CN102068971B - Preparation method of poly-aluminum silicate - Google Patents
Preparation method of poly-aluminum silicate Download PDFInfo
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- CN102068971B CN102068971B CN 201010572926 CN201010572926A CN102068971B CN 102068971 B CN102068971 B CN 102068971B CN 201010572926 CN201010572926 CN 201010572926 CN 201010572926 A CN201010572926 A CN 201010572926A CN 102068971 B CN102068971 B CN 102068971B
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Abstract
The invention provides a preparation method of poly-aluminum silicate catalyst, and belongs to the field of water treatment. The preparation method comprises the following steps of: titrating alkali metal silicate aqueous solution in aluminum salt solution for copolymerization; keeping standing for a period of time after complete reaction; and activating and drying precipitate to obtain the needed catalyst. The preparation method is characterized in that under a certain temperature and mechanical stirring strength, reaction is carried out according to a certain stoichiometric ratio and dosing sequence; and after the reaction, white solid powder of the poly-aluminum silicate is obtained by activating, washing, drying and other procedures. The preparation method has the advantages of simple process and low requirement for reaction conditions; and the obtained product has the advantages of high efficiency, excellent stability and long service life, and is applicable to industrial production.
Description
Technical field
The invention belongs to water treatment field.
Background technology
In recent years, along with the develop rapidly of China's industrialization degree and increasing substantially of economic level, the production of multi-form chemical substance and use increasingly causes the kind of water source water pollutant and quantity obviously to increase, and has increased the weight of the pollution level of water environment.The trace toxic persistent organic pollutants that exist in water body are more and more paid close attention to because its damaging effect, toxicological characteristics, pollution level and trend have been subject to people.Conventional handling technology of water supply (coagulation-precipitation-filtration-sterilization) is to remove that in water, suspension and colloid pollution thing are main, and is very poor to the removal effect of persistent organic pollutants, even helpless.In order significantly to improve water quality, guarantee, the advanced treating technology is widely used in the middle of water treatment.Wherein, the heterogeneous catalytic ozonation technology of utilizing organic matter in the hydroxyl radical free radical oxidation Decomposition water that produces in course of reaction to reach the purification of water quality purpose has been subject to people's extensive attention.This technical operation is simple, does not need to introduce other energy and poisonous and hazardous chemical agent in technique, and catalyst can disposablely be loaded in reactor, is convenient to apply in the water treatment technology of reality.Metal oxide (TiO
2, MnO
2, ZnOOH, FeOOH etc.) the existing a large amount of report of pollutant in catalytic ozonation degradation water.But the preparation method of relevant polymeric silicicacid Al catalysts is rarely seen report also.
Summary of the invention
The preparation method who the purpose of this invention is to provide polymer aluminium silicate.
The preparation method of polymer aluminium silicate of the present invention carries out in the steps below: one, the mixing speed take 100r/min ~ 150r/min constantly stirs concentration as the soluble aluminum salting liquid of 0.5mol/L ~ 2.0mol/L, and slowly drip the alkali metal silicate aqueous solution that concentration is 0.5mol/L ~ 2.5mol/L until the pH value is 8 ~ 9, obtain mixed liquor; Two, with gained in step 1 the quiet heavy 20 ~ 30min of mixture, then the environment that is placed in 40 ℃ ~ 90 ℃ activates 10 ~ 30h, sediment after activation deionized water cyclic washing, adopt the centrifuge of 2000 ~ 4000r/min to carry out Separation of Solid and Liquid, clean be 7.0 ~ 7.5 to the pH value of supernatant after, drying, then grind, sieve, getting particle diameter is 0.075 ~ 0.15mm, namely obtains polymer aluminium silicate.
This catalyst is the particle diameter white powder that is evenly distributed, and is easy to disperse in water, and specific area is large, and settling property is good.
The catalyst sedimentation performance of the present invention's preparation is good, is whole sedimentations after 30s in polymeric silicicacid Al catalysts input water in static test.After granulation, mechanical strength is high, and water resistant power impact property is good.Promote ozone decomposed to generate hydroxyl radical free radical, increase generating rate and the quantity of free radical in water body, can make the utilization rate of ozone improve 15 ~ 25 percentage points, O3 catalytic oxidation has improved 43 ~ 51 percentage points than independent ozone oxidation to the clearance of organic pollutants.
Technique of the present invention is simple, the reaction condition requirement is low, and the product that makes has advantages of efficiently, stable and long service life, is applicable to suitability for industrialized production.That form with powder exists after the prepared polymer aluminium silicate drying of the inventive method.This catalyst can be combined with jointing material prilling process such as adopting mold pressing or extruding and be processed to form larger particle, thereby is applicable in actual water treatment technology.Normally the particle form with diameter 0.5-5mm is the most favourable when polymer aluminium silicate is tested as O3 catalytic oxidation.
