CN103752268A - Preparation method of filter core for adsorbing heavy metal, arsenic and fluorine in drinking water and application thereof - Google Patents

Preparation method of filter core for adsorbing heavy metal, arsenic and fluorine in drinking water and application thereof Download PDF

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CN103752268A
CN103752268A CN201410021223.6A CN201410021223A CN103752268A CN 103752268 A CN103752268 A CN 103752268A CN 201410021223 A CN201410021223 A CN 201410021223A CN 103752268 A CN103752268 A CN 103752268A
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filter core
arsenic
drinking water
preparation
fluorine
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魏志钢
袁建珍
尤灿
李隋亮
汤丽贤
邹燕娣
潘湛昌
胡光辉
梁凯
陈耀祖
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Guangzhou Greenview Environmental Protection Equipment Co ltd
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Guangdong University of Technology
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Abstract

The invention discloses a preparation method of a filter core for adsorbing heavy metal, arsenic and fluorine in drinking water and application thereof. The preparation method comprises the following steps: selecting coconut shell granular activated carbon to carry out pretreatment; loading titanium dioxide on the surface of active carbon by using an impregnation method; drying the loaded active carbon to obtain a filter core for adsorbing heavy metal, arsenic and fluorine in drinking water. The invention also discloses application of the filter core. The filter core is applied to filter equipment to adsorb heavy metal, and arsenic and fluorine ions in the drinking water, the capacity of the active carbon for adsorbing a plurality of heavy metals and arsenic and fluorine ions is improved by loading TiO2, the national standard of the drinking water is achieved, guarantee of the safety of the drinking water for residents is facilitated, the production cost is obviously reduced by loading the TiO2 to the active carbon at normal temperature, and the method is simple and convenient, simple in equipment and easy to popularize.

Description

The filter core preparation method and application of heavy metal and arsenic, fluorine in absorption drinking water
Technical field
The invention belongs to water treatment field, be specifically related to a kind of filter core preparation method and application of adsorbing heavy metal and arsenic in drinking water, fluorine, this filter core is applied to various drinking water treatment equipments, as household drinker etc., and also can be for sewage disposal.
Background technology
Along with developing rapidly of industrial and agricultural production and urban modernization, environmental pollution is day by day serious, wherein heavy metal ion and arsenic, fluorine, mercury plasma can only change form or be transferred, dilute, accumulate in environment, but can not degrade and thoroughly eliminate, and are threatening mankind's safe drinking water and health.Therefore the harmful heavy metal of, how eliminating in water is extremely urgent environmental problem.
At present, the method for processing heavy metal has a lot, comprising: coagulant sedimentation, absorption method, oxidizing process, ion-exchange, membrane separation process, biological method, photo chemistry technology etc.But for the processing of drinking water, because the content of these harmful ions is conventionally very low, so much the application of methods is restricted, as coagulant sedimentation is more suitable in sewage disposal; Oxidation-reduction method must use continuously and some oxidants also exist pollution to water; Bioanalysis needs the long period just can take effect; Ion-exchange and membrane separation process cost are higher; The equipment such as photocatalytic method dependence light source and Kaolinite Preparation of Catalyst cost are higher.The processing method of drinking water is with absorption method at present, and counter-infiltration and milipore filter are main.Due to the small volume of heavy metal ion, if adopt counter-infiltration and milipore filter just to need aperture very little, water yield also can reduce like this, and water supply goes wrong, and cost also can improve simultaneously.Absorption method is simply effective, and cost is low, is applicable to heavy metal ion and arsenic, fluorine, the isoionic elimination of mercury.
Active carbon, as a kind of high-quality adsorbent, has unique pore structure and surface functional group, and its mechanical strength is high, has enough chemical stabilities, and can be acidproof, alkaline-resisting, heat-resisting.In water treatment procedure active carbon not only can deodorizing, taste removal, except colourity, can also remove the organic pollutions such as OCPs (organo-chlorine pesticide), ABS (sodium alkyl benzene sulfonate, synthetic detergent), active carbon has become one of widely used water treatment absorbent at present.Although active carbon can be for the common removal of various heavy metals, adsorption capacity is unsatisfactory, need be to activated carbon modified.In recent years, titanium dioxide (TiO 2) as novel catalyst and adsorbent, become a study hotspot of materialogy, environmental science; TiO 2many metal ions are had to stronger adsorption capacity; But TiO 2as powder, use separately, cost is higher, and is difficult to reclaim.Therefore based on above 2 points, TiO 2need carrier loaded.This patent utilizes active carbon (AC) load TiO 2form TiO 2/ AC adsorbent, Adsorption of Heavy Metal Ions and arsenic, fluorine, mercury plasma, guarantee resident's drinking water safety.
