 3
Step one, blast furnace slag is crushed to below 80 mesh.
Step 2, the blast furnace slag through step one is inserted chamber type electric resistance furnace roasting 10h at 600 DEG C.
Step 3, it is 40wt% sodium hydroxide to be inserted 78-1 type magnetic force stir by blast furnace slag and the mass fraction through step 2
Mixing in device, wherein the consumption of sodium hydroxide is 6, is in terms of 1 by the quality of blast furnace slag, impregnates 5h, filters, retain leaching at 30 DEG C
Slag.
Step 4, it is 25wt% hydrochloric acid to be inserted in 78-1 type magnetic stirring apparatus by above-mentioned leaching slag and mass fraction, wherein salt
The consumption of acid is 50ml, counts with the quality of blast furnace slag for 1g, impregnates 1h, obtain the mother solution containing aluminum chloride at 100 DEG C.
Step 5, by above-mentioned mother solution add sodium hydroxide to regulate pH to 7.5, at 20 DEG C, the time of described hydrolysis
For 4h, obtain the sol solutions containing aluminium polychlorid.
Step 6, above-mentioned sol solutions is centrifugal so that its layering at 3000～5000rpm rotating speeds, suck supernatant with siphon
Liquid, collects the gel of aluminium polychlorid.
Step 7, the gel of above-mentioned aluminium polychlorid is used vacuum freeze-drying, obtain polyaluminium aluminium powder.
Embodiment 4
Step one, blast furnace slag is crushed to below 80 mesh.
Step 2, the blast furnace slag through step one is inserted chamber type electric resistance furnace roasting 8h at 700 DEG C.
Step 3, it is 30wt% sodium hydroxide to be inserted 78-1 type magnetic force stir by blast furnace slag and the mass fraction through step 2
Mixing in device, wherein the consumption of sodium hydroxide is 4, is in terms of 1 by the quality of blast furnace slag, impregnates 5h, filters, retain leaching at 50 DEG C
Slag.
Step 4, it is 20wt% hydrochloric acid to be inserted in 78-1 type magnetic stirring apparatus by above-mentioned leaching slag and mass fraction, wherein salt
The consumption of acid is 30ml, counts with the quality of blast furnace slag for 1g, impregnates 2h, obtain the mother solution containing aluminum chloride at 95 DEG C.
Step 5, by above-mentioned mother solution add sodium hydroxide to regulate pH to 7.5, at 30 DEG C, the time of described hydrolysis
For 3h, obtain the sol solutions containing aluminium polychlorid.
Step 6, above-mentioned sol solutions is centrifugal so that its layering at 3000～5000rpm rotating speeds, suck supernatant with siphon
Liquid, collects the gel of aluminium polychlorid.
Step 7, the gel of above-mentioned aluminium polychlorid is used vacuum freeze-drying, obtain polyaluminium aluminium powder.
Embodiment 5
Step one, blast furnace slag is crushed to below 80 mesh.
Step 2, the blast furnace slag through step one is inserted chamber type electric resistance furnace roasting 8h at 700 DEG C.
Step 3, it is 30wt% sodium hydroxide to be inserted 78-1 type magnetic force stir by blast furnace slag and the mass fraction through step 2
Mixing in device, wherein the consumption of sodium hydroxide is 5, is in terms of 1 by the quality of blast furnace slag, impregnates 4h, filters, retain leaching at 40 DEG C
Slag.
Step 4, it is 20wt% hydrochloric acid to be inserted in 78-1 type magnetic stirring apparatus by above-mentioned leaching slag and mass fraction, wherein salt
The consumption of acid is 40ml, counts with the quality of blast furnace slag for 1g, impregnates 1.5h, obtain the mother solution containing aluminum chloride at 95 DEG C.
Step 5, by above-mentioned mother solution add sodium hydroxide to regulate pH to 7, at 30 DEG C, the time of described hydrolysis is
3h, obtains the sol solutions containing aluminium polychlorid.
Step 6, above-mentioned sol solutions is centrifugal so that its layering at 3000～5000rpm rotating speeds, suck supernatant with siphon
Liquid, collects the gel of aluminium polychlorid.
Step 7, the gel of above-mentioned aluminium polychlorid is used vacuum freeze-drying, obtain polyaluminium aluminium powder.
Use the turbidity removal rate of known colorimetric method for determining embodiment 1 to embodiment 5, result such as following table:
Owing to the numerical range of each technological parameter involved in the present invention can not all embody in the above-described embodiments, but this
As long as the most envisioned any numerical value fallen in this numerical range above-mentioned of the technical staff in field all can implement the present invention,
Certainly the combination in any of occurrence in the range of some numerical value is also included.Herein, for the consideration of length, eliminate be given a certain
The embodiment of occurrence in item or multinomial numerical range, this is not to be construed as the insufficient disclosure of technical scheme.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, i.e. do not mean that the present invention have to rely on above-mentioned in detail
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The equivalence of raw material each to product of the present invention is replaced and the interpolation of auxiliary element, concrete way choice etc., all falls within the present invention's
Within the scope of protection domain and disclosure.
Claims (9)
1. the preparation method of an aluminium polychlorid, it is characterised in that comprise the following steps:
(1) use highly basic to impregnate blast furnace slag, obtain soaking slag；
(2) described leaching slag use strong acid is carried out molten taking, obtain the mother solution containing aluminum chloride；
(3) make the aluminum chloride in described mother solution carry out hydrolysis, obtain the sol solutions containing aluminium polychlorid；
(4) make the aluminium polychlorid in described sol solutions occur heavy poly-, obtain aluminium polychlorid.
Preparation method the most according to claim 1, it is characterised in that highly basic described in step (1) be mass fraction be 20
～40wt% sodium hydroxide or potassium hydroxide；The consumption of described highly basic is 4～6, is in terms of 1 by the quality of blast furnace slag.
Preparation method the most according to claim 1, it is characterised in that described in step (1), the temperature of dipping is 30～50
℃。
Preparation method the most according to claim 1, it is characterised in that strong acid described in step (2) be mass fraction be 15
～25wt% hydrochloric acid.
Preparation method the most according to claim 1, it is characterised in that the consumption of described strong acid is 20～40ml, with blast furnace
The quality of slag is 1g meter.
Preparation method the most according to claim 1, it is characterised in that described in step (2), the molten temperature taken is 90～100
DEG C, the time of described dipping is 1～2h.
Preparation method the most according to claim 1, it is characterised in that described in step (3), the temperature of hydrolysis is 20
～40 DEG C, the time of described hydrolysis is 2～4h.
Preparation method the most according to claim 1, it is characterised in that the pH of hydrolysis described in step (3) be 6.8～
7.5。
Preparation method the most according to claim 1, it is characterised in that also include roasting before step (1), described roasting
Temperature is 600～800 DEG C.
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Cited By (1)
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| CN115974119A (en) * | 2022-12-01 | 2023-04-18 | 百色实华环保科技有限公司 | Method for preparing polyaluminum chloride from medium-high aluminum slag in electrolytic aluminum overhaul slag |
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Application publication date: 20170104 |