CN106186019A - A kind of preparation method of the aluminium polychlorid of low-residue aluminum - Google Patents
A kind of preparation method of the aluminium polychlorid of low-residue aluminum Download PDFInfo
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- CN106186019A CN106186019A CN201610530149.XA CN201610530149A CN106186019A CN 106186019 A CN106186019 A CN 106186019A CN 201610530149 A CN201610530149 A CN 201610530149A CN 106186019 A CN106186019 A CN 106186019A
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- aluminium polychlorid
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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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- Separation Of Suspended Particles By Flocculating Agents (AREA)
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Abstract
The present invention relates to the preparation method of a kind of aluminium polychlorid, especially relate to the preparation method of the aluminium polychlorid of a kind of low-residue aluminum.Its mainly solve existing for prior art in the water body of high pH or high alkalinity, use aluminium polychlorid to exceed drinking water national standard, the i.e. technical problem more than 0.2mg/Kg etc. as the residual Al that flocculant causes in water.The method comprise the steps that a. is in closed reactor, put into hydrochloric acid and the stirring containing aluminum raw material is abundant, water is added to above-mentioned aluminium polychlorid liquid in closed reactor, aluminic acid acid calcium powder or sodium aluminate, reaction is discharged to agitator tank completely after filter pressing, mixed aqueous solution 50 150Kg of addition sodium dihydrogen phosphate per ton and disodium hydrogen phosphate in agitator 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, finished product aluminium polychlorid is i.e. gone out after stirring.
Description
Technical field
The present invention relates to the preparation method of a kind of aluminium polychlorid, especially relate to the aluminium polychlorid of a kind of low-residue aluminum
Preparation method.
Background technology
In the flocculating sedimentation of Water purification processes, aluminium polychlorid has been most popular inorganic flocculating agent.High ph-values
With the water body of high alkalinity, it is most commonly that the reservoir water in autumn, owing to the reasons such as the breeding of algae and decomposition cause the PH of water body
Raising and the increase of basicity, the most often there is this situation in the most some other water system, is more such as giving of former water with Huanghe water
Water there is also these problems in processing.The preparation method that Chinese patent discloses the aluminium polychlorid of a kind of high aluminium content is (open
Number: CN1718543), its raw material is aluminium hydroxide and hydrochloric acid, is initially charged hydrochloric acid solution in a kettle., under stirring condition, adds
The crystalline aluminium hydroxide of industrial goods, aluminium hydroxide is 0.4-1: 2 with the molar ratio of hydrochloric acid, and has catalyst A to participate in reacting
Journey, aluminium hydroxide is 2-50 with the mol ratio of A, is 1-8Kgf/cm at steam pressure2Under conditions of, reaction temperature is 90-180
DEG C, more than 2 hours response time, after reaction terminates, the polymeric aluminium reaction thing of generation, put in stillpot, be aged 2 hours
Above, after ageing, the stillness of night is aluminium polychlorid finished product above, and this polyaluminium constructed of aluminium is with or without setting feature；Catalyst A is
Inorganic phosphorus compound.But in the water body of high pH or high alkalinity, use aluminium polychlorid to cause in water as flocculant
Residual Al exceed drinking water national standard, i.e. more than 0.2mg/Kg.
Summary of the invention
The present invention is to provide the preparation method of the aluminium polychlorid of a kind of low-residue aluminum, and it mainly solves prior art institute
Exist in the water body of high pH or high alkalinity, use the residual Al that causes in water as flocculant of aluminium polychlorid to exceed drink
Use water national standard, the i.e. technical problem more than 0.2mg/Kg etc..