Description of drawings
Fig. 1 be nine pairs of organic pollutants nitro-chlorobenzenes of the specific embodiment (the 2-chloronitrobenzene (
oCNB), the 3-chloronitrobenzene (
mCNB) and the 4-chloronitrobenzene (
pCNB)) removal effect figure, zero expression polymer aluminium silicate catalysis ozone pair in figure
oCNB removes curve, and ■ represents polymer aluminium silicate catalysis ozone pair
pCNB removes curve, and the △ curve represents polymer aluminium silicate catalysis ozone pair
mCNB removes curve, and in figure, ▼ represents ozone pair
pCNB removes curve,
Expression ozone pair
oCNB removes curve,
Expression ozone pair
mCNB removes curve.
The specific embodiment
The specific embodiment one: in present embodiment, the preparation method of polymer aluminium silicate carries out in the steps below: one, the mixing speed take 100r/min ~ 150r/min constantly stirs concentration as the soluble aluminum salting liquid of 0.5mol/L ~ 2.0mol/L, and slowly drip the alkali metal silicate aqueous solution that concentration is 0.5mol/L ~ 2.5mol/L until the pH value is 8 ~ 9, obtain mixed liquor; Two, with gained in step 1 the quiet heavy 20 ~ 30min of mixture, then the environment that is placed in 40 ℃ ~ 90 ℃ activates 10 ~ 30h, sediment after activation deionized water cyclic washing, adopt the centrifuge of 2000 ~ 4000r/min to carry out Separation of Solid and Liquid, clean be 7.0 ~ 7.5 to the pH value of supernatant after, drying, then grind, sieve, getting particle diameter is 0.075 ~ 0.15mm, namely obtains polymer aluminium silicate.
The specific embodiment two: what present embodiment was different from the specific embodiment one is: the described alkali silicate of step 1 is sodium metasilicate, potassium silicate or waterglass.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from the specific embodiment one or two is: the described aluminum soluble salt of step 1 is aluminum nitrate, aluminum sulfate or aluminium chloride.Other step and parameter are identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment was different from one of specific embodiment one to three is: the described activation temperature of step 2 is 50 ℃ ~ 80 ℃.Other step and parameter are identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to three is: the described activation temperature of step 2 is 60 ℃.Other step and parameter are identical with one of specific embodiment one to three.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is: the described soak time of step 2 is 16 ~ 20h.Other step and parameter are identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different from one of specific embodiment one to five is: the described soak time of step 2 is 18h.Other step and parameter are identical with one of specific embodiment one to five.
The specific embodiment eight: what present embodiment was different from one of specific embodiment one to seven is: the described baking temperature of step 2 is 40 ~ 90 ℃, drying time 18 ~ 32h.Other step and parameter are identical with one of specific embodiment one to seven.
The specific embodiment nine: the preparation method of present embodiment polymer aluminium silicate carries out in the steps below: the soluble aluminum salting liquid that, constantly stirs concentration 1.5mol/L with the mixing speed of 150r/min, and slowly drip the alkali metal silicate aqueous solution that concentration is 2.0mol/L until the pH value is 8, obtain mixed liquor; Two, with gained in step 1 the quiet heavy 20min of mixture, then the environment that is placed in 60 ℃ activates 24h, sediment after activation deionized water cyclic washing, adopt the centrifuge of 3000r/min to carry out Separation of Solid and Liquid, clean be=7.0 to the pH value of supernatant after, dry 24h in the drying box of 65 ℃, then grind, sieve, getting particle diameter is 0.075 ~ 0.15mm, namely obtains polymer aluminium silicate.
