CN109126734A - A kind of high efficiency, low cost adsorbent and preparation method for heavy metal containing wastewater treatment - Google Patents

A kind of high efficiency, low cost adsorbent and preparation method for heavy metal containing wastewater treatment Download PDF

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CN109126734A
CN109126734A CN201811185396.6A CN201811185396A CN109126734A CN 109126734 A CN109126734 A CN 109126734A CN 201811185396 A CN201811185396 A CN 201811185396A CN 109126734 A CN109126734 A CN 109126734A
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powder
weight
parts
heavy metal
low cost
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蒋涛
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Chengdu Qiqi Decimal Technology Co Ltd
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Chengdu Qiqi Decimal Technology Co Ltd
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

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Abstract

The present invention provides a kind of high efficiency, low cost adsorbents and preparation method for heavy metal containing wastewater treatment.Waste ceramic powder is made pottery charcoal mixed-powder with charcoal powder, furfural powder and is modified using eight hydration zirconium oxychlorides by this method, shuck is pulverized and is modified using potassium permanganate, then modified zirconia pottery charcoal mixed-powder, modified shuck powder, thickener, deionized water mixed and is granulated, be sintered, the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment is made.It is compared with the traditional method, adsorbent prepared by the present invention, using waste ceramic, charcoal powder, furfural powder and shuck as primary raw material, turn waste into wealth, it is at low cost, and pass through the modified adsorption capacity improved to heavy metal ion, and adsorbent is graininess, can realize recycling utilization by desorption.

Description

A kind of high efficiency, low cost adsorbent and preparation method for heavy metal containing wastewater treatment
Technical field
The invention belongs to the technical fields of wastewater treatment, provide a kind of high efficiency, low cost for heavy metal containing wastewater treatment Adsorbent and preparation method.
Background technique
Heavy metal wastewater thereby is mainly derived from mining, machining, non-ferrous metal metallurgy, old and useless battery garbage disposal, And the waste water of the production processes such as pesticide, medicine, paint, pigment discharge.After heavy metal enters water body, has on food chain and put Big effect can put aside to get up to cause slow poisoning, be detrimental to health in certain organs of human body.Heavy metal pollution of water body is As China and in the world one of the environmental problem of most serious, to the improvement of heavy metal wastewater thereby by domestic and international researcher Pay much attention to.
Can be decomposed destruction different from organic matter, heavy metal can only shift its there are position and change they physics and Chemical state.Currently used process for treating heavy-metal waste water mainly includes chemical precipitation method, reduction method, absorption method, UF membrane Method, Coagulation Method, ion-exchange, electrochemical process etc., wherein Heavymetal Wastewater Treatment by Adsorption have efficiently, it is economical, easy, Good selective, therefore the extensive concern by environmental protection sector.
Heavy metal wastewater thereby absorption method is the method that waste water is handled using porous solid adsorbent.According to adsorbent and suction The difference of active force property when adsorbing between attached matter, absorption can be divided into 3 classes: physical absorption is (by intermolecular force The absorption of generation), chemisorption (being adsorbed as caused by chemical bond force) and exchange adsorption (ion of solute due to electrostatic attraction and It is gathered in the electrification point of adsorbent surface above and displaces other ions being originally fixed on these electrification points).Heavy metal is useless The research of water treatment absorbent has become research hotspot project in recent years.
Chinese invention patent application number 201710531162.1 discloses a kind of heavy metal absorbent.Heavy metal species absorption Agent is made of following raw material according to parts by weight: charcoal, artificial zeolite, sodium bicarbonate, alkali face, molecular sieve, cocoanut shell, graphite Alkene and plant extracts.Plant extracts is by Qiu Guo indian rorippa herb, dayflower, calamus, Bermuda grass according to parts by weight than 1:0.6: 0.5:0.3 is formulated.The defect of the invention is that the absorption property of gained heavy metal wastewater thereby adsorbent is lower, water treatment effect It is undesirable.