Through patent retrieval, utilize at present TiO 2heavy-metal ion removal and arsenic, fluorine, the isoionic patent of mercury have a lot, can be divided into after first catalytic oxidation absorption and direct absorption two large classes.The method of adsorbing after first catalytic oxidation needs TiO 2possess the required conditions such as illumination of stronger photo-catalysis capability and catalysis, compare direct absorption more complicated.As the document of application number 201010157248.0 and 201110402563.X, be all first by high temperature more than 400 degree, to prepare TiO 2, then utilize photoelectrocatalysis to process industry water and mud.Also have some patents just to mention and improve TiO 2preparation method improve its photocatalysis performance, as 200510049369.2,200610025568.4,200810034554.8,200910153373.1,201010017935.2,201010259771.4,201110004813.4,201110093927.0,201210270940.3,201210271973.X etc. are to prepare TiO by the high temperature more than 400 degree 2.Document 201210054103.7 is prepared TiO for hydro-thermal method 2.Document 201110328561.0 need to, at 100 ℃～300 ℃, be dried 4h under vacuum condition.In a word, these methods all need higher synthesis condition and catalytic condition.
The most of powder that adopts of method for direct absorption directly adsorbs, and has like this certain difficulty when powder reclaims.Document 200910238505.0,201310013818.2 and 201110022984.X adopt the synthetic TiO of the precipitation method 2powder is for absorption.Document 201110066392.8 utilizes hydro-thermal method to prepare powder, adsorbs.Document 201010500917.X needs calcination when synthetic powder, utilizes powder to adsorb.
For the method for direct absorption, also have and load on the document adsorbing on carrier.Utilize the load of imvite high temperature sintering as 200410099361.2; 201110258143.9 take cross-linked chitosan as matrix, with the bonding nano-TiO of crosslinking agent 2and nanometer Fe 3o 4powder load; 201110341090.7 hydro-thermal method load TiO 2on active carbon; 200910223338.2 by high-temperature roasting by TiO 2be carried on active carbon with lanthana.In these methods, by high temperature sintering, can make cost raise, by crosslinking agent, bonding and hydro-thermal method also can make operation become complicated.
This patent is by normal temperature load TiO 2on active carbon, significantly reduced production cost, method is easier, and has obtained good adsorption effect.Its principle is that the adsorption capacity of adsorbent depends on the quantity of adsorbent surface titanium ion, and does not depend on TiO 2crystal structure.High-temperature calcination can make TiO 2form Detitanium-ore-type crystal, contribute to photocatalysis, but impact is little for absorption.Therefore this patent has removed high-temperature calcination process, and adsorption effect is still remarkable.
Summary of the invention:
The present invention is directed to first three level (PP cotton of at present general Household water purification equipment; granular activated carbon and Powdered Activated Carbon); to removing the not ideal problem of effect of multiple harmful metal ion and arsenic, fluorine, mercury ion, granular activated carbon is wherein carried out to modification, load TiO 2make its ability that possesses multiple harmful metal ion and arsenic in efficient removal drinking water, fluorine, mercury ion, and preparation process is simple, easily large-scale production, with low cost.
The invention provides a kind of filter core preparation method of adsorbing heavy metal and arsenic in drinking water, fluorine comprises the steps:
(1) choose coconut husk granular activated carbon and carry out pretreatment;
(2) use infusion process at activated carbon surface carried titanium dioxide;
(3) by the dry filter core that obtains adsorbing heavy metal and arsenic in drinking water, fluorine of the active carbon after load;
(4) as required, repeat above-mentioned steps (2) and (3) and carry out repeatedly load.
