CN105327675A - Nanometer-ZnO-loaded expanded vermiculite adsorbing material and preparation method thereof - Google Patents

Nanometer-ZnO-loaded expanded vermiculite adsorbing material and preparation method thereof Download PDF

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CN105327675A
CN105327675A CN201510833285.1A CN201510833285A CN105327675A CN 105327675 A CN105327675 A CN 105327675A CN 201510833285 A CN201510833285 A CN 201510833285A CN 105327675 A CN105327675 A CN 105327675A
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expanded vermiculite
preparation
zinc acetate
zno
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管登高
孙遥
徐冠立
孙传敏
林金辉
陈婷
崔迎辉
戴泽航
吴彩文
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Chengdu Univeristy of Technology
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Abstract

The invention discloses a nanometer-ZnO-loaded expanded vermiculite adsorbing material and a preparation method thereof. The preparation method of the nanometer-ZnO-loaded expanded vermiculite adsorbing material comprises the following steps: adding expanded vermiculite into zinc acetate dihydrate mixed solution, and evenly stirring to obtain zinc acetate mixed solution; then, dropwise adding oxalic acid ethyl alcohol solution into the zinc acetate dihydrate mixed solution, and regulating the pH (Potential Of Hydrogen) value of the zinc acetate dihydrate mixed solution to 6-10; then, stirring the obtained mixture in a constant-temperature water bath kettle at the temperature of 60-90DEG C to react for 0.5-4h, and then filtering to obtain gel; after the gel is roasted for 1.5-3h at the temperature of 450-600DEG C, cooling to the room temperature to obtain the nanometer-ZnO-loaded expanded vermiculite adsorbing material. The obtained nanometer-ZnO-loaded expanded vermiculite adsorbing material can simultaneously adsorb and process heavy metal ions, such as lead, mercury, cadmium, nickel ins and the like in a water body and kill pathogenic bacteria, such as colibacillus in the water body, the adsorption rate of the obtained nanometer-ZnO-loaded expanded vermiculite adsorbing material is 90-99%, the effective killing rate of the obtained nanometer-ZnO-loaded expanded vermiculite adsorbing material on bacteria is above 95%, and the adsorbing material has good and stable thermostability and is safe and nontoxic for a human body.

Description

Expanded vermiculite sorbing material of a kind of loaded with nano ZnO and preparation method thereof
Technical field
The present invention relates to heavy metal ion adsorbed field, relate to expanded vermiculite sorbing material of a kind of loaded with nano ZnO and preparation method thereof in particular.
Background technology
Earth freshwater resources reserves are limited, and the fresh water drunk for the mankind only accounts for 0.26% of water globe total amount, and mostly is underground water.According to the data estimation of UNESCO (UNESCO) water institute of education, the year two thousand fifty the population of whole world lack of water may reach 3,000,000,000.China is one of water resource country that there is a serious shortage in the supply per capita in the world.
But along with in the exploitation of heavy metal, smelting, the discharge of processing industry " three wastes " and the use procedure of sewage irrigation, agricultural chemicals, herbicide, chemical fertilizer etc., cause the heavy metals such as lead, mercury, cadmium, cobalt to enter air, water and soil and cause serious environmental pollution.Wherein, heavy metal is particularly serious to the pollution of water quality, according to the statistics such as " water resources in china publication in 2010 " and " the sewage treatment industry market prediction of 2013-2017 China is reported with investment strategy planning application ", the urban groundwater of China about 90% is subject to the pollutions such as heavy metal.
Heavy metal-pollutedly have a finger in every pie the environmental pollution caused by heavy metal or its compound, its extent of injury depends on the concentration that heavy metal exists in environment, food and organism and chemical form.Heavy metal pollution is mainly manifested in water pollutions.Kind, the physicochemical property of metal are not only depended in the harm of Heavy Metals in Waters, but also depend on the concentration of metal and the valence state of existence and form, even if useful metallic element concentration exceedes a certain numerical value also have violent toxicity, make animals and plants poisoning, even dead.