Chinese invention patent application number 201810259153.6 disclose a kind of hemicellulose group high-efficiency environment friendly heavy metal from The preparation method of sub- adsorbent, this method is using plant as raw material, by the microwave-assisted alkalinity extraction hemicellulose of plant material, Hemicellulose epoxidation is crosslinked with diethylenetriamine or polyethylene polyamine again, then generates a large amount of branches with triethylamine is quaternary ammoniated, Crude product expands rapidly bulk multi-hole, and finally by crude product, grafted propylene is sour under ultrasound-enhanced effect, strengthens various heavy Ionic adsorption performance.But the preparation cost of adsorbent for heavy metal made from the invention is higher, and economy is bad.
In conclusion usually there is at high cost, adsorption effect for the heavy metal absorbent of wastewater treatment in the prior art The disadvantage of difference, therefore a kind of efficiently heavy metal containing wastewater treatment adsorbent of low cost is developed, it has great significance.
Summary of the invention
As it can be seen that usually having for the heavy metal absorbent of wastewater treatment in the prior art, at high cost, adsorption effect is poor Disadvantage.In response to this, the present invention proposes a kind of for the high efficiency, low cost adsorbent of heavy metal containing wastewater treatment and preparation side Method turns waste into wealth using waste ceramic, charcoal powder, furfural powder and shuck as primary raw material, at low cost, and is mentioned by modification The high adsorption capacity to heavy metal ion, and adsorbent is graininess, can pass through desorption and realize recycling utilization.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment, the high efficiency, low cost adsorbent system It is standby that specific step is as follows:
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and 22 ~ 26h of oscillation treatment in 20 DEG C of shaken cultivation casees is then centrifuged for separating, will sink Starch is added in sodium hydroxide solution, continues 15 ~ 20h of oscillation treatment in 20 DEG C of shaken cultivation casees, is centrifugated, dry, system Obtain modified zirconia pottery charcoal mixed-powder；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 1.5 ~ 2%, after mixing evenly 25 ~ 30h is stood, refilters, wash, dry, modified shuck powder is made；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment.
Preferably, in step (1) the pottery charcoal mixed-powder, 68 ~ 84 parts by weight of waste ceramic powder, 10 ~ 20 weight of charcoal powder Measure part, 6 ~ 12 parts by weight of furfural powder.
Preferably, the parts by weight of step (2) each raw material are pottery 20 ~ 30 parts by weight of charcoal mixed-powder, ethyl alcohol and amino 30 ~ 40 parts by weight of mixed aqueous solution of sulfonic acid, eight hydration 10 ~ 15 parts by weight of zirconium oxychloride, 15 ~ 40 weight of sodium hydroxide solution Part.
Preferably, in the mixed aqueous solution of step (2) ethyl alcohol and sulfamic acid, 20 ~ 30 parts by weight of ethyl alcohol, amino sulphur Sour 5 ~ 10 parts by weight, 60 ~ 75 parts by weight of water；The mass concentration of the sodium hydroxide solution is 2 ~ 4%.
Preferably, step (3) shuck is chestnut shell, walnut shell, green shell, bar denier wood shell, pine nut shell, almond One or more of shell composition.
Preferably, the parts by weight of step (3) each raw material are, 2 ~ 10 parts by weight of shuck powder, liquor potassic permanganate 90 ~ 98 parts by weight.
Preferably, step (4) thickener is one of diatomite, Silica hydrogel, attapulgite soil, sodium bentonite Or several compositions.
Preferably, step (4) modified zirconia pottery 30 ~ 40 parts by weight of charcoal mixed-powder, modified 10 ~ 20 weight of shuck powder Part, 30 ~ 56 parts by weight of deionized water, 4 ~ 10 parts by weight of thickener.
Preferably, the temperature of step (4) described high temperature sintering is 200 ~ 280 DEG C, and the time is 2 ~ 3h.
