CN104478051A - Method for preparing poly-aluminum ferric silicate sulfate flocculating agent - Google Patents
Method for preparing poly-aluminum ferric silicate sulfate flocculating agent Download PDFInfo
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- CN104478051A CN104478051A CN201410749847.XA CN201410749847A CN104478051A CN 104478051 A CN104478051 A CN 104478051A CN 201410749847 A CN201410749847 A CN 201410749847A CN 104478051 A CN104478051 A CN 104478051A
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- tetraethoxy
- molysite
- aluminium salt
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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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- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Water Supply & Treatment (AREA)
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a method for preparing a poly-aluminum ferric silicate sulfate flocculating agent. The method comprises the following steps: reacting tetraethyl orthosilicate serving as raw material with boiling water to generate silica sol; controlling the rotating speed to be 400 revolutions per minute, adding an aluminum salt into the silica sol at the temperature of 50 DEG C, adding a ferric salt after the aluminum salt is completely dissolved, controlling the rotating speed to be 100 to 200 revolutions per minute, further stirring until the solution becomes a reddish brown transparent solution, stopping stirring, keeping in a dark place and curing for 4-6 hours, thereby obtaining the poly-aluminum ferric silicate sulfate flocculating agent. According to the amount of the aluminum salt and the ferric salt, the molar ratio of the total amount of Al and Fe to Si in the silica sol is 1:1, and the ratio of Al to Fe is 1.2-2:1. According to the preparation method, tetraethyl orthosilicate serves as a silicon source, the selectivity of the silicon source is improved, and the obtained poly-aluminum ferric silicate sulfate flocculating agent is slightly influenced by the pH value and is good in flocculating effect; the preparation method is simple in process, convenient to operate, low in requirements on reaction equipment and suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of polymeric aluminium ferrum silicate flocculant.
Background technology
Polymeric aluminium ferrum silicate (PSAF) is a kind of novel water-soluble macromolecule electrolyte.Be mainly used in purifying drinking water, also can be used for the special water quality process of feedwater, except cadmium, except fluorine, radioactive contamination eliminating, de-floating wet goods.This external Industrial Wastewater Treatment, as dyeing waste water etc., also extensive application in casting, papermaking, medicine, process hides etc.It has the effect of getting instant result at sewage treatment area for the process of sewage, is sewage treatment drug very salable at present.
The most frequently used method of current synthesized polymer aluminium iron silicate is exactly take silicate solutions as raw material, and activation generates silicic acid in acid condition, and then adds aluminium salt and molysite, can obtain silicate aluminium ferric flocculating agent.Paper " preparation and application of polymeric aluminium ferrum silicate " " Sichuan chemical industry and corrosion control " (2003 phase in the end of the year 1 the 6th volume) as Ma Yongmei discloses in one water glass and sulfuric acid and obtained polysilicon acid solution, react with Tai-Ace S 150, liquor ferri trichloridi again, the poly silicate aluminium ferric flocculating agent that obtained flocculating property is excellent.The paper " development of poly-aluminum-ferric-silicate-sulfate and flocculating property thereof " " water technology " (volume the 9th phase September the 34th in 2008) of Zhang Mengcun discloses a kind of preparation method of poly-aluminum-ferric-silicate-sulfate, utilize industrial waste sulfuric acid pickling waste liquid, water glass and aluminum chloride for raw material, make polymeric aluminium ferrum silicate (PASS) under certain condition.
Patent CN 1907878A is with water glass, sulfuric acid, aluminium salt, molysite for raw material, and Si:Al:Fe mol ratio is that 0.3:1:2 or 0.3:1:1.5 carries out reaction generation poly silicate aluminium ferric flocculating agent.Although this poly silicate aluminium ferric flocculating agent can play the part advantage of polymeric aluminium ferrum silicate, but be raw material with silicate, the polymeric aluminium ferrum silicate flocculant of gained is comparatively large by the impact of pH, thus have impact on flocculating effect.