At present, China's heavy metal pollution is quite serious, and many places water body exists the heavy metal ion such as lead, mercury, arsenic, cadmium, chromium, zinc, copper, nickel and to exceed standard phenomenon.The pollution of heavy metal ion to water body has that toxicity is large, difficult degradation, disguise and cumulative bad feature, be permanent and serious to the harm of environment, organism and human body.These heavy metals can not be decomposed in water, and people drinks rear toxicity and amplifies, and other toxin in water are combined and generate the larger metallo-organic compound (as organic mercury, Organic leadP, organo-arsenic, organotin etc.) of toxicity.Meanwhile, heavy metal is the enrichment by food chain easily, as the heavy metal of discharging with waste water, even if concentration is little, also can accumulate in algae and bed mud, is adsorbed by fish and shellfish body surface, produces food chain and concentrates, thus cause public hazards.Heavy metal in human body can and protein and various enzyme there is strong interaction, make them lose activity, also may enrichment in some organ of human body, if exceed the tolerant limit of human body, human body acute poisoning, subacute poisoning, slow poisoning etc. can be caused, people is known from experience and causes very large harm, such as, the nuisance diseases such as the minamata disease (mercury pollution) that Japan occurs and Itai-itai diseases (cadmium pollution), are all caused by heavy metal pollution.
The harm of heavy metal ion should not be underestimated, and letting alone the discharge of heavy metal wastewater thereby, is the destruction to environment, is also not responsible to mankind itself, especially to the waste of resource.Heavy metal ion has caused the great attention of countries in the world scientist to the pollution of water quality, addresses this problem extremely urgent.Administering heavy-metal pollution in water is the important component part of water pollution control." water prevention and cure of pollution action plan " (being called for short " ten, water ") that State Council of China issues is the guide of national heavy metal pollution of water body preventing and controlling.
Different according to the existing forms of Heavy Metals in Waters ion, heavy metal ion control can be divided into morphologic change method and form not to change method.Wherein, morphologic change method effectively can reduce, eliminate heavy-metal pollution, but not to reclaim for the purpose of heavy metal ion resource, mainly comprises the precipitation method, oxidation-reduction method, electrochemical treatment, bioanalysis etc.; Not changing waveforms method is method heavy metal ion reclaimed according to original form, mainly comprises ion-exchange, evaporation concentration method, solvent extraction, absorption method etc.
Wherein, absorption method is that cost performance is higher and can the method for effective heavy-metal ion removal.The advantage that mineral adsorbing material has applied range to heavy metal contaminants in water, cost is low, harmonious environment, clearance are high, simple to operate, can be recycled is that in water, the measure of heavy metal conventional control cannot be compared.The heavy metal ion mineral adsorbing material with practical value has active carbon, attapulgite, bentonite, zeolite, medical stone, diatomite, sepiolite etc.With mineral material have that adsorbance is large, removal effect good as adsorbent heavy-metal ion removal, with low cost, operating procedure and equipment simple and the advantage such as to recycle.Medical stone is the silicate rock class complex mineral of nonhazardous, and chemical composition and the loose structure feature of medical stone make it have certain absorption property.But composition, the factor such as structure and pattern of medical stone can affect its absorption property.
Vermiculite is a kind of secondary metamorphic mineral of water aluminosilicate containing magnesium of layer structure, and raw ore is outer to be formed through hydrothermal alteration effect or weathering by black (gold) mica usually like mica, and because being flexure shape when its dehydration of being heated is expanded, form exactly likes leech, therefore claims vermiculite.Fabric and raw-vermiculite sheet after high-temperature roasting, its volume energy undergoes rapid expansion several times to tens times, the vermiculite after volumetric expansion is just expanded vermiculite.The purposes of vermiculite has been widely applied to building, gold of living, oil, shipbuilding, environmental protection, insulation, heat insulation, insulate, the field such as energy-conservation.Expanded vermiculite has unique structural property and surface nature, and nontoxic, aseptic and chemical inertness, can be used as carrier, sticking agent, feed addictive and adsorbent for heavy metal etc.But independent vermiculite uses as adsorbent, its adsorption capacity is general, obtain good adsorption capacity, and the consumption of vermiculite is comparatively large, and the Appropriate application saving not meeting resource uses agreement.
