CN103752268B - The filter core preparation method and application of heavy metal and arsenic, fluorine in absorption drinking water - Google Patents
The filter core preparation method and application of heavy metal and arsenic, fluorine in absorption drinking water Download PDFInfo
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- CN103752268B CN103752268B CN201410021223.6A CN201410021223A CN103752268B CN 103752268 B CN103752268 B CN 103752268B CN 201410021223 A CN201410021223 A CN 201410021223A CN 103752268 B CN103752268 B CN 103752268B
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Abstract
The invention discloses a kind of filter core preparation method and application of adsorbing heavy metal and arsenic in drinking water, fluorine, this preparation method comprises the steps: that choosing coconut husk granular activated carbon carries out pretreatment; By infusion process at activated carbon surface carried titanium dioxide; Active carbon drying after load is obtained adsorbing the filter core of heavy metal and arsenic in drinking water, fluorine ion; The invention also discloses the application of filter core, described filter core is used in filter plant and is used for adsorbing heavy metal and arsenic, fluorine ion in drinking water; By load TiO
2thus improve the ability of charcoal absorption contents of many kinds of heavy metal ion and arsenic, fluorine ion, reach national drinking water standard, be conducive to the drinking water safety ensureing resident; By normal temperature by TiO
2be carried on active carbon, significantly reduce production cost, method is easy, and equipment is simple, is easy to promote.
Description
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 equipment, as household drinker etc., also may be used 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 in the environment or be transferred, dilute, accumulate, and but can not degrade and thoroughly eliminate, threaten mankind's safe drinking water and health.Therefore, the harmful heavy metal how eliminated in water is extremely urgent environmental problem.
At present, the method for process 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 process of drinking water, because the content of these harmful ions is usually very low, application be in many ways restricted, as coagulant sedimentation is more suitable for 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 higher; Photocatalytic method rely on the equipment such as light source and also Kaolinite Preparation of Catalyst cost higher.The processing method of current drinking water is with absorption method, 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, such water yield also can reduce, 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 is as a kind of high-quality adsorbent, and have unique pore structure and surface functional group, its mechanical strength is high, has enough chemical stabilities, and can be acidproof, alkaline-resisting, heat-resisting.In water treatment procedure active carbon can not only deodorizing, taste removal, except colourity, can also remove the organic pollutions such as OCPs (organo-chlorine pesticide), ABS (sodium alkyl benzene sulfonate, synthetic detergent), current active carbon has become one of widely used water treatment absorbent.Although active carbon may be used for the common removal of each heavy metal species, adsorption capacity is unsatisfactory, need 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
2to many metal ions, there is stronger adsorption capacity; But TiO
2be used alone as powder, 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, ensure the drinking water safety of resident.
Through patent retrieval, utilize TiO at present
2heavy-metal ion removal and arsenic, fluorine, the isoionic patent of mercury have a lot, and after can being divided into first catalytic oxidation, absorption adsorbs two large classes with direct.The method of adsorbing after first catalytic oxidation needs TiO
2possess the conditions such as the illumination needed for stronger photo-catalysis capability and catalysis, compare directly absorption more complicated.As the document of application number 201010157248.0 and 201110402563.X, be all first prepare TiO by the high temperature of more than 400 degree
2, then utilize photoelectrocatalysis 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 need the high temperature more than 400 degree to prepare TiO
2.Document 201210054103.7 prepares TiO for hydro-thermal method
2.Document 201110328561.0 needs, at 100 DEG C ~ 300 DEG C, to dry 4h under vacuum condition.In a word, these methods all need higher synthesis condition and catalytic condition.
Method major part for directly absorption adopts powder directly to adsorb, and has certain difficulty like this when powder reclaims.Document 200910238505.0,201310013818.2 and 201110022984.X adopt precipitation method synthesis TiO
2powder is used 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 document that the method for directly absorption also has load to adsorb on carrier.As 200410099361.2 utilize the load of imvite high temperature sintering; 201110258143.9 be matrix with cross-linked chitosan, bond nano-TiO with crosslinking agent
2and nanometer Fe
3o
4powder load; 201110341090.7 hydro-thermal method load TiO
2on the activated carbon; 200910223338.2 by high-temperature roasting by TiO
2be carried on active carbon with lanthana.Cost can be made to raise by high temperature sintering in these methods, to be bonded by crosslinking agent and hydro-thermal method also can make operation become complicated.
This patent is by normal temperature load TiO
2on active carbon, significantly reduce production cost, method is easier, and achieves 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 anatase crystal, contribute to photocatalysis, but impact is little for absorption.Therefore this patent eliminates high-temperature burning process, and adsorption effect is still remarkable.
Summary of the invention:
The present invention is directed to first three level (PP cotton of Household water purification equipment general at present; granular activated carbon and Powdered Activated Carbon); to the not ideal problem of effect removing multiple harmful metal ion and arsenic, fluorine, mercury ion, modification is carried out to granular activated carbon wherein, load TiO
2make it possess the efficient ability removing multiple harmful metal ion and arsenic in drinking water, fluorine, mercury ion, and preparation process is simple, easy large-scale production, with low cost.
The invention provides a kind ofly adsorb heavy metal and arsenic in drinking water, the filter core preparation method of 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) the active carbon drying after load is obtained adsorbing the filter core of heavy metal and arsenic in drinking water, fluorine;
(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 DEG C of oven dry.