In above-mentioned steps (1), the pretreatment of coconut husk granular activated carbon is with water boil or ultrasonic or pickling, then washes with water, then 95～104.5 ℃ of oven dry.
In above-mentioned steps (2), in activated carbon surface carried titanium dioxide method, be:
(a) butyl titanate is slowly added to absolute ethyl alcohol and the glacial acetic acid mixed liquor stirring, form A liquid; Absolute ethyl alcohol, glacial acetic acid and distilled water are mixed simultaneously, form B liquid; B liquid is slowly splashed into A liquid, and the mixed liquor that obtains continues to stir that 3 hours, ageing must be stablized after 12 hours, even, as clear as crystal TiO 2colloidal sol; The mol ratio of the butyl titanate in described A liquid, absolute ethyl alcohol, glacial acetic acid is 1:26:12; In B liquid, the mol ratio of absolute ethyl alcohol, glacial acetic acid, distilled water is 34:9:36;
(b) the good coconut husk granular activated carbon of pretreatment is soaked in to the TiO after ageing 2in colloidal sol, carry out load 30min, after load, active carbon is separated with remaining colloidal sol; Before load, the mass ratio of Butyl Phthalate and active carbon is 1:10.
In above-mentioned steps (a), in B solution, add slaine or non-metal salt, regulate TiO 2absorption property, the mol ratio of the slaine adding or non-metal salt and butyl titanate is 0.1～3%.
The slaine adding or non-metal salt are: ScCl 3, Sc (NO 3) 3, VCl 5, V (NO 3) 5, CrCl 3.6H 2o, Cr (NO 3) 3, MnCl 2.6H 2o, Mn (NO 3) 2.4H 2o, FeCl 36H 2o, Fe (NO 3) 3, CoCl 26H 2o, Co (NO 3) 2, NiCl 26H 2o, Ni (NO 3) 2, CuCl 22H 2o, Cu (NO 3) 2, ZnCl 2, Zn (NO 3) 2, YCl 3, Y (NO 3) 3, SmCl 3, Sm (NO 3) 3, EuCl 3, Eu (NO 3) 3, TbCl 3, Tb (NO 3) 3, CeCl 3, (NH4) 2ce (NO 3) 6, LuCl 3, Lu (NO 3) 3, YbCl 3, Yb (NO 3) 3, DyCl 3, Dy (NO 3) 3, NdCl 3, Nd (NO 3) 3, LaCl 3, La (NO 3) 3, PrCl 3, Pr (NO 3) 3, HoCl 3, Ho (NO 3) 3, GdCl 3, Gd (NO 3) 3, TmCl 3, Tm (NO 3) 3, ErCl 3, Er (NO 3) 3, urea (CO (NH 2) 2) or NH 4nO 3.
The dry of active carbon in above-mentioned steps (3) after carried titanium dioxide is natural air drying under normal temperature condition.
The dry raising baking temperature of the active carbon after above-mentioned carried titanium dioxide or interpolation ventilation equipment can be accelerated rate of drying.
The present invention also provides the application of the filter core of heavy metal and arsenic in a kind of described absorption drinking water, fluorine, and described filter core is used in filter plant for adsorbing drinking water heavy metal and arsenic, fluorine ion.
Beneficial effect of the present invention:
(1) by load TiO 2thereby the ability that improves charcoal absorption contents of many kinds of heavy metal ion and arsenic, fluorine, mercury ion, reaches national drinking water standard, is conducive to ensure resident's drinking water safety;
(2) by normal temperature by TiO 2be carried on active carbon, significantly reduced production cost, method is easy, and equipment is simple, is easy to promote.
Accompanying drawing explanation
Fig. 1 is load TiO 2the scanning electron microscope (SEM) photograph of absorbent charcoal material.
Fig. 2 is load TiO 2active carbon filter core remove the experimental provision of contents of many kinds of heavy metal ion and arsenic, fluorine ion.