And existing most of anti-biotic material is organic substance, there is poor heat resistance, volatile, easy decomposition produces the shortcomings such as nuisance, security be poor.Therefore there is again the novel absorption material of good anti-microbial property to tackle the improvement demand polluted and be on the rise while being badly in need of now wanting a kind of inorganic adsorbent ability powerful.
Summary of the invention
The invention provides expanded vermiculite sorbing material of a kind of loaded with nano ZnO and preparation method thereof, the feature of this adsorbent combining nano ZnO and expanded vermiculite, with two water zinc acetates for zinc source, oxalic acid is complexing agent, and ethanol is solvent, and NaOH is stabilizing agent, polyethylene glycol is surface modifier, adopt sol-gel process to load on expanded vermiculite by nano-ZnO, through operations such as gel, drying and roastings, make the expanded vermiculite sorbing material of loaded with nano ZnO.Compared with vermiculite, can the heavy metal ion such as lead, mercury, arsenic, cadmium, chromium, zinc, copper, nickel simultaneously in adsorption treatment water body and kill Escherichia coli in water body, gold-coloured staphylococci, salmonella, its adsorption rate reaches 90-99%, more than 95% is reached to effective killing rate of bacterium simultaneously, this adsorbent good heat resistance, stable, to human-body safety nonhazardous.
For solving above-mentioned technical problem, the present invention by the following technical solutions:
A preparation method for the expanded vermiculite sorbing material of loaded with nano ZnO, comprises the following steps:
(1), by two water zinc acetate Zn (Ac) 22H 2o, is dissolved in ethanol, forms Zn (Ac) 22H 2o ethanolic solution, adds the equimolar polyethylene glycol with zinc ion, obtains two water zinc acetate mixed liquors;
(2), expanded vermiculite is added two water zinc acetate mixed solutions to stir, the ratio of two water zinc acetates and expanded vermiculite is 4-40mmol/g, obtain the zinc acetate mixed solution that zinc acetate concentration is 0.4-0.8mol/L, again oxalic acid ethanolic solution is added drop-wise in zinc acetate mixed solution, regulate the pH value of zinc acetate mixed solution to 6-10 with NaOH ethanolic solution, then filter after being placed in the thermostat water bath stirring reaction 0.5-4h of 60-90 DEG C, obtain gel;
(3), by after gel detergent twice, after 80-110 DEG C of heating 0.4-1h, then after 450 DEG C-600 DEG C roasting 1.5-3h, the expanded vermiculite sorbing material that namely room temperature obtains loaded with nano ZnO is cooled to.
In gel process, need the cation exchange effect in conjunction with zinc oxide and expanded vermiculite, select suitable chemical reagent, can obtain good gel result (as whether gel stablizes plastic, whether part plastic and part coacervation of colloid), and good gel result directly has influence on internal structure and the physical property of the expanded vermiculite sorbing material of final loaded with nano ZnO.The particle diameter of such as expanded vermiculite and interlayer structure are on the impact of exchange interaction, and the particle diameter of expanded vermiculite and interlayer structure are all relevant with the preparation method of expanded vermiculite.
The granularity of expanded vermiculite is 9-1500 μm.
The preparation method of expanded vermiculite is: after vermiculite mineral being ground to granularity 1.5-150 μm, carries out roasting, and sintering temperature is 500-850 DEG C, and roasting time is 0.5-5min.The preparation method of expanded vermiculite is to the endothecium structure important of expanded vermiculite, and the performance of the expanded vermiculite that diverse ways obtains is different, and adsorption capacity is naturally different.
Sintering temperature is 650-850 DEG C, and roasting time is 1-3min.
The mol ratio of step (2) mesoxalic acid and two water zinc acetates is 1:1-1:5.
Sintering temperature in step (3) is 550-600 DEG C.
Mixing speed in step (3) is 1400-2000r/min.
