CN101298346B - Polysilicate aluminum sulphate flocculant, preparation process and use thereof - Google Patents

Polysilicate aluminum sulphate flocculant, preparation process and use thereof Download PDF

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CN101298346B
CN101298346B CN2008101159895A CN200810115989A CN101298346B CN 101298346 B CN101298346 B CN 101298346B CN 2008101159895 A CN2008101159895 A CN 2008101159895A CN 200810115989 A CN200810115989 A CN 200810115989A CN 101298346 B CN101298346 B CN 101298346B
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flocculant
aluminum sulphate
aluminum
pasc
polysilicate aluminum
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CN101298346A (en
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赵华章
彭建雄
孙娟娟
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Peking University
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Abstract

The invention relates to a poly-aluminum silicate chloride (PASC) flocculant, a production technique and an application thereof. The invention adopts the tetra ethyl ortho silicate (TEOS) as the silicon source, which is mixed with aluminum chloride solution and is gradually dripped with alkaline to obtain the PASC flocculant. The poly-aluminum silicate chloride (PASC) flocculant, the production technique and the application thereof have the advantages that the silicon and aluminum distribution in the PASC flocculant is more uniform, the molecular weight is bigger and the product has better reproduction quality reproduction quality; at the same time, the product has good turbidity removal and decoloring effect, and the content of the residual aluminum is low and is less affected by the PH value; also, the product is an efficient water treatment agent with wider optimal chemical dosing range. The invention can be widely used for the water purification and the turbidity removal, decoloration, deoiling and solid-liquid separation during the wastewater treatment.