The present invention also provides a kind of above-mentioned preparation method be prepared it is a kind of for the efficient of heavy metal containing wastewater treatment Low Cost Sorbents.The high efficiency, low cost adsorbent is mixed by the way that pottery charcoal is made with charcoal powder, furfural powder in waste ceramic powder It closes powder and is modified using eight hydration zirconium oxychlorides, shuck is pulverized and is modified using potassium permanganate, so Modified zirconia pottery charcoal mixed-powder, modified shuck powder, thickener, deionized water are mixed afterwards and are granulated, is sintered and is made.
It is and existing the present invention provides a kind of high efficiency, low cost adsorbent and preparation method for heavy metal containing wastewater treatment Technology is compared, and the feature and excellent effect protruded is:
1. preparation method of the invention turns waste into wealth using waste ceramic, charcoal powder, furfural powder and shuck as primary raw material, bright The aobvious cost for reducing heavy metal absorbent.
2. preparation method of the invention, pottery charcoal mixed-powder is modified with eight hydration zirconium oxychlorides, on the one hand, zirconium with Ion exchange occurs for the ion in pottery carbon powder, so that the porous structure surface of pottery carbon powder is become coarse, specific surface area increases, separately On the one hand, the hydroxyl ion and hydrone that eight hydration zirconium oxychlorides have may participate in ligand substituting, increase pottery charcoal mixed-powder and inhale The active site of attached heavy-metal ion removal improves adsorption effect.
3. preparation method of the invention, is modified shuck powder with potassium permanganate, not only make the surface of shuck powder Become coarse by opposed flattened, specific surface area dramatically increases, and opens simultaneously more multi-pore channel and hole holds increase, and make powder surface The feature of the groups such as C=O, C-O-C, C-O, O-H is shown more obviously, provides more active sites for heavy metal adsorption, To improve adsorption effect.
4. adsorbent is made graininess, is easily separated from water, and inorganic acid solution can be used by preparation method of the invention Desorption processing is carried out, realizes recycling utilization.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；Pottery In charcoal mixed-powder, 75 parts by weight of waste ceramic powder, 16 parts by weight of charcoal powder, 9 parts by weight of furfural powder；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and the oscillation treatment 25h in 20 DEG C of shaken cultivation casees is then centrifuged for separating, by sediment It is added in sodium hydroxide solution, continues the oscillation treatment 17h in 20 DEG C of shaken cultivation casees, be centrifugated, it is dry, modified zirconia is made Pottery charcoal mixed-powder；In the mixed aqueous solution of ethyl alcohol and sulfamic acid, 24 parts by weight of ethyl alcohol, 7 parts by weight of sulfamic acid, 69 weight of water Measure part；The mass concentration of sodium hydroxide solution is 3%；The parts by weight of each raw material are, pottery 26 parts by weight of charcoal mixed-powder, ethyl alcohol with 36 parts by weight of mixed aqueous solution of sulfamic acid, eight hydration 13 parts by weight of zirconium oxychloride, 25 parts by weight of sodium hydroxide solution；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 1.7%, it is quiet after mixing evenly 27h is set, refilters, wash, dry, modified shuck powder is made；Shuck is chestnut shell；The parts by weight of each raw material are nut 5 parts by weight of shell powder, 95 parts by weight of liquor potassic permanganate；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment；Thickener is diatomite；The temperature of high temperature sintering is 250 DEG C, when Between be 2.5h；Modified zirconia pottery 34 parts by weight of charcoal mixed-powder, 45 parts by weight of deionized water, increase modified 14 parts by weight of shuck powder Thick dose of 7 parts by weight.