Summary of the invention
The object of the invention is to solve above-mentioned raw materials single, be subject to the technical problems such as pH impact and a kind of preparation method of polymeric aluminium ferrum silicate flocculant is provided, this preparation method take tetraethyl orthosilicate as silicon source, add the selectivity in silicon source, and the polymeric aluminium ferrum silicate flocculant of gained is little by pH impact effect, and flocculating effect is better.
Technical scheme of the present invention
A preparation method for polymeric aluminium ferrum silicate flocculant, specifically comprises the steps:
(1), distilled water is heated to boil, then controlling drop rate is 1ml/mim, and rotating speed is be added drop-wise to wherein by tetraethoxy under 500r/min, dropwises and continues to control to adjust pH to be 9-11 with aqueous sodium hydroxide solution after identical rotating speed stirs 40min, then slaking 4h, obtains silicic acid sol;
The consumption of tetraethoxy, in distilled water: the volume ratio of tetraethoxy is the ratio calculating of 10-20:1;
Above-mentioned is must slowly and rapid stirring adding tetraethoxysilance in boiling water, generates, if rate of addition is too fast, may set off an explosion because have ethanol in the process of reacting at tetraethoxy and boiling water;
(2), controlling rotating speed is 400r/min, temperature is add aluminium salt to the silicic acid sol of step (1) gained at 50 DEG C, molysite is added again after aluminium salt dissolves completely, controlling rotating speed is that 100-200r/min continues to stir until solution becomes reddish-brown clear solution, then stop stirring, lucifuge slaking 4-6h, namely obtains polymeric aluminium ferrum silicate flocculant;
Described aluminium salt is the mixture of aluminum chloride, Tai-Ace S 150 or aluminum chloride and Tai-Ace S 150;
Described molysite is the mixture of iron(ic) chloride, ferric sulfate or iron(ic) chloride and ferric sulfate;
The consumption of described aluminium salt and molysite, calculates in molar ratio, i.e. the total amount of Al and Fe: the Si in silicic acid sol is 1:1, and wherein Al:Fe is 1.2-2:1.
Beneficial effect of the present invention
The preparation method of a kind of polymeric aluminium ferrum silicate flocculant of the present invention, owing to using tetraethoxysilance for silicon source in preparation process, add the silicon source diversity preparing poly silicate aluminium ferric flocculating agent, and the polymeric aluminium ferrum silicate flocculant of final gained is less by the impact of pH, flocculating effect is better, and use range is wider.
Embodiment
Below by specific embodiment, the present invention is set forth further, but do not limit the present invention.
The measuring method (provide INSTRUMENT MODEL and producer in an embodiment, do not have concrete method, just survey with instrument) of turbidity in Application Example of the present invention.
embodiment 1
A preparation method for polymeric aluminium ferrum silicate flocculant, specifically comprises the steps:
(1) beaker of 500ml, is got, add 200ml distilled water, distilled water in beaker is boiled, then controlling drop rate is 1ml/mim, mixing speed is in boiling water, slowly add 10ml tetraethoxy under 500r/min, drips the identical rotating speed of rear continuation control and carries out stirring 30min, then regulate pH to be 10 with sodium hydroxide solution, slaking 4h, obtains silicic acid sol;
The consumption of tetraethoxy, calculates by volume, i.e. distilled water: tetraethoxy is 20:1;
Above-mentioned is must slowly and rapid stirring adding tetraethoxysilance in boiling water, generates, if rate of addition is too fast, may set off an explosion because have ethanol in the process of reacting at tetraethoxy and boiling water;
(2), controlling rotating speed is 400r/min, temperature is first add 6.27g aluminium salt to the silicic acid sol of step (1) gained at 50 DEG C, the solution of gained becomes oyster white, when it becomes again clarification, add 8.8g molysite again, controlling rotating speed is that 200r/min continues to stir, now solution colour starts to deepen gradually, and it is muddy with orange, then color again further deepen and solution becomes clarification gradually, finally become reddish-brown clear solution, then stop stir, lucifuge slaking 6h, namely obtains polymeric aluminium ferrum silicate flocculant;
Described aluminium salt is AlCl
36H
2o;
Described molysite is Fe
2(SO
4)
3;
The consumption of described aluminium salt and molysite, calculates in molar ratio, i.e. the total amount of Al and Fe: the Si in silicic acid sol is 1:1, and wherein Al:Fe is 1.2:1.