Description

A kind of polysilicate aluminum sulphate flocculant, preparation technology and application thereof
Technical field
The present invention relates to the synthesis technical field of polymeric flocculant in the water treatment field, specifically, the present invention relates to a kind of polysilicate aluminum sulphate flocculant, preparation technology and application thereof.
Background technology
In water technology, coagulation process is one of the most general key technique.It is determining the operation condition of follow-up flow process, final outflow water quality and cost.The fine or not key of coagulation effect depends on flocculation agent, so the preparation of flocculation agent is in important status always.As s-generation flocculation agent, the flocculating effect that has of inorganic polymer flocculant (IPOs) is better than traditional flocculant (aluminium salt, molysite, silicic acid etc.), and simultaneously price is lower than the advantage of organic floculant, its research and be applied in the past few decades between develop rapidly.
Polysilicate aluminum sulphate flocculant be a class than the novel inorganic polymeric flocculant, it is the combination product that grows up on the basis of inorganic flocculating agents such as poly-silicic acid (being activated silicic acid) and aluminum chloride.Such flocculation agent has charge neutrality and adsorption bridging effect simultaneously, and flocculating effect is good, and handling low temperature and low turbidity water has special efficacy, low price, advantage such as the residual aluminum in water is low.
The preparation method of present polysilicate aluminum sulphate flocculant adds acid to make poly-silicic acid (activated silicic acid) in water glass, adding polymerization under the alkali condition with aluminum salt solution (or polymeric aluminum) then.As adopting the mixed polymeric aluminium-silica flocculation agent that gets of polymerize aluminum chloride and activated silicic acid among the patent CN1197038A; Among the patent CN1556047A with AlCl 36H 2O and poly-silicic acid are main raw material, adopt copolymerization method technology to make the polymeric aluminium-silica flocculation agent; Among the patent CN1400172A with inorganic aluminate and poly-silicic acid mixed polysilicate aluminum sulphate flocculant; Among the patent CN101186371A liquor alumini chloridi is mixed with poly-silicic acid, add under the alkali condition polymerization and make poly-silicon aluminum chloride flocculant.But this class preparation method forms the segmented copolymer of aluminium silicon or homopolymer separately easily, and the circulation ratio of product is bad, has brought certain degree of difficulty for the practical application of product.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, and a kind of novel polysilicate aluminum sulphate flocculant, preparation technology and application thereof are provided.
The present invention seeks to realize by following measure: polysilicate aluminum sulphate flocculant raw material of the present invention is that (molecular formula is Si (OC to tetraethoxy for Tetraethylorthosilicate, TEOS 2H 5) 4. claim tetraethoxysilane again) and liquor alumini chloridi, the total aluminium concentration of polysilicate aluminum sulphate flocculant is 0.05~0.25mol/L, Si/Al mol ratio 0.05~0.4, and basicity 0.5~2.5, the pH value is 3.0~4.0.
Reaction structure formula of the present invention is:
Figure S2008101159895D00021
TEOS hydrolyzable in water becomes silicic acid, then with aluminium salt hydrolysis product---and aluminium hydroxyl generation polycondensation generates the sial combination product.
Water in the reaction formula is from AlCl 3Water in water in the solution and the NaOH solution.Reaction back Al is a kind of polymeric form.
The preparation technology of polysilicate aluminum sulphate flocculant: with AlCl 3Solution and tetraethoxy mix, and adopting slowly, an alkaline process makes polysilicate aluminum sulphate flocculant.
Concrete preparation technology: it is quantitative to press Si/Al mol ratio 0.05~0.4 to there-necked flask, gets AlCl 3Solution and tetraethoxy mix, and stir fast under room temperature then, adopt constant flow pump to drip NaOH solution, NaOH mole number and AlCl 3Ratio be 0.5~2.5, to basicity B=0.5~2.5, gained solution left standstill question response fully after, promptly obtain polysilicate aluminum sulphate flocculant.
The application of polysilicate aluminum sulphate flocculant is used for turbidity removal, decolouring, de-oiling and the solid-liquid separation of water supply purification, wastewater treatment process.
The relative prior art of polysilicate aluminum sulphate flocculant of the present invention has following advantage:
The sial of 1 polysilicate aluminum sulphate flocculant is more evenly distributed, and molecular weight is bigger, the product favorable reproducibility.
2 turbidity removal good decolorizing effect, and residual aluminum content is low, and it is little influenced by pH, best dispensing a wider range.
Embodiment
Enumerate 2 embodiment and 4 application examples below, the present invention is further specified, but be not limited thereto.
Example 1:
Polysilicate aluminum sulphate flocculant, total aluminium concentration 0.07mol/L, the Si/Al mol ratio is 0.2, and basicity B is 2.5, and the pH value is 3.8.
The preparation method is as follows:
At room temperature, in there-necked flask, add the AlCl that 50mL concentration is 0.25mol/L in proportion 3The TEOS of solution and 0.58mL stirs under room temperature then fast, adopt constant flow pump slowly drip 125mL concentration be the NaOH solution of 0.25mol/L to aequum, NaOH mole number and AlCl 3Ratio be 2.5, drip off promptly reaction and finish, gained solution left standstill question response is complete, promptly obtains polysilicate aluminum sulphate flocculant after 24 hours.
Example 2:
Polysilicate aluminum sulphate flocculant, total aluminium concentration 0.2mol/L, the Si/Al mol ratio is 0.4, and basicity B is 2.0, and the pH value is 3.5.
The preparation method is as follows:
In there-necked flask,, quantitatively add the AlCl that 50mL concentration is 1.0mol/L respectively by predetermined Si/Al mol ratio 3The TEOS of solution and 4.61mL.Under room temperature, stir fast then, adopt constant flow pump slowly to drip the extremely predetermined B value of NaOH solution that 200mL concentration is 0.5mol/L, NaOH mole number and AlCl 3Ratio be 2.0, titration time is 3 hours, gained solution left standstill question response is complete, promptly obtains the product that total aluminium concentration is 0.2mol/L after 2 days.
1 of application example
This example is the coagulation evaluation experimental to turbidity water
The polysilicate aluminum sulphate flocculant product of above example 1 preparation is used for the coagulation turbidity removal processing of kaolin muddy water.Simultaneously be that the identical basicity that makes of silicon source and the poly-silicon aluminum chloride flocculant of Si/Al mol ratio contrast with activated silicic acid, raw water turbidity is 80NTU, the pH value is respectively 5.5,7.1,8.5.The results are shown in Table 1 for coagulating treatment.
(in Al, mol/L), polysilicate aluminum sulphate flocculant (example 1) is handled the coagulation turbidity removal effect of the residual turbidity (NTU) of back water to the different dosages of table 1
Figure S2008101159895D00031
As can be seen from Table 1, the prepared polysilicate aluminum sulphate flocculant of the present invention with compare with the poly-silicon aluminum chloride of activated silicic acid preparation, the prepared polysilicate aluminum sulphate flocculant of the present invention has better turbidity removal effect, and it is less to be subject to processing the pH influence of water.
2 of application example
This example is a residual aluminum Determination on content in the water
The polysilicate aluminum sulphate flocculant that above example 1 is made carries out coagulation experiment according to the method for one of application example under different pH values, the supernatant liquor of getting after the experiment is surveyed its residual aluminum content, the results are shown in table 2.
Residual aluminum content under the table 2 different treatment condition in the water
Figure S2008101159895D00032
Figure S2008101159895D00041
Annotate: *The aluminium dosage is 14 * 10 -5Mol/L, other are 70 * 10 -5Mol/L
As can be seen from Table 2, the residual aluminum content of the polysilicate aluminum sulphate flocculant that the present invention is prepared, being lower than with the activated silicic acid is the poly-silicon aluminum chloride that the silicon source prepares.
3 of application example
The coagulation turbidity removal that the polysilicate aluminum sulphate flocculant product of above example 2 preparations is used for the kaolin muddy water is handled, simultaneously and traditional aluminum salt flocculant---polymerize aluminum chloride (being called for short PAC, basicity 2.0) contrasts.Raw water turbidity is 90NTU, pH value 7.8.Result is listed in the table 3.
(in Al, mol/L), polysilicate aluminum sulphate flocculant (example 2) is handled the coagulation turbidity removal effect of the residual turbidity (NTU) of back water to the different dosages of table 3
Figure S2008101159895D00042
As can be seen from Table 3, the polysilicate aluminum sulphate flocculant of the inventive method preparation has the turbidity removal effect more excellent than polymerize aluminum chloride.
4 of application example
The coagulation decoloration that the polysilicate aluminum sulphate flocculant product of above example 2 preparations is used to contain the colored water of humic acid is handled, simultaneously and traditional aluminum salt flocculant---polymerize aluminum chloride (be called for short PAC, basicity is 2.0) contrasts.Former colority of water represents that with the 370nm light absorption value its value is 0.240.The pH value is 7.8.Result is listed in the table 4.
(in Al, mol/L), polysilicate aluminum sulphate flocculant (example 2) is handled the coagulate decoloring effect of the residue colourity of back water to the different dosages of table 4
Figure S2008101159895D00043
As can be seen from Table 4, the polysilicate aluminum sulphate flocculant of the inventive method preparation has the decolorizing effect more excellent than polymerize aluminum chloride.