Embodiment 2
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；Pottery In charcoal mixed-powder, 80 parts by weight of waste ceramic powder, 12 parts by weight of charcoal powder, 8 parts by weight of furfural powder；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and the oscillation treatment 23h in 20 DEG C of shaken cultivation casees is then centrifuged for separating, by sediment It is added in sodium hydroxide solution, continues the oscillation treatment 16h in 20 DEG C of shaken cultivation casees, be centrifugated, it is dry, modified zirconia is made Pottery charcoal mixed-powder；In the mixed aqueous solution of ethyl alcohol and sulfamic acid, 22 parts by weight of ethyl alcohol, 6 parts by weight of sulfamic acid, 72 weight of water Measure part；The mass concentration of sodium hydroxide solution is 2.5%；The parts by weight of each raw material are make pottery 23 parts by weight of charcoal mixed-powder, ethyl alcohol 33 parts by weight of mixed aqueous solution, eight hydration 11 parts by weight of zirconium oxychloride, 33 parts by weight of sodium hydroxide solution with sulfamic acid；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 1.6%, it is quiet after mixing evenly 29h is set, refilters, wash, dry, modified shuck powder is made；Shuck is walnut shell；The parts by weight of each raw material are nut 5 parts by weight of shell powder, 95 parts by weight of liquor potassic permanganate；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment；Thickener is Silica hydrogel；The temperature of high temperature sintering is 220 DEG C, when Between be 3h；Modified zirconia pottery 33 parts by weight of charcoal mixed-powder, modified 12 parts by weight of shuck powder, 48 parts by weight of deionized water, thickening 6 parts by weight of agent.
Embodiment 3
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；Pottery In charcoal mixed-powder, 73 parts by weight of waste ceramic powder, 17 parts by weight of charcoal powder, 10 parts by weight of furfural powder；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and the oscillation treatment 25h in 20 DEG C of shaken cultivation casees is then centrifuged for separating, by sediment It is added in sodium hydroxide solution, continues the oscillation treatment 19h in 20 DEG C of shaken cultivation casees, be centrifugated, it is dry, modified zirconia is made Pottery charcoal mixed-powder；In the mixed aqueous solution of ethyl alcohol and sulfamic acid, 27 parts by weight of ethyl alcohol, 8 parts by weight of sulfamic acid, 65 weight of water Measure part；The mass concentration of sodium hydroxide solution is 3.5%；The parts by weight of each raw material are make pottery 27 parts by weight of charcoal mixed-powder, ethyl alcohol 37 parts by weight of mixed aqueous solution, eight hydration 14 parts by weight of zirconium oxychloride, 22 parts by weight of sodium hydroxide solution with sulfamic acid；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 1.9%, it is quiet after mixing evenly 26h is set, refilters, wash, dry, modified shuck powder is made；Shuck is green shell；The parts by weight of each raw material are, hard 8 parts by weight of shell powder, 92 parts by weight of liquor potassic permanganate；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment；Thickener is attapulgite soil；The temperature of high temperature sintering is 270 DEG C, time 2h；Modified zirconia make pottery 37 parts by weight of charcoal mixed-powder, modified 17 parts by weight of shuck powder, 38 parts by weight of deionized water, 8 parts by weight of thickener.
Embodiment 4
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；Pottery In charcoal mixed-powder, 84 parts by weight of waste ceramic powder, 10 parts by weight of charcoal powder, 6 parts by weight of furfural powder；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and the oscillation treatment 22h in 20 DEG C of shaken cultivation casees is then centrifuged for separating, by sediment It is added in sodium hydroxide solution, continues the oscillation treatment 15h in 20 DEG C of shaken cultivation casees, be centrifugated, it is dry, modified zirconia is made Pottery charcoal mixed-powder；In the mixed aqueous solution of ethyl alcohol and sulfamic acid, 20 parts by weight of ethyl alcohol, 5 parts by weight of sulfamic acid, 75 weight of water Measure part；The mass concentration of sodium hydroxide solution is 2%；The parts by weight of each raw material are, pottery 20 parts by weight of charcoal mixed-powder, ethyl alcohol with 30 parts by weight of mixed aqueous solution of sulfamic acid, eight hydration 10 parts by weight of zirconium oxychloride, 40 parts by weight of sodium hydroxide solution；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 1.5%, it is quiet after mixing evenly 25h is set, refilters, wash, dry, modified shuck powder is made；Shuck is bar denier wood shell；The parts by weight of each raw material are, hard 2 parts by weight of shell powder, 98 parts by weight of liquor potassic permanganate；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment；Thickener is sodium bentonite；The temperature of high temperature sintering is 200 DEG C, time 3h；Modified zirconia make pottery 30 parts by weight of charcoal mixed-powder, modified 10 parts by weight of shuck powder, 56 parts by weight of deionized water, 4 parts by weight of thickener.
