CN106186019B - A kind of preparation method of the aluminium polychloride of low-residue aluminum - Google Patents
A kind of preparation method of the aluminium polychloride of low-residue aluminum Download PDFInfo
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- CN106186019B CN106186019B CN201610530149.XA CN201610530149A CN106186019B CN 106186019 B CN106186019 B CN 106186019B CN 201610530149 A CN201610530149 A CN 201610530149A CN 106186019 B CN106186019 B CN 106186019B
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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
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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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- Environmental & Geological Engineering (AREA)
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Abstract
The present invention relates to a kind of preparation methods of aluminium polychloride, more particularly, to a kind of preparation method of the aluminium polychloride of low-residue aluminum.Its residual Al for mainly solving that aluminium polychloride in the water body of high pH or high alkalinity, is used to cause as flocculant in water present in the prior art is more than drinking water national standard, that is, is greater than the technical problem of 0.2mg/Kg etc..The method comprise the steps that a. is in closed reactor, it puts into hydrochloric acid and the stirring of raw material containing aluminium is abundant, water is added to above-mentioned aluminium polychloride liquid in closed reactor, aluminic acid acid calcium powder or sodium aluminate, fully reacting is discharged to stirred tank after filters pressing, the mixed aqueous solution 50-150Kg per ton that sodium dihydrogen phosphate and disodium hydrogen phosphate is added in stirred tank, in the mixed aqueous solution of sodium dihydrogen phosphate and disodium hydrogen phosphate, the mass fraction of sodium dihydrogen phosphate is 20-30%, the mass fraction of disodium hydrogen phosphate is 5-15%, remaining is water, go out finished product aluminium polychloride after stirring.
Description
Technical field
The present invention relates to a kind of preparation methods of aluminium polychloride, more particularly, to a kind of aluminium polychloride of low-residue aluminum
Preparation method.
Background technique
Aluminium polychloride has been most popular inorganic flocculating agent in the flocculating setting processing of Water purification.High ph-values
With the water body of high alkalinity, the most commonly reservoir water in autumn, the PH of water body is caused due to breeding and decomposition of algae etc.
It increases and such case, such as some giving using Huanghe water as raw water also often occurs in the increase of basicity, also some other water system
There is also these problems in water process.The preparation method that Chinese patent discloses a kind of aluminium polychloride of high aluminium content is (open
Number: CN1718543), raw material is aluminium hydroxide and hydrochloric acid, is first added hydrochloric acid solution in a kettle, under stirring condition, is added
The molar ratio of the crystalline aluminium hydroxide of industrial goods, aluminium hydroxide and hydrochloric acid is 0.4-1: 2, and has catalyst A participation to react
The molar ratio of journey, aluminium hydroxide and A are 2-50, are 1-8Kgf/cm in steam pressure2Under conditions of, reaction temperature 90-180
DEG C, the reaction time 2 hours or more, after reaction, the polymeric aluminium reaction object of generation was put into precipitation tank, was aged 2 hours
More than, the stillness of night is aluminium polychloride finished product above after ageing, and whether there is or not setting features for the polyaluminium constructed of aluminium；Catalyst A is
Inorganic phosphorus compound.But in the water body of high pH or high alkalinity, aluminium polychloride is used to cause in water as flocculant
Residual Al be more than drinking water national standard, that is, be greater than 0.2mg/Kg.
Summary of the invention
The present invention is to provide a kind of preparation method of the aluminium polychloride of low-residue aluminum, mainly solves prior art institute
It is existing in the water body of high pH or high alkalinity, using aluminium polychloride to cause residual Al in water as flocculant is more than drink
With water national standard, that is, it is greater than the technical problem of 0.2mg/Kg etc..
Above-mentioned technical problem of the invention is mainly to be addressed by following technical proposals:
The preparation method of the aluminium polychloride of a kind of low-residue aluminum of the invention, it is characterised in that the method includes:
A. in closed reactor, hydrochloric acid and the stirring of raw material containing aluminium are put into sufficiently, and be warmed to 120-1400C, in kettle
Pressure obtains the aluminium polychloride liquid that basicity is 0-30% and alchlor content is 5-15% in 0.15-0.3Mpa；
B. water, aluminic acid acid calcium powder or sodium aluminate is added to above-mentioned aluminium polychloride liquid in closed reactor, wherein three
Alumina content 7-9.5%, basicity are controlled in 80-90%；
C fully reacting is discharged to stirred tank after filters pressing, addition sodium dihydrogen phosphate and phosphoric acid hydrogen per ton in stirred tank
In the mixed aqueous solution of the mixed aqueous solution 50-150Kg of disodium, sodium dihydrogen phosphate and disodium hydrogen phosphate, the matter of sodium dihydrogen phosphate
Amount score is 20-30%, and the mass fraction of disodium hydrogen phosphate is 5-15%, remaining is water, and finished product aluminium polychloride is gone out after stirring.