embodiment 2
A preparation method for polymeric aluminium ferrum silicate flocculant, specifically comprises the steps:
(1) beaker of 500ml, is got, add 200ml distilled water, distilled water in beaker is boiled, then controlling drop rate is 1ml/mim, mixing speed is in boiling water, slowly add 20ml tetraethoxy under 500r/min, and drip the identical rotating speed of rear continuation control and carry out stirring 40min, then carrying out adjustment pH with sodium hydroxide solution is 11, slaking 4h, obtains silicic acid sol;
The consumption of tetraethoxy, calculates by volume, i.e. distilled water: tetraethoxy is 10:1;
Above-mentioned is must slowly and rapid stirring adding tetraethoxysilance in boiling water, generates, if rate of addition is too fast, may set off an explosion because have ethanol in the process of reacting at tetraethoxy and boiling water;
(2), controlling rotating speed is 200r/min, temperature is in the silicic acid sol of step (1) gained, first add 15.73g aluminium salt at 60 DEG C, the solution of gained becomes oyster white, when it becomes again clarification, add 8.66g molysite again, controlling rotating speed is that 200r/min continues to stir, now solution colour starts to deepen gradually, and it is muddy with orange, then color again further deepen and solution becomes clarification gradually, finally become reddish-brown clear solution, then stop stir, lucifuge slaking 6h, namely obtains polymeric aluminium ferrum silicate flocculant;
Described aluminium salt is Al
2(SO
4)
3;
Described molysite is FeCl
36H
2o
The consumption of described aluminium salt and molysite, calculates in molar ratio, i.e. the total amount of Al and Fe: the Si in silicic acid sol is 1:1, and wherein Al:Fe is 2:1.
application Example 1
The polymeric aluminium ferrum silicate flocculant of embodiment 1 gained and commercially available polymeric aluminium ferrum silicate (Hubei flourishing age Environmental Protection Technology Co., Ltd) are rendered to prior instrument (A15/76 respectively, great river, Beijing mechanical electronic equipment) turbidity that measured is the unit of 60NTU(turbidity), pH value is respectively in the muddy water of 4.6,6.9,9.3, simple mix and blend 30min, settlement treatment 2h, the turbidity value of injected volume and the rear muddy water of process is as following table:
As can be seen from the above table, the poly-ferrosilicoaluminum flocculation agent prepared by the present invention, compared with commercially available polymeric aluminium ferrum silicate, has more excellent turbidity removal effect, and affects also less by the pH of pending muddy water.
In sum, the present invention is that the poly silicate aluminium ferric flocculating agent of silicon source gained affects less by pH with tetraethoxysilance, and better to the treatment effect of muddy water, therefore use range is wider.
The above is only the citing of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (3)
1. a preparation method for polymeric aluminium ferrum silicate flocculant, is characterized in that specifically comprising the steps:
(1), distilled water is heated to boil, then controlling drop rate is 1ml/mim, rotating speed is be added drop-wise to wherein by tetraethoxy under 500r/min, dropwise and continue to control to adjust pH to be 9-11 with aqueous sodium hydroxide solution after identical rotating speed carries out stirring 40min, then slaking 4h, obtains silicic acid sol;
The consumption of tetraethoxy, in distilled water: the volume ratio of tetraethoxy is the ratio calculating of 10-20:1;
(2), controlling rotating speed is 400r/min, temperature is first add aluminium salt to the silicic acid sol of step (1) gained at 50 DEG C, molysite is added again after aluminium salt dissolves completely, controlling rotating speed is that 100-200r/min continues to stir until solution becomes reddish-brown clear solution, then stop stirring, lucifuge slaking 4-6h, namely obtains polymeric aluminium ferrum silicate flocculant;
Described aluminium salt is the mixture of aluminum chloride, Tai-Ace S 150 or aluminum chloride and Tai-Ace S 150;
Described molysite is the mixture of iron(ic) chloride, ferric sulfate or iron(ic) chloride and ferric sulfate;
The consumption of described aluminium salt and molysite, calculates in molar ratio, i.e. the total amount of Al and Fe: the Si in silicic acid sol is 1:1, and wherein Al:Fe is 1.2-2:1.