Wherein: 1. water circulating pump 2. water inlet tank 3. circulation self priming pump 4. flow speed control valve 5. modified activated carbon filter core 6. delivery ports.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention will be further described:
Embodiment 1:
One, the preparation of the filter core of heavy metal and arsenic, mercury, fluorine ion in absorption drinking water: by the about 0.5h of coconut husk granular activated carbon water boil, then wash with water, 95～104.5 ℃ of oven dry, cooling standby.Butyl titanate is slowly added to absolute ethyl alcohol and the glacial acetic acid mixed liquor stirring, form A liquid; Absolute ethyl alcohol, glacial acetic acid and distilled water are mixed simultaneously, form B liquid; B liquid is slowly splashed into A liquid, and the mixed liquor that obtains continues to stir that 3 hours, ageing must be stablized after 12 hours, even, as clear as crystal TiO 2colloidal sol; The mol ratio of the butyl titanate in described A liquid, absolute ethyl alcohol, glacial acetic acid is 1:26:12; In B liquid, the mol ratio of absolute ethyl alcohol, glacial acetic acid, distilled water is 34:9:36; The good active carbon of pretreatment is soaked in to the TiO after ageing 2in colloidal sol, carry out the about 30min of load, before load, the mass ratio of Butyl Phthalate and active carbon is 1:10.Active carbon after load is separated with remaining colloidal sol, and the active carbon after carried titanium dioxide is natural air drying under normal temperature condition.Repeated boad process, carries out load three times altogether, obtains filter core.
Two, as shown in Figure 2, by deionized water, be made into volume is 6L to reactor assembly, and concentration is the As of 100 μ g/L 3+solution is poured into into water tank, regulator solution pH value is 6.5～7.5, in tank, there is the operation always in experimentation of two water circulating pumps that solution is mixed, by circulation self priming pump, water sample is passed into modified activated carbon filter core, before entering filter core, there is a valve of controlling water sample flow velocity, flow velocity 5min/L; Access by the water sample of modified activated carbon filter core, detect.
Experimental result: after modified activated carbon filter core, go out As in the aqueous solution 3+concentration is lower than national standard 10 μ g/L.
Embodiment 2:
The present embodiment as different from Example 1 in experimentation B solution add salt, water inlet solution is the As of concentration 400 μ g/L 3+solution.Add the molecular formula of slaine or non-metal salt, add the mol ratio of slaine or non-metal salt and butyl titanate, As in water outlet 3+concentration (μ g/L) as following table:
Figure BDA0000457830700000051
Figure BDA0000457830700000061
Embodiment 3:
The present embodiment as different from Example 1 experimentation water inlet solution is the As of concentration 100 μ g/L 5+solution.
Experimental result: after modified activated carbon filter core, go out As in the aqueous solution 5+concentration is lower than national standard 10 μ g/L.
Embodiment 4:
The present embodiment as different from Example 1 experimentation water inlet solution is the Hg of concentration 5 μ g/L 2+solution.
Experimental result: after modified activated carbon filter core, water outlet Hg solution 2+concentration is lower than national standard 1 μ g/L.
Embodiment 5:
The present embodiment as different from Example 1 experimentation water inlet solution is the F of concentration 3000 μ g/L -solution.
Experimental result: after modified activated carbon filter core, go out F in the aqueous solution -concentration is lower than national standard 1000 μ g/L.
Embodiment 6:
The present embodiment as different from Example 1 experimentation water inlet solution is the Cd of concentration 10 μ g/L 2+solution.
Experimental result: after modified activated carbon filter core, go out Cd in the aqueous solution 2+concentration is lower than national standard 5 μ g/L.
Embodiment 7:
The present embodiment as different from Example 1 experimentation water inlet solution is the Mo of concentration 700 μ g/L 6+solution.
Experimental result: after modified activated carbon filter core, go out Mo in the aqueous solution 6+concentration is lower than national standard 70 μ g/L.
Embodiment 8:
The present embodiment as different from Example 1 experimentation water inlet solution is that concentration is the Cr of 250 μ g/L 3+solution.
Experimental result: after modified activated carbon filter core, go out Cr in the aqueous solution 3+concentration is lower than national standard 50 μ g/L.
Embodiment 9:
The present embodiment as different from Example 1 experimentation water inlet solution is the Sd of concentration 50 μ g/L 3+solution.
Experimental result: after modified activated carbon filter core, go out Sd in the aqueous solution 3+concentration is lower than national standard 5 μ g/L.
Embodiment 10:
The present embodiment as different from Example 1 experimentation water inlet solution is the Pb of concentration 100 μ g/L 2+solution.