First is that when adjusting basicity, the control of feed liquid alchlor content exists key of the invention in 7-9.5%, basicity control
80-90%, second is that using sodium dihydrogen phosphate and phosphorus when the product after filters pressing adds the degree of polymerization of other anion to increase product
The mixture of sour disodium hydrogen.
When adjusting product basicity, if the content of the aluminum oxide of aluminium polychloride feed liquid is greater than 10%, even if product
Basicity be adjusted to 90%, for this kind of product when handling the raw water of high pH value high alkalinity, the residual Al of water is also relatively high after sinking,
But flocculating effect is relatively good；As aluminium polychloride feed liquid aluminum oxide content less than 7%, this kind of product is handling high pH
When being worth the raw water of high alkalinity, the available control of residual Al of water after sinking, but flocculating effect is relatively poor.Be added phosphate radical from
Son is come during increasing the degree of polymerization of product to improve flocculating effect, if only using sodium dihydrogen phosphate as adding
Agent causes product to increase in the residual Al of use process after addition, this is because sodium dihydrogen phosphate is in acidity, in addition
Process will lead to the change of aluminum species；If only using disodium hydrogen phosphate as additive, since disodium hydrogen phosphate is in
Alkalinity, occurs gel aluminum hydroxide in the product after addition, and the flocculating effect of product is almost without being obviously improved.
The present invention is the aluminium polychloride that first production basicity is 10-30%；Aluminium is added in above-mentioned aluminium polychloride again
Sour calcium powder or sodium aluminate, the alchlor content of aluminium polychloride are strict controlled in 7-9.5%, basicity control in 80-90%,
While the residual Al in water body after reaching flocculating setting is not exceeded, improve the flocculating effect of product；Fully reacting and filters pressing
Afterwards, the mixed aqueous solution of sodium dihydrogen phosphate and disodium hydrogen phosphate is added, is not improving the residual Al in the water body after flocculating setting
Content simultaneously, enhance the elimination of colloid stability ability and hydrogen bond bridge formation ability of product, greatly improve the flocculating setting effect of product.
Preferably, the raw material containing aluminium are aluminium hydroxide, bauxite, calcium aluminate powder.
Preferably, the concentration of hydrochloric acid in the step a is 10-31%.
Preferably, reaction temperature when adding calcium aluminate powder or sodium aluminate in the step b is 900C or more, reaction
Time is 1-2 hours.
Preferably, adding the reaction temperature of the mixed aqueous solution of sodium dihydrogen phosphate and disodium hydrogen phosphate in the step C
Degree is maintained at 500C or more, reaction time are 30-60 minutes.
Preferably, the heating in the step a includes: first slowly to be warming up to 70-800C, then rapid cooling is to 20-
300C simultaneously keeps the temperature 5-10 minutes；It is slowly warming up to 90-100 for the second time0C, then rapid cooling is to 40-500C simultaneously keeps the temperature 5-10 minutes；
Third time is slowly warming up to 120-1400C is simultaneously kept the temperature；The rate slowly to heat up is 1-50C/min, the rate of rapid cooling
For 20-300C/min.Aluminium raw material can will be contained by, which slowly rising three times, sufficiently decomposes, and then reacts with hydrochloric acid generation.Pass through three
Reaction can be interrupted rapidly, to carry out next secondary response, be reacted repeatedly for three times in this way by secondary rapid cooling, can be made anti-
It should more completely, so that the purity of aluminium polychloride is higher.
Preferably, the inner wall of the stirred tank in the step c is equipped with several fins, the outer surface of fin, which is equipped with, is in
The stirring rod of sector distribution.The each component in stirred tank can be sufficiently stirred by stirring rod, since stirring rod is in fan
Shape distribution, the area stirred in this way are larger.
Preferably, the bottom of the stirred tank in the step c is provided with several punching grooves, the width inside punching groove is small
In the width of its opening.When can make stirring by punching groove, liquid is able to enter in punching groove, due in punching groove
The width in portion is less than the width of its opening, hydraulic larger inside such punching groove, so that mixing is more complete.
Therefore, for aluminium polychloride of the invention when handling the raw water of high PH high alkalinity, the heavy rear water after flocculating setting is residual
Remaining aluminium significantly reduces, and can guarantee excellent flocculating effect.
Detailed description of the invention
Attached drawing 1 is a kind of structural schematic diagram of the inner wall of stirred tank of the present invention；
Attached drawing 2 is a kind of structural schematic diagram of the bottom of stirred tank of the present invention.