Embodiment 5
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；Pottery In charcoal mixed-powder, 68 parts by weight of waste ceramic powder, 20 parts by weight of charcoal powder, 12 parts by weight of furfural powder；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and the oscillation treatment 26h in 20 DEG C of shaken cultivation casees is then centrifuged for separating, by sediment It is added in sodium hydroxide solution, continues the oscillation treatment 20h in 20 DEG C of shaken cultivation casees, be centrifugated, it is dry, modified zirconia is made Pottery charcoal mixed-powder；In the mixed aqueous solution of ethyl alcohol and sulfamic acid, 30 parts by weight of ethyl alcohol, 10 parts by weight of sulfamic acid, water 60 Parts by weight；The mass concentration of sodium hydroxide solution is 4%；The parts by weight of each raw material are make pottery 30 parts by weight of charcoal mixed-powder, ethyl alcohol 40 parts by weight of mixed aqueous solution, eight hydration 15 parts by weight of zirconium oxychloride, 15 parts by weight of sodium hydroxide solution with sulfamic acid；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 2%, stands after mixing evenly 30h is refiltered, washs, is dried, and modified shuck powder is made；Shuck is pine nut shell；The parts by weight of each raw material are shuck 10 parts by weight of powder, 90 parts by weight of liquor potassic permanganate；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment；Thickener is diatomite；The temperature of high temperature sintering is 280 DEG C, when Between be 2h；Modified zirconia pottery 40 parts by weight of charcoal mixed-powder, modified 20 parts by weight of shuck powder, 30 parts by weight of deionized water, thickening 10 parts by weight of agent.
Embodiment 6
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；Pottery In charcoal mixed-powder, 76 parts by weight of waste ceramic powder, 15 parts by weight of charcoal powder, 9 parts by weight of furfural powder；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and oscillation treatment for 24 hours, is then centrifuged for separating in 20 DEG C of shaken cultivation casees, by sediment It is added in sodium hydroxide solution, continues the oscillation treatment 18h in 20 DEG C of shaken cultivation casees, be centrifugated, it is dry, modified zirconia is made Pottery charcoal mixed-powder；In the mixed aqueous solution of ethyl alcohol and sulfamic acid, 25 parts by weight of ethyl alcohol, 8 parts by weight of sulfamic acid, 67 weight of water Measure part；The mass concentration of sodium hydroxide solution is 3%；The parts by weight of each raw material are, pottery 25 parts by weight of charcoal mixed-powder, ethyl alcohol with 35 parts by weight of mixed aqueous solution of sulfamic acid, eight hydration 12 parts by weight of zirconium oxychloride, 28 parts by weight of sodium hydroxide solution；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 1.8%, it is quiet after mixing evenly 28h is set, refilters, wash, dry, modified shuck powder is made；Shuck is Pericarppium Armeniacae Amarum；The parts by weight of each raw material are nut 6 parts by weight of shell powder, 94 parts by weight of liquor potassic permanganate；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment；Thickener is sodium bentonite；The temperature of high temperature sintering is 240 DEG C, time 2.5h；Modified zirconia pottery 35 parts by weight of charcoal mixed-powder, modified 15 parts by weight of shuck powder, 43 weight of deionized water Part, 7 parts by weight of thickener.
Comparative example 1
In preparation process, pottery charcoal mixed-powder is not modified using eight hydration zirconium oxychlorides, other preparation conditions and implementation Example 6 is consistent.
Comparative example 2
In preparation process, shuck powder is not modified using potassium permanganate, other preparation conditions and embodiment 6 are consistent.