Experimental result: after modified activated carbon filter core, go out Pb in the aqueous solution 2+concentration is lower than national standard 10 μ g/L.

Claims (8)

1. a filter core preparation method of adsorbing heavy metal and arsenic in drinking water, fluorine, is characterized in that comprising the steps:
(1) choose coconut husk granular activated carbon and carry out pretreatment;
(2) use infusion process at activated carbon surface carried titanium dioxide;
(3) by the dry filter core that obtains adsorbing heavy metal and arsenic in drinking water, fluorine of the active carbon after load;
(4) as required, repeat above-mentioned steps (2) and (3) and carry out repeatedly load.
2. preparation method according to claim 1, is characterized in that: in above-mentioned steps (1), the pretreatment of coconut husk granular activated carbon is with water boil or ultrasonic or pickling, then washes with water, then 95～104.5 ℃ of oven dry.
3. preparation method according to claim 1, is characterized in that: in above-mentioned steps (2), in activated carbon surface carried titanium dioxide method, be:
(a) butyl titanate is slowly added to absolute ethyl alcohol and the glacial acetic acid mixed liquor stirring, form A liquid; Absolute ethyl alcohol, glacial acetic acid and distilled water are mixed simultaneously, form B liquid; B liquid is slowly splashed into A liquid, and the mixed liquor that obtains continues to stir that 3 hours, ageing must be stablized after 12 hours, even, as clear as crystal TiO 2colloidal sol; The mol ratio of the butyl titanate in described A liquid, absolute ethyl alcohol, glacial acetic acid is 1:26:12; In B liquid, the mol ratio of absolute ethyl alcohol, glacial acetic acid, distilled water is 34:9:36;
(b) the good coconut husk granular activated carbon of pretreatment is soaked in to the TiO after ageing 2in colloidal sol, carry out load 30min, after load, active carbon is separated with remaining colloidal sol; Before load, the mass ratio of Butyl Phthalate and active carbon is 1:10.
4. preparation method according to claim 3, is characterized in that: in above-mentioned steps (a), add slaine or non-metal salt in B solution, regulate TiO 2absorption property, the mol ratio of the slaine adding or non-metal salt and butyl titanate is 0.1～3%.
5. preparation method according to claim 4, is characterized in that: the slaine adding or non-metal salt are: ScCl 3, Sc (NO 3) 3, VCl 5, V (NO 3) 5, CrCl 3.6H 2o, Cr (NO 3) 3, MnCl 2.6H 2o, Mn (NO 3) 2.4H 2o, FeCl 36H 2o, Fe (NO 3) 3, CoCl 26H 2o, Co (NO 3) 2, NiCl 26H 2o, Ni (NO 3) 2, CuCl 22H 2o, Cu (NO 3) 2, ZnCl 2, Zn (NO 3) 2, YCl 3, Y (NO 3) 3, SmCl 3, Sm (NO 3) 3, EuCl 3, Eu (NO 3) 3, TbCl 3, Tb (NO 3) 3, CeCl 3, (NH4) 2ce (NO 3) 6, LuCl 3, Lu (NO 3) 3, YbCl 3, Yb (NO 3) 3, DyCl 3, Dy (NO 3) 3, NdCl 3, Nd (NO 3) 3, LaCl 3, La (NO 3) 3, PrCl 3, Pr (NO 3) 3, HoCl 3, Ho (NO 3) 3, GdCl 3, Gd (NO 3) 3, TmCl 3, Tm (NO 3) 3, ErCl 3, Er (NO 3) 3, urea (CO (NH 2) 2) or NH 4nO 3.
6. preparation method according to claim 1, is characterized in that: the dry of active carbon in above-mentioned steps (3) after carried titanium dioxide is natural air drying under normal temperature condition.
7. preparation method according to claim 6, is characterized in that: the dry raising baking temperature of the active carbon after above-mentioned carried titanium dioxide or interpolation ventilation equipment can be accelerated rate of drying.
8. an application for the filter core of heavy metal and arsenic, fluorine in absorption drinking water claimed in claim 1, is characterized in that: described filter core is used in filter plant for adsorbing drinking water heavy metal and arsenic, fluorine ion.
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