Components, position and number in figure: stirred tank 1, fin 2, stirring rod 3, punching groove 4.
Specific embodiment
Below with reference to the embodiments and with reference to the accompanying drawing the technical solutions of the present invention will be further described.
Embodiment 1: a kind of preparation method of the aluminium polychloride of low-residue aluminum of this example the steps include:
The hydrochloric acid of 5 tons of concentration 15%, the aluminium hydroxide of 570Kg are added into 10000L reaction kettle, which contains
Al2O3% is 64%(m/m), moisture content 5.5% is first slowly warming up to 75 in closed reactor0C, then rapid cooling is to 250C is simultaneously
Heat preservation 8 minutes；It is slowly warming up to 95 for the second time0C, then rapid cooling is to 450C simultaneously keeps the temperature 8 minutes；Third time is slowly warming up to
1300C is simultaneously kept the temperature；The rate slowly to heat up is 30C/min, the rate of rapid cooling are 300C/min.It is stirred to react 3 hours, obtains
To containing Al2O3For 6.1%(m/m), the aluminium chloride liquid that basicity is 2% adds calcium aluminate powder in above-mentioned aluminium polychloride liquid
1.1 tons, the Al of the calcium powder2O3% is 50%(m/m), total calcium is 32%(m/m), 2.76 tons of water, it is maintained at 900C or more, confined reaction
It reacts 1 hour, is obtained containing Al in kettle2O3For 8.9%(m/ m)；Basicity is 88%；The polyaluminium of 1.20 grams per milliliter of density
Aluminium；Filters pressing immediately after fully reacting, cleaner liquid are put into intermediate agitation slot, and feed liquid temperature is 65 at this time0Phosphoric acid is added in C or so
The mixed aqueous solution 800Kg of disodium hydrogen and sodium dihydrogen phosphate, the composition of the mixed aqueous solution are as follows: the mass fraction of sodium dihydrogen phosphate
It is 20%, the mass fraction of disodium hydrogen phosphate is 10%, stirs 30 minutes to get to containing Al2O3For 8.4%(m/ m)；Basicity is
91%；Phosphate content is 1.8%；The aluminium polychloride of 1.20 grams per milliliter of density.
Chemical equation are as follows:
1、HCl+Al(OH)3→Al(OH)0.06Cl2.94+H2O；
2、Al(OH)0.06Cl2.94+ Al2O3.CaO+H2O→Al(OH)2.64Cl0.36+CaCl2。
Wherein such as Fig. 1, for the inner wall of stirred tank 1 equipped with several fins 2, the outer surface of fin is equipped with stirring for fan-shaped distribution
Mix stick 3.
Such as Fig. 2, the bottom of stirred tank 1 is provided with several punching grooves 4, and the width inside punching groove is less than the width of its opening
Degree.
Embodiment 2: a kind of preparation method of the aluminium polychloride of low-residue aluminum of this example the steps include:
The hydrochloric acid for claiming 100 grams of concentration 31%, is added 26 grams of aluminium hydroxides, which contains Al2O3% is 64%(m/m), contain
Water rate is 4%(m/m), is first slowly warming up to 75 in closed container in closed reactor0C, then rapid cooling is to 250C simultaneously keeps the temperature 8 points
Clock；It is slowly warming up to 95 for the second time0C, then rapid cooling is to 450C simultaneously keeps the temperature 8 minutes；Third time is slowly warming up to 1300C is simultaneously protected
Temperature；The rate slowly to heat up is 30C/min, the rate of rapid cooling are 300C/min is stirred to react 2.5 hours, is contained
Al2O3For 12.6%(m/m), the aluminium chloride liquid that basicity is 10% adds calcium aluminate powder 42g in above-mentioned aluminium polychloride liquid,
The Al of the calcium powder2O3% is 50%(m/m), total calcium is 32%(m/m), water 180g is maintained at 900C or more reacts in closed reactor
It 90 minutes, obtains containing Al2O3For 9.9%(m/ m)；Basicity is 85%；The aluminium polychloride of 1.23 grams per milliliter of density；It has reacted
It is filtered immediately after complete, cleaner liquid is put into intermediate agitation slot, and the mixed aqueous solution of disodium hydrogen phosphate and sodium dihydrogen phosphate is added
38g, the composition of the mixed aqueous solution are as follows: the mass fraction of sodium dihydrogen phosphate is 20%, and the mass fraction of disodium hydrogen phosphate is 15%,
Heating keeps temperature 55-600C stirs 45 minutes to get to containing Al2O3For 8.9%(m/ m)；Basicity is 88%；Phosphate content
It is 2.5%；The aluminium polychloride of 1.21 grams per milliliter of density.