The above-mentioned technical problem of the present invention is mainly addressed by following technical proposals:
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum of the present invention, it is characterised in that described method includes:
A., in closed reactor, put into hydrochloric acid and the stirring containing aluminum raw material is abundant, and be warmed to 120-1400C, pressure in still
At 0.15-0.3Mpa, obtain the aluminium polychlorid liquid that basicity is 0-30% and alchlor content is 5-15%；
B. in closed reactor, water, aluminic acid acid calcium powder or sodium aluminate, wherein three oxidations are added to above-mentioned aluminium polychlorid liquid
Aluminum content 7-9.5%, basicity controls at 80-90%；
C. reaction is discharged to agitator tank completely after filter pressing, addition sodium dihydrogen phosphate per ton and disodium hydrogen phosphate in agitator tank
Mixed aqueous solution 50-150Kg, in the mixed aqueous solution of sodium dihydrogen phosphate and disodium hydrogen phosphate, the quality of sodium dihydrogen phosphate is divided
Number is 20-30%, and the mass fraction of disodium hydrogen phosphate is 5-15%, and remaining is water, i.e. goes out finished product aluminium polychlorid after stirring.
When the key one of the present invention is to adjust basicity, feed liquid alchlor content controls at 7-9.5%, and basicity controls
80-90%, two is that the product after filter pressing uses sodium dihydrogen phosphate and phosphorus when adding other anion to increase the degree of polymerization of product
The mixture of acid disodium hydrogen.
When adjusting product basicity, the content such as the aluminium sesquioxide of aluminium polychlorid feed liquid is more than 10%, though product
Basicity be adjusted to 90%, this kind of product when processing the former water of high pH value high alkalinity, heavy after the residual Al of water the highest,
But flocculating effect is relatively good；As the content of the aluminium sesquioxide of aluminium polychlorid feed liquid is less than 7%, this kind of product is processing high pH
When being worth the former water of high alkalinity, the residual Al of heavy rear water can be controlled, but flocculating effect is relatively poor.Add phosphate radical from
During son increases the degree of polymerization of product thus improves flocculating effect, iff using sodium dihydrogen phosphate as interpolation
Agent, causes product to raise at the residual Al of the process of use after interpolation, this is owing to sodium dihydrogen phosphate is acidity, add
Process can cause the change of aluminum species；Iff use disodium hydrogen phosphate as additive, due to disodium hydrogen phosphate in
, there is gel aluminum hydroxide, and the flocculating effect of product is almost without being obviously improved in alkalescence in the product after interpolation.
The present invention is that formerly production basicity is the aluminium polychlorid of 10-30%；Aluminum is added again in above-mentioned aluminium polychlorid
Acid calcium powder or sodium aluminate, the alchlor content of aluminium polychlorid is strict controlled in 7-9.5%, and basicity controls at 80-90%,
Reach while the residual Al in the water body after flocculating sedimentation do not exceeds standard, to improve the flocculating effect of product；Reaction the most also filter pressing
After, add sodium dihydrogen phosphate and the mixed aqueous solution of disodium hydrogen phosphate, the residual Al in water body after not improving flocculating sedimentation
Content simultaneously, strengthen elimination of colloid stability ability and the hydrogen bond bridge formation ability of product, the flocculating sedimentation effect of product be greatly improved.
As preferably, described is aluminium hydroxide, bauxite, calcium aluminate powder containing aluminum raw material.
As preferably, the described concentration of hydrochloric acid in step a is 10-31%.
As preferably, reaction temperature when adding calcium aluminate powder or sodium aluminate in described step b is 900More than C, reaction
Time is 1-2 hour.
As preferably, described step C is added the reaction temperature of the mixed aqueous solution of sodium dihydrogen phosphate and disodium hydrogen phosphate
Degree is maintained at 500More than C, the response time is 30-60 minute.
As preferably, heating in described step a includes: be first slowly warmed up to 70-800C, then rapid cooling is to 20-
300C is also incubated 5-10 minute；Second time is slowly warmed up to 90-1000C, then rapid cooling is to 40-500C is also incubated 5-10 minute；
Third time is slowly warmed up to 120-1400C is also incubated；The described speed slowly heated up is 1-50C/min, the speed of rapid cooling
For 20-300C/min.Three slow risings fully can be decomposed containing aluminum raw material, then produces reaction with hydrochloric acid.By three
Secondary rapid cooling, can interrupt reaction rapidly, thus react next time, react the most repeatedly for three times, so that instead
Should be more complete so that the purity of aluminium polychlorid is higher.