2. the preparation method of a kind of polymeric aluminium ferrum silicate flocculant as claimed in claim 1, is characterized in that:
In step (1), the consumption of tetraethoxy, calculates, i.e. distilled water: tetraethoxy is 20:1 by volume;
Described in step (2), aluminium salt is AlCl
36H
2o, described molysite is Fe
2(SO
4)
3; The consumption of described aluminium salt and molysite, calculates in molar ratio, i.e. the integral molar quantity of Al and Fe: the molar weight of the Si in silicic acid sol is 1:1, and wherein Al:Fe is 1.2:1.
3. the preparation method of a kind of polymeric aluminium ferrum silicate flocculant as claimed in claim 1, is characterized in that:
In step (1), the consumption of tetraethoxy, calculates, i.e. distilled water: tetraethoxy is 10:1 by volume;
Described in step (2), aluminium salt is Al
2(SO
4)
3, described molysite is FeCl
36H
2o; The consumption of described aluminium salt and molysite, calculates in molar ratio, i.e. the integral molar quantity of Al and Fe: the molar weight of the Si in silicic acid sol is 1:1, and wherein Al:Fe is 2:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410749847.XA CN104478051A (en) | 2014-12-10 | 2014-12-10 | Method for preparing poly-aluminum ferric silicate sulfate flocculating agent |
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| CN201410749847.XA CN104478051A (en) | 2014-12-10 | 2014-12-10 | Method for preparing poly-aluminum ferric silicate sulfate flocculating agent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909440A (en) * | 2015-04-29 | 2015-09-16 | 南通大学 | New composite ethyl orthosilicate-polyaluminium chloride flocculant preparation method |
| CN105481072A (en) * | 2016-01-19 | 2016-04-13 | 昆明跃高工贸有限公司 | Preparation method of PSAF (polysilicate aluminum ferric) flocculant |
| CN106006900A (en) * | 2016-07-21 | 2016-10-12 | 陈师颖 | Composite water treatment reagent and preparation method thereof |
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| CN1328970A (en) * | 2000-06-15 | 2002-01-02 | 中国科学院地球化学研究所 | Cleaning agent of aqueous aluminium iron polysilicate waste water and its production method |
| CN1907878A (en) * | 2006-08-10 | 2007-02-07 | 哈尔滨工程大学 | Method of preparation polymeric aluminium ferrum silicate flocculant |
| CN101298346A (en) * | 2008-07-01 | 2008-11-05 | 北京大学 | Polysilicate aluminum sulphate flocculant, preparation process and use thereof |
| CN101337727A (en) * | 2008-08-22 | 2009-01-07 | 内蒙古科技大学 | Method for preparing inorganic composite polysilicate aluminum ferric chloride flocculant |
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| CN102838197A (en) * | 2012-10-09 | 2012-12-26 | 重庆理工大学 | Method for preparing novel composite flocculant PSAFS (poly-silicate aluminum ferrous sulfate) |
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2014
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| CN101298346A (en) * | 2008-07-01 | 2008-11-05 | 北京大学 | Polysilicate aluminum sulphate flocculant, preparation process and use thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909440A (en) * | 2015-04-29 | 2015-09-16 | 南通大学 | New composite ethyl orthosilicate-polyaluminium chloride flocculant preparation method |
| CN105481072A (en) * | 2016-01-19 | 2016-04-13 | 昆明跃高工贸有限公司 | Preparation method of PSAF (polysilicate aluminum ferric) flocculant |
| CN105481072B (en) * | 2016-01-19 | 2017-11-07 | 昆明跃高工贸有限公司 | A kind of preparation method of polymeric aluminium ferrum silicate flocculant |
| CN106006900A (en) * | 2016-07-21 | 2016-10-12 | 陈师颖 | Composite water treatment reagent and preparation method thereof |
| CN106006900B (en) * | 2016-07-21 | 2018-09-04 | 陈师颖 | A kind of composite water treatment medicament and preparation method thereof |
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Application publication date: 20150401 |