Chemical equation are as follows:
1、HCl+Al(OH)3→Al(OH)1.2Cl1.8+3H2O；
2、Al(OH)1.2Cl1.8+ NaAlO2+H2O→Al(OH)2.4Cl0.6+NaCl。
Wherein such as Fig. 1, for the inner wall of stirred tank 1 equipped with several fins 2, the outer surface of fin is equipped with stirring for fan-shaped distribution
Mix stick 3.
Such as Fig. 2, the bottom of stirred tank 1 is provided with several punching grooves 4, and the width inside punching groove is less than the width of its opening
Degree.
Use residual Al after typical polymerization aluminium chloride exceeded at present with Mr. Yu above embodiments 1, embodiment 2, product
Raw water coagulation stirring test, while being compared with currently used aluminium polychloride.Processing result see the table below:
| Raw water water temperature: 20.30C | Raw water turbidity: 4.2NTU | Raw water aluminium ion concentration: 0.05 mg/Kg |
From result above as it can be seen that the aluminium polychloride ensure that just when processing is also easy to produce the exceeded raw water of residual Al
On the basis of normal flocculating effect, residual Al reduces by 50% or so.
Above is only a specific embodiment of the present invention, but structure feature of the invention is not limited thereto, Ren Heben
Within the field of the present invention, made changes or modifications all cover within the scope of the patent of the present invention the technical staff in field.
Claims (5)
1. a kind of preparation method of the aluminium polychloride of low-residue aluminum, it is characterised in that the method includes:
A. in closed reactor, hydrochloric acid and the stirring of raw material containing aluminium is put into sufficiently, is first slowly warming up to 70-80 DEG C, then rapidly
It cools to 20-30 DEG C and keeps the temperature 5-10 minutes；Slowly it is warming up to 90-100 DEG C for the second time, then rapid cooling is to 40-500C is simultaneously
Heat preservation 5-10 minutes；Third time is slowly warming up to 120-140 DEG C and keeps the temperature；The rate slowly to heat up be 1-5 DEG C/
Min, the rate of rapid cooling are 20-30 DEG C/min；Pressure is in 0.15-0.3MPa in kettle, obtain basicity be 0-30% and
Alchlor content is the aluminium polychloride liquid of 5-15%；
B. water and calcium aluminate powder or water and sodium aluminate is added to above-mentioned aluminium polychloride liquid in closed reactor, wherein three
Alumina content 7-9.5%, basicity are controlled in 80-90%；
C. fully reacting is discharged to stirred tank after filters pressing, and the inner wall of stirred tank (1) is equipped with several fins (2), outside fin
Surface is equipped with the stirring rod (3) of fan-shaped distribution, and the bottom of stirred tank (1) is provided with several punching grooves (4), the width inside punching groove
Degree is less than the width of its opening, the mixed aqueous solution 50- per ton that sodium dihydrogen phosphate and disodium hydrogen phosphate is added in stirred tank
In the mixed aqueous solution of 150Kg, sodium dihydrogen phosphate and disodium hydrogen phosphate, the mass fraction of sodium dihydrogen phosphate is 20-30%, phosphoric acid
The mass fraction of disodium hydrogen is 5-15%, remaining is water, and finished product aluminium polychloride is gone out after stirring.
2. a kind of preparation method of the aluminium polychloride of low-residue aluminum according to claim 1, it is characterised in that described
Raw material containing aluminium are aluminium hydroxide, bauxite, calcium aluminate powder.
3. a kind of preparation method of the aluminium polychloride of low-residue aluminum according to claim 1, it is characterised in that described
Concentration of hydrochloric acid in step a is 10-31%.
4. a kind of preparation method of the aluminium polychloride of low-residue aluminum according to claim 1, it is characterised in that described
Reaction temperature when adding calcium aluminate powder or sodium aluminate in step b is 90 DEG C or more, and the reaction time is 1-2 hours.
5. a kind of preparation method of the aluminium polychloride of low-residue aluminum according to claim 1, it is characterised in that described
The reaction temperature that the mixed aqueous solution of sodium dihydrogen phosphate and disodium hydrogen phosphate is added in step C is maintained at 50 DEG C or more, when reaction
Between be 30-60 minutes.
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| CN110255595A (en) * | 2019-06-27 | 2019-09-20 | 嘉施利（宜城）化肥有限公司 | The preparation method of aluminium polychloride |
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| CN114832756A (en) * | 2022-04-13 | 2022-08-02 | 安徽仕佰化工有限公司 | Method and equipment for preparing polyaluminium chloride |
| CN115838177A (en) * | 2022-07-27 | 2023-03-24 | 杭州萧山三江净水剂有限公司 | Preparation method of high-basicity polymerized aluminum silicon chloride and treatment method of papermaking wastewater containing low-concentration organic halide |
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