In above-mentioned steps (2) in activated carbon surface carried titanium dioxide method be:
A butyl titanate is slowly added the absolute ethyl alcohol and glacial acetic acid mixed liquor that are stirring by (), form A liquid; Absolute ethyl alcohol, glacial acetic acid and distilled water are mixed simultaneously, form B liquid; B liquid is slowly instilled A liquid, the mixed liquor that obtains continues stirring 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 coconut husk granular activated carbon good for pretreatment is soaked in the TiO after ageing by ()
2carry out load 30min in colloidal sol, 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 added or non-metal salt and butyl titanate is 0.1 ~ 3%.
The slaine added 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 drying of the active carbon in above-mentioned steps (3) after carried titanium dioxide is natural air drying under normal temperature condition.
The drying of the active carbon after above-mentioned carried titanium dioxide improves baking temperature or adds ventilation equipment can accelerate 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, is used in filter plant by described filter core and is used for adsorbing heavy metal and arsenic, fluorine ion in drinking water.
Beneficial effect of the present invention:
(1) by load TiO
2thus improve the ability of charcoal absorption contents of many kinds of heavy metal ion and arsenic, fluorine, mercury ion, reach national drinking water standard, be conducive to the drinking water safety ensureing resident;
(2) by normal temperature by TiO
2be carried on active carbon, significantly reduce 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 removing contents of many kinds of heavy metal ion and arsenic, fluorine ion experimental provision.
Wherein: 1. water circulating pump 2. tank 3. of intaking circulates self priming pump 4. flow speed control valve 5. modified activated carbon filter core 6. delivery port.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention will be further described:
Embodiment 1:
One, the preparation of filter core of heavy metal and arsenic in drinking water, mercury, fluorine ion is adsorbed: coconut husk granular activated carbon water boil is about 0.5h, then washes with water, 95 ~ 104.5 DEG C of oven dry, cool for subsequent use.Butyl titanate is slowly added the absolute ethyl alcohol stirred and glacial acetic acid mixed liquor, form A liquid; Absolute ethyl alcohol, glacial acetic acid and distilled water are mixed simultaneously, form B liquid; B liquid is slowly instilled A liquid, the mixed liquor that obtains continues stirring 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 active carbon that pretreatment is good is soaked in the TiO after ageing
2carry out load in colloidal sol and be about 30min, before load, the mass ratio of Butyl Phthalate and active carbon is 1:10.Be separated with remaining colloidal sol by active carbon after load, 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, reactor assembly as shown in Figure 2, and being made into volume by deionized water is 6L, and concentration is the As of 100 μ g/L
3+solution is poured into into water tank, solution ph is regulated to be 6.5 ~ 7.5, have two water circulating pumps to run in experimentation in tank makes solution mix always, by circulation self priming pump, water sample is passed into modified activated carbon filter core, a valve controlling water sample flow velocity is had, flow velocity 5min/L before entering filter core; Access the water sample by modified activated carbon filter core, detect.
Experimental result: after modified activated carbon filter core, As in 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:
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, As in 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, Hg in aqueous 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, F in 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, Cd in 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, Mo in aqueous solution
6+concentration is lower than national standard 70 μ g/L.
Embodiment 8:
The Cr of the present embodiment experimentation water inlet solution to be concentration be 250 μ g/L as different from Example 1
3+solution.
Experimental result: after modified activated carbon filter core, Cr in 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, Sd in 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, Pb in aqueous solution
2+concentration is lower than national standard 10 μ g/L.
Claims (6)
1. adsorb a filter core preparation method for heavy metal and arsenic in drinking water, fluorine, it is characterized in that comprising the steps:
(1) choose coconut husk granular activated carbon and carry out pretreatment; The pretreatment of coconut husk granular activated carbon is with water boil or ultrasonic or pickling, then washes with water, then 95 ~ 104.5 DEG C of oven dry;
(2) use infusion process at activated carbon surface carried titanium dioxide;
A butyl titanate is slowly added the absolute ethyl alcohol and glacial acetic acid mixed liquor that are stirring by (), form A liquid; Absolute ethyl alcohol, glacial acetic acid and distilled water are mixed simultaneously, form B liquid; B liquid is slowly instilled A liquid, the mixed liquor that obtains continues stirring 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 coconut husk granular activated carbon good for pretreatment is soaked in the TiO after ageing by ()
2carry out load 30min in colloidal sol, after load, active carbon is separated with remaining colloidal sol; Before load, the mass ratio of butyl titanate and active carbon is 1:10;
(3) the active carbon drying after load is obtained adsorbing the filter core of heavy metal and arsenic in drinking water, fluorine;
(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 (a), adds slaine or non-metal salt in B solution, regulates TiO
2absorption property, the mol ratio of the slaine added or non-metal salt and butyl titanate is 0.1 ~ 3%.
3. preparation method according to claim 2, is characterized in that: the slaine added 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.
4. preparation method according to claim 1, is characterized in that: the drying of the active carbon in above-mentioned steps (3) after carried titanium dioxide is natural air drying under normal temperature condition.
5. preparation method according to claim 4, is characterized in that: the drying of the active carbon after above-mentioned carried titanium dioxide, improves baking temperature or add ventilation equipment to be used for accelerating rate of drying.
6. the application of the filter core of heavy metal and arsenic, fluorine in the absorption drinking water prepared of preparation method described in claim 1, is characterized in that: be used in filter plant by described filter core and be used for adsorbing heavy metal and arsenic, fluorine ion in drinking water.
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