As preferably, the inwall of the described agitator tank in step c is provided with some fins, the outer surface of fin be provided with in
The stirring rod of fan-shaped distribution.Each component in agitator tank can be sufficiently stirred for by stirring rod, owing to stirring rod is fan
Shape is distributed, and so area of stirring is bigger.
As preferably, the bottom of the described agitator tank in step c has some punching grooves, and the width within punching groove is little
Width in its opening part.During by punching groove so that stir, liquid can enter in punching groove, due in punching groove
The width in portion is less than the width of its opening part, and the hydraulic pressure within such punching groove is relatively big, so that mixing is more complete.
Therefore, the aluminium polychlorid of the present invention is when processing the former water of high PH high alkalinity, and the heavy rear water after flocculating sedimentation is residual
Remaining aluminum significantly reduces, and can guarantee that excellent flocculating effect.
Accompanying drawing explanation
Accompanying drawing 1 is a kind of structural representation of the inwall of agitator tank of the present invention；
Accompanying drawing 2 is a kind of structural representation of the bottom of agitator tank of the present invention.
Parts, position and numbering in figure: agitator tank 1, fin 2, stirring rod 3, punching groove 4.
Detailed description of the invention
Below by embodiment, and combine accompanying drawing, technical scheme is described in further detail.
Embodiment 1: the preparation method of the aluminium polychlorid of a kind of low-residue aluminum of this example, the steps include:
Adding the hydrochloric acid of 5 tons of concentration 15%, the aluminium hydroxide of 570Kg in 10000L reactor, this aluminium hydroxide contains Al2O3% is
64%(m/m), moisture content is 5.5%, is first slowly warmed up to 75 in closed reactor0C, then rapid cooling is to 250C is also incubated 8 points
Clock；Second time is slowly warmed up to 950C, then rapid cooling is to 450C is also incubated 8 minutes；Third time is slowly warmed up to 1300C also protects
Temperature；The speed slowly heated up is 30C/min, the speed of rapid cooling is 300C/min.Stirring reaction 3 hours, obtains containing Al2O3
For 6.1%(m/m), basicity is the aluminum chloride liquid of 2%, adds calcium aluminate powder 1.1 tons, this calcium in above-mentioned aluminium polychlorid liquid
The Al of powder2O3% is 50%(m/m), total calcium is 32%(m/m), 2.76 tons of water, it is maintained at 900More than C, reacts 1 in closed reactor
Hour, obtain containing Al2O3For 8.9%(m/ m)；Basicity is 88%；The aluminium polychlorid of density 1.20 grams per milliliter；Reaction is completely
After filter pressing immediately, cleaner liquid is put in intermediate agitation groove, and now feed temperature is 650About C, adds disodium hydrogen phosphate and phosphoric acid
The mixed aqueous solution 800Kg of sodium dihydrogen, consisting of of this mixed aqueous solution: the mass fraction of sodium dihydrogen phosphate is 20%, phosphoric acid hydrogen
The mass fraction of disodium is 10%, stirs 30 minutes, i.e. obtains containing Al2O3For 8.4%(m/ m)；Basicity is 91%；Phosphate radical contains
Amount is 1.8%；The aluminium polychlorid of density 1.20 grams per milliliter.
Chemical equation is:
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, the inwall of agitator tank 1 is provided with some fins 2, and the outer surface of fin is provided with in sector stirring of distribution
Mix rod 3.
Such as Fig. 2, the bottom of agitator tank 1 has some punching grooves 4, and the width within punching groove is less than the width of its opening part
Degree.