Performance test:
Heavy metal ion static state maximal absorptive capacity and time of equilibrium adsorption: it takes a certain amount of containing Pb2+、Cu2+And Cd2+Heavy metal it is useless Water is added in beaker, and adsorbent produced by the present invention, pH value 7 is then added, and magnetic agitation rotating speed 120r/min is used Inductively coupled plasma optical emission spectrometer tests the amount of heavy metal ion, after repeating adsorption saturation, records adsorption saturation time, Measure and calculate the maximal absorptive capacity of heavy metal ion.
The data obtained is as shown in table 1.
Table 1:

Claims (10)

1. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment, which is characterized in that described efficient Specific step is as follows for Low Cost Sorbents preparation:
(1) it by discarded potsherd grind into powder, is uniformly mixed with charcoal powder, furfural powder, pottery charcoal mixed-powder is made；
(2) step (1) pottery charcoal mixed-powder obtained is added in the mixed aqueous solution of ethyl alcohol and sulfamic acid, adds eight water Zirconium oxychloride is closed, dispersion obtains suspension, and 22 ~ 26h of oscillation treatment in 20 DEG C of shaken cultivation casees is then centrifuged for separating, will sink Starch is added in sodium hydroxide solution, continues 15 ~ 20h of oscillation treatment in 20 DEG C of shaken cultivation casees, is centrifugated, dry, system Obtain modified zirconia pottery charcoal mixed-powder；
(3) it by shuck grind into powder, is then added in the liquor potassic permanganate that mass concentration is 1.5 ~ 2%, after mixing evenly 25 ~ 30h is stood, refilters, wash, dry, modified shuck powder is made；
(4) by modified shuck powder and deionized water made from the pottery of modified zirconia made from step (2) charcoal mixed-powder, step (3) Mixing, and is added thickener, is uniformly mixing to obtain jelly, then extruding pelletization at normal temperature, then high temperature sintering molding, is made High efficiency, low cost adsorbent for heavy metal containing wastewater treatment.
2. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, It is characterized in that: in step (1) the pottery charcoal mixed-powder, 68 ~ 84 parts by weight of waste ceramic powder, 10 ~ 20 parts by weight of charcoal powder, chaff 6 ~ 12 parts by weight of aldehyde powder.
3. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, Be characterized in that: the parts by weight of step (2) each raw material are make pottery 20 ~ 30 parts by weight of charcoal mixed-powder, ethyl alcohol and sulfamic acid 30 ~ 40 parts by weight of mixed aqueous solution, eight hydration 10 ~ 15 parts by weight of zirconium oxychloride, 15 ~ 40 parts by weight of sodium hydroxide solution.
4. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, It is characterized in that: in the mixed aqueous solution of step (2) ethyl alcohol and sulfamic acid, 20 ~ 30 parts by weight of ethyl alcohol, sulfamic acid 5 ~ 10 Parts by weight, 60 ~ 75 parts by weight of water；The mass concentration of the sodium hydroxide solution is 2 ~ 4%.
5. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, Be characterized in that: step (3) shuck is chestnut shell, in walnut shell, green shell, bar denier wood shell, pine nut shell, Pericarppium Armeniacae Amarum One or more composition.
6. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, Be characterized in that: the parts by weight of step (3) each raw material are 2 ~ 10 parts by weight of shuck powder, 90 ~ 98 weight of liquor potassic permanganate Part.
7. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, Be characterized in that: step (4) thickener is one or more of diatomite, Silica hydrogel, attapulgite soil, sodium bentonite Composition.
8. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, Be characterized in that: step (4) modified zirconia pottery 30 ~ 40 parts by weight of charcoal mixed-powder, are gone at modified 10 ~ 20 parts by weight of shuck powder 30 ~ 56 parts by weight of ionized water, 4 ~ 10 parts by weight of thickener.
9. a kind of preparation method of the high efficiency, low cost adsorbent for heavy metal containing wastewater treatment according to claim 1, Be characterized in that: the temperature of step (4) described high temperature sintering is 200 ~ 280 DEG C, and the time is 2 ~ 3h.
10. any one of claim 1 ~ 9 preparation method is prepared a kind of for the efficient low of heavy metal containing wastewater treatment Cost adsorbents.
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