Claims (2)

1. polysilicate aluminum sulphate flocculant, it is characterized in that: raw material is tetraethoxy TEOS and liquor alumini chloridi, and the total aluminium concentration of polysilicate aluminum sulphate flocculant is 0.2mol/L, and the Si/Al mol ratio is 0.4, and basicity is 2.0, the pH value is 3.5.
2. by the preparation technology of the described polysilicate aluminum sulphate flocculant of claim 1, it is characterized in that, press Si/Al mol ratio 0.4, quantitatively get liquor alumini chloridi and tetraethoxy respectively, mix the back and under room temperature, stir fast, adopt constant flow pump slowly to drip NaOH solution, NaOH and AlCl 3The ratio of mole number is 2.0, to basicity B=2.0, after gained solution left standstill question response is complete, promptly obtains the polysilicate aluminum sulphate flocculant that total aluminium concentration is 0.2mol/L.
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CN102068971B (en) * 2010-12-03 2013-06-19 哈尔滨工业大学 Preparation method of poly-aluminum silicate
CN104478051A (en) * 2014-12-10 2015-04-01 上海应用技术学院 Method for preparing poly-aluminum ferric silicate sulfate flocculating agent
CN114149065A (en) * 2021-12-27 2022-03-08 襄垣县万普净水材料有限公司 Novel water purifying agent production reaction curing flash evaporation process

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