The expanded vermiculite sorbing material of the loaded with nano ZnO that preparation method as the aforementioned obtains, the weight of nano-ZnO is the 5-40wt% of the expanded vermiculite sorbing material weight of loaded with nano ZnO.The heap(ed) capacity of nano zine oxide can have influence on follow-up adsorption capacity, the problem of an ion-exchange absorption existence saturation degree, therefore in the sense that, the more adsorption capacities of nano zine oxide amount are stronger, but the loading of nano zine oxide can not be The more the better, otherwise cost intensive, also extensive use is unfavorable for, the heap(ed) capacity of too much nano zine oxide also improves little to antibiotic property, being loaded in addition technically also can be restricted, loading affects by preparation condition, therefore controls preparation condition of the present invention significant.
Nano zine oxide is a kind of polyfunctional new inorganic material, and its granular size is about 1 ~ 100 nanometer.Due to the granular of crystal grain, its Electronic Structure and crystal structure change, create skin effect, bulk effect, quantum size effect and macroscopical tunnel-effect that common zinc oxide does not have, and the high grade of transparency, polymolecularity and good counter infrared ray, ultraviolet and sterilizing function.Nano-ZnO has been widely used in ultraviolet light masking material, antiseptic, fluorescent material, catalysis material and water treatment agent etc.
Present invention applicant finds that the adsorption capacity of the expanded vermiculite sorbing material of the loaded with nano ZnO obtained by said method is not that the two adsorption capacity of nano zine oxide and expanded vermiculite is simply added, but there is obvious complex effect, this may except the specific area of loaded with nano ZnO itself be comparatively large, in the expanded vermiculite sorbing material forming process of loaded with nano ZnO, between the structure sheaf that Zn ion enters expanded vermiculite and the effect of expanded vermiculite generation cation exchange, the structure sheaf of expanded vermiculite is destroyed and at random unordered, caused by surface area in the structure sheaf of expanded vermiculite significantly increases.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention with two water zinc acetates for zinc source, oxalic acid is complexing agent, ethanol is solvent, NaOH is stabilizing agent, polyethylene glycol is surface modifier, sol-gel process is adopted to load on expanded vermiculite by nano-ZnO, through gel, the operations such as drying and roasting, the obtained expanded vermiculite sorbing material carrying nano-ZnO, compared with vermiculite, can lead simultaneously in adsorption treatment water body, mercury, cadmium, chromium, copper, the heavy metal ion such as nickel and the Escherichia coli killed in water body, gold-coloured staphylococci, salmonella, its adsorption rate reaches 90-99%, more than 95% is reached to effective killing rate of bacterium simultaneously, this adsorbent good heat resistance, stable, to human-body safety nonhazardous.
Detailed description of the invention
The present invention is further illustrated below.Embodiments of the present invention include but not limited to the following example.
Embodiment 1
A preparation method for the expanded vermiculite sorbing material of loaded with nano ZnO, comprises the following steps:
(1), by two water zinc acetate Zn (Ac) 22H 2o, is dissolved in ethanol, forms Zn (Ac) 22H 2o ethanolic solution, adds the equimolar polyethylene glycol with zinc ion, obtains two water zinc acetate mixed liquors;
(2), expanded vermiculite is added two water zinc acetate mixed solutions to stir, the ratio of two water zinc acetates and expanded vermiculite is 20mmol/g, obtain the zinc acetate mixed solution that zinc acetate concentration is 0.4-0.8mol/L, again oxalic acid ethanolic solution is added drop-wise in zinc acetate mixed solution, regulate the pH value of zinc acetate mixed solution to 6-10 with NaOH ethanolic solution, then filter after being placed in the thermostat water bath stirring reaction 0.5-4h of 60-90 DEG C, obtain gel;
(3), by after gel detergent twice, after 80-110 DEG C of heating 0.4-1h, then after 450 DEG C of roasting 1.5-3h, the expanded vermiculite sorbing material that namely room temperature obtains load 25wt% nano-ZnO is cooled to.
The granularity of expanded vermiculite is 750 μm.
The preparation method of expanded vermiculite is: after vermiculite mineral being ground to granularity 60-80 μm, carries out roasting, and sintering temperature is 500 DEG C, and roasting time is 4-5min.