Embodiment 2: the preparation method of the aluminium polychlorid of a kind of low-residue aluminum of this example, the steps include:
Claiming the hydrochloric acid of 100 grams of concentration 31%, add 26 grams of aluminium hydroxide, this aluminium hydroxide contains Al2O3% is 64%(m/m), aqueous
Rate is 4%(m/m), hermetic container is first slowly warmed up to 75 in closed reactor0C, then rapid cooling is to 250C is also incubated 8 points
Clock；Second time is slowly warmed up to 950C, then rapid cooling is to 450C is also incubated 8 minutes；Third time is slowly warmed up to 1300C also protects
Temperature；The speed slowly heated up is 30C/min, the speed of rapid cooling is 300C/min, stirring reaction 2.5 hours, contained
Al2O3For 12.6%(m/m), basicity is the aluminum chloride liquid of 10%, adds calcium aluminate powder 42g in above-mentioned aluminium polychlorid liquid,
The Al of this calcium powder2O3% is 50%(m/m), total calcium is 32%(m/m), water 180g, it is maintained at 900More than C, reacts in closed reactor
90 minutes, obtain containing Al2O3For 9.9%(m/ m)；Basicity is 85%；The aluminium polychlorid of density 1.23 grams per milliliter；React
Sucking filtration immediately after Quan, cleaner liquid is put in intermediate agitation groove, adds disodium hydrogen phosphate and the mixed aqueous solution of sodium dihydrogen phosphate
38g, consisting of of this mixed aqueous solution: the mass fraction of sodium dihydrogen phosphate is 20%, the mass fraction of disodium hydrogen phosphate is 15%,
Heating keeps temperature 55-600C stirs 45 minutes, i.e. obtains containing Al2O3For 8.9%(m/ m)；Basicity is 88%；Phosphate content
It is 2.5%；The aluminium polychlorid of density 1.21 grams per milliliter.
Chemical equation is:
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, the inwall of agitator tank 1 is provided with some fins 2, and the outer surface of fin is provided with in sector stirring of distribution
Mix rod 3.
Such as Fig. 2, the bottom of agitator tank 1 has some punching grooves 4, and the width within punching groove is less than the width of its opening part
Degree.
After above example 1, embodiment 2, product are used for certain currently used typical polymerization aluminum chloride, residual Al exceeds standard
Former water coagulation stirring test, contrasts with currently used aluminium polychlorid simultaneously.Result see table:
| Former water water temperature: 20.30C | Raw water turbidity: 4.2NTU | Former water aluminium ion concentration: 0.05 mg/Kg |
From result above, this aluminium polychlorid is when process is easily generated the former water that residual Al exceeds standard, normal ensure that
On the basis of flocculating effect, residual Al reduces about 50%.
The foregoing is only the specific embodiment of the present invention, but the architectural feature of the present invention is not limited thereto, Ren Heben
The technical staff in field is in the field of the invention, and change or the modification made all are contained among the scope of the claims of the present invention.
Claims (8)
1. the preparation method of the aluminium polychlorid of a low-residue aluminum, it is characterised in that described method includes:
A., in closed reactor, put into hydrochloric acid and the stirring containing aluminum raw material is abundant, and be warmed to 120-1400C, in still, pressure exists
0.15-0.3Mpa, obtains the aluminium polychlorid liquid that basicity is 0-30% and alchlor content is 5-15%；
B. in closed reactor, water, aluminic acid acid calcium powder or sodium aluminate, wherein three oxidations are added to above-mentioned aluminium polychlorid liquid
Aluminum content 7-9.5%, basicity controls at 80-90%；
C. reaction is discharged to agitator tank completely after filter pressing, addition sodium dihydrogen phosphate per ton and disodium hydrogen phosphate in agitator tank
In the mixed aqueous solution of mixed aqueous solution 50-150Kg, sodium dihydrogen phosphate and disodium hydrogen phosphate, the mass fraction of sodium dihydrogen phosphate
For 20-30%, the mass fraction of disodium hydrogen phosphate is 5-15%, and remaining is water, i.e. goes out finished product aluminium polychlorid after stirring.