Adopt following verification experimental verification effect of the present invention:
Depollution experiment is carried out in capacity is the plan boiling flask reactor of 1.2L, passes into O in the reactor that contains 1000mL distilled water (preset pH=7.5)
3/ O
2Mist, after certain hour, stop aeration, in the aqueous solution at this moment, ozone concentration is 0.5mg/L, adding 1mL concentration in the reactor at once is the CNBs stock solution of 100mg/L and the polymerization catalyst alumina silicate of 150mg, opens magnetic stirring apparatus and carries out stirring reaction.Analyze the moment (0min, 1min, 3min, 5min, 10min and 15min) from the sample tap sampling, institute's water sampling need be used the Na of 100 μ L immediately at each
2S
2O
3Solution (0.1mol/L) stops ozone oxidation reaction.Adopt the acetate fiber ultrafiltration membrance filter 40mL water sample of 0.45 μ m, get 1.5mL with liquid-transfering gun and pack into and carry out liquid-phase chromatographic analysis after chromatogram bottle.Result as shown in Figure 1, as shown in Figure 1, separately during ozone oxidation,
mCNB,
oCNB and
pThe clearance of CNB is respectively 48%, 53% and 54%, show that independent ozone oxidation is limited to the oxidability of CNBs. during polymer aluminium silicate O3 catalytic oxidation CNBs, after reaction 15min, the CNBs clearance all can reach respectively more than 94%, more independent oxygen oxidation CNBs has improved respectively 51%, 43% and 45%.
Claims (8)
1. the preparation method of polymer aluminium silicate, the preparation method who it is characterized in that polymer aluminium silicate carries out in the steps below: one, the mixing speed take 100r/min ~ 150r/min constantly stirs concentration as the soluble aluminum salting liquid of 0.5mol/L ~ 2.0mol/L, and slowly drip the alkali metal silicate aqueous solution that concentration is 0.5mol/L ~ 2.5mol/L until the pH value is 8 ~ 9, obtain mixed liquor; Two, with gained in step 1 the quiet heavy 20 ~ 30min of mixture, then the environment that is placed in 40 ℃ ~ 90 ℃ activates 10 ~ 30h, sediment after activation deionized water cyclic washing, adopt the centrifuge of 2000 ~ 4000r/min to carry out Separation of Solid and Liquid, clean be 7.0 ~ 7.5 to the pH value of supernatant after, drying, then grind, sieve, getting particle diameter is 0.075 ~ 0.15mm, namely obtains polymer aluminium silicate.
2. the preparation method of polymer aluminium silicate according to claim 1, is characterized in that the described alkali silicate of step 1 is sodium metasilicate, potassium silicate or waterglass.
3. the preparation method of polymer aluminium silicate according to claim 2, is characterized in that the described aluminum soluble salt of step 1 is aluminum nitrate, aluminum sulfate or aluminium chloride.
4. the preparation method of polymer aluminium silicate according to claim 3, is characterized in that the described activation temperature of step 2 is 50 ℃ ~ 80 ℃.
5. the preparation method of polymer aluminium silicate according to claim 3, is characterized in that the described activation temperature of step 2 is 60 ℃.
6. the preparation method of polymer aluminium silicate according to claim 4, is characterized in that the described soak time of step 2 is 16 ~ 20h.
7. the preparation method of polymer aluminium silicate according to claim 4, is characterized in that the described soak time of step 2 is 18h.
8. the preparation method of polymer aluminium silicate according to claim 6, is characterized in that the described baking temperature of step 2 is 40 ~ 90 ℃, drying time 18 ~ 32h.
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| CN102527368A (en) * | 2011-12-21 | 2012-07-04 | 哈尔滨工业大学 | Preparation method for zinc aluminum polysilicate catalyst |
| CN109336122B (en) * | 2018-12-06 | 2023-02-28 | 中国矿业大学(北京) | Preparation method of aluminum silicate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100369827C (en) * | 2005-11-10 | 2008-02-20 | 暨南大学 | Process for producing basic poly aluminium sulfate silicate by one step method |
| CN101298346A (en) * | 2008-07-01 | 2008-11-05 | 北京大学 | Polysilicate aluminum sulphate flocculant, preparation process and use thereof |
| CN101798092A (en) * | 2010-04-26 | 2010-08-11 | 哈尔滨工业大学 | Polyferro-silicate, preparation method thereof and applications thereof in water treatment |
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2010
- 2010-12-03 CN CN 201010572926 patent/CN102068971B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100369827C (en) * | 2005-11-10 | 2008-02-20 | 暨南大学 | Process for producing basic poly aluminium sulfate silicate by one step method |
| CN101298346A (en) * | 2008-07-01 | 2008-11-05 | 北京大学 | Polysilicate aluminum sulphate flocculant, preparation process and use thereof |
| CN101798092A (en) * | 2010-04-26 | 2010-08-11 | 哈尔滨工业大学 | Polyferro-silicate, preparation method thereof and applications thereof in water treatment |
Non-Patent Citations (2)
| Title |
|---|
| 周风山等.含硅多核无机高分子絮凝剂研究进展.《油田化学》.2002,第19卷(第4期),391-394页. * |
| 林莉.聚硅酸铝盐絮凝剂的应用及研究进展.《广东化工》.2008,第35卷(第180期),39-41,96页. * |
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