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum the most according to claim 1, it is characterised in that described
It is aluminium hydroxide, bauxite, calcium aluminate powder containing aluminum raw material.
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum the most according to claim 1, it is characterised in that described
Concentration of hydrochloric acid in step a is 10-31%.
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum the most according to claim 1, it is characterised in that described
Reaction temperature when adding calcium aluminate powder or sodium aluminate in step b is 900More than C, the response time is 1-2 hour.
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum the most according to claim 1, it is characterised in that described
The reaction temperature of the mixed aqueous solution adding sodium dihydrogen phosphate and disodium hydrogen phosphate in step C is maintained at 500More than C, during reaction
Between be 30-60 minute.
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum the most according to claim 1, it is characterised in that described
Heating in step a includes: be first slowly warmed up to 70-800C, then rapid cooling is to 20-300C is also incubated 5-10 minute；For the second time
Slowly it is warmed up to 90-1000C, then rapid cooling is to 40-500C is also incubated 5-10 minute；Third time is slowly warmed up to 120-1400C
And be incubated；The described speed slowly heated up is 1-50C/min, the speed of rapid cooling is 20-300C/min。
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum the most according to claim 1, it is characterised in that described
The inwall of the agitator tank (1) in step c is provided with some fins (2), and the outer surface of fin is provided with the stirring rod of distribution in sector
(3).
The preparation method of the aluminium polychlorid of a kind of low-residue aluminum the most according to claim 1, it is characterised in that described
The bottom of the agitator tank (1) in step c has some punching grooves (4), and the width within punching groove is less than the width of its opening part.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107265591A (en) * | 2017-07-27 | 2017-10-20 | 柳三春 | Complex solid water treatment agent and preparation method thereof |
| CN107540066A (en) * | 2017-07-27 | 2018-01-05 | 杭州萧山三江净水剂有限公司 | A kind of preparation technology of poly- phosphorus aluminium chloride |
| CN110002484A (en) * | 2019-05-20 | 2019-07-12 | 河南爱尔福克化学股份有限公司 | A kind of preparation method of basicity aluminium polychloride |
| 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 |
| CN110963662A (en) * | 2019-12-09 | 2020-04-07 | 上海净屹环保科技有限公司 | Method for recovering aluminum salt coagulant from aluminum-containing sludge |
| CN111320194A (en) * | 2020-04-24 | 2020-06-23 | 山东中科天泽净水材料有限公司 | Preparation method of aluminum glue and polyaluminium chloride |
| CN112142173A (en) * | 2020-08-04 | 2020-12-29 | 广西锋盛环保科技有限公司 | Preparation method of high-basicity polyaluminium chloride water purifying agent |
| 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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| CN107265591A (en) * | 2017-07-27 | 2017-10-20 | 柳三春 | Complex solid water treatment agent and preparation method thereof |
| CN107540066A (en) * | 2017-07-27 | 2018-01-05 | 杭州萧山三江净水剂有限公司 | A kind of preparation technology of poly- phosphorus aluminium chloride |
| CN107540066B (en) * | 2017-07-27 | 2020-09-04 | 杭州萧山三江净水剂有限公司 | Preparation process of poly-phosphorus aluminum chloride |
| CN110002484A (en) * | 2019-05-20 | 2019-07-12 | 河南爱尔福克化学股份有限公司 | A kind of preparation method of basicity aluminium polychloride |
| 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 |
| CN110963662A (en) * | 2019-12-09 | 2020-04-07 | 上海净屹环保科技有限公司 | Method for recovering aluminum salt coagulant from aluminum-containing sludge |
| CN111320194A (en) * | 2020-04-24 | 2020-06-23 | 山东中科天泽净水材料有限公司 | Preparation method of aluminum glue and polyaluminium chloride |
| CN112142173A (en) * | 2020-08-04 | 2020-12-29 | 广西锋盛环保科技有限公司 | Preparation method of high-basicity polyaluminium chloride water purifying agent |
| 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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