Embodiment 2
A preparation method for the expanded vermiculite sorbing material of loaded with nano ZnO, comprises the following steps:
(1), by two water zinc acetate Zn (Ac) 22H 2o, is dissolved in ethanol, forms Zn (Ac) 22H 2o ethanolic solution, adds the equimolar polyethylene glycol with zinc ion, obtains two water zinc acetate mixed liquors;
(2), expanded vermiculite is added two water zinc acetate mixed solutions to stir, the ratio of two water zinc acetates and expanded vermiculite is 4mmol/g, obtain the zinc acetate mixed solution that zinc acetate concentration is 0.4-0.8mol/L, again oxalic acid ethanolic solution is added drop-wise in zinc acetate mixed solution, regulate the pH value of zinc acetate mixed solution to 6-10 with NaOH ethanolic solution, then filter after being placed in the thermostat water bath stirring reaction 0.5-4h of 60-90 DEG C, obtain gel;
(3), by after gel detergent twice, after 80-110 DEG C of heating 0.4-1h, then after 600 DEG C of roasting 1.5-3h, the expanded vermiculite sorbing material that namely room temperature obtains loaded with nano 40wt%ZnO is cooled to.
The granularity of expanded vermiculite is 9 μm.
The preparation method of expanded vermiculite is: after vermiculite mineral being ground to granularity 1.5-15 μm, carries out roasting, and sintering temperature is 550 DEG C, and roasting time is 4-5min.
Embodiment 3
A preparation method for the expanded vermiculite sorbing material of loaded with nano ZnO, comprises the following steps:
(1), by two water zinc acetate Zn (Ac) 22H 2o, is dissolved in ethanol, forms Zn (Ac) 22H 2o ethanolic solution, adds the equimolar polyethylene glycol with zinc ion, obtains two water zinc acetate mixed liquors;
(2), expanded vermiculite is added two water zinc acetate mixed solutions to stir, the ratio of two water zinc acetates and expanded vermiculite is 40mmol/g, obtain the zinc acetate mixed solution that zinc acetate concentration is 0.4-0.8mol/L, again oxalic acid ethanolic solution is added drop-wise in zinc acetate mixed solution, the mol ratio of oxalic acid and two water zinc acetates is 1:1-1:5, regulate the pH value of zinc acetate mixed solution to 6-10 with NaOH ethanolic solution, then filter after being placed in the thermostat water bath stirring reaction 0.5-4h of 60-90 DEG C, obtain gel;
(3), by after gel detergent twice, after 80-110 DEG C of heating 0.4-1h, then after 550 DEG C of roasting 1.5-3h, the expanded vermiculite sorbing material that namely room temperature obtains load 10wt% nano-ZnO is cooled to.
The granularity of expanded vermiculite is 800-1200 μm.
The preparation method of expanded vermiculite is: after vermiculite mineral being ground to granularity 90-150 μm, carries out roasting,
Sintering temperature is 750 DEG C, and roasting time is 1-1.5min.
Mixing speed in step (3) is 1400-2000r/min.
Embodiment 4
A preparation method for the expanded vermiculite sorbing material of loaded with nano ZnO, comprises the following steps:
(1), by two water zinc acetate Zn (Ac) 22H 2o, is dissolved in ethanol, forms Zn (Ac) 22H 2o ethanolic solution, adds the equimolar polyethylene glycol with zinc ion, obtains two water zinc acetate mixed liquors;
(2), expanded vermiculite is added two water zinc acetate mixed solutions to stir, the ratio of two water zinc acetates and expanded vermiculite is 30mmol/g, obtain the zinc acetate mixed solution that zinc acetate concentration is 0.4-0.8mol/L, again oxalic acid ethanolic solution is added drop-wise in zinc acetate mixed solution, the mol ratio of oxalic acid and two water zinc acetates is 1:1-1:5, regulate the pH value of zinc acetate mixed solution to 6-10 with NaOH ethanolic solution, then filter after being placed in the thermostat water bath stirring reaction 0.5-4h of 60-90 DEG C, obtain gel;
(3), by after gel detergent twice, after 80-110 DEG C of heating 0.4-1h, then after 600 DEG C of roasting 1.5-3h, the expanded vermiculite sorbing material that namely room temperature obtains loaded with nano 30wt%ZnO is cooled to.
Sintering temperature is 550-650 DEG C, and roasting time is 2-3min.
The granularity of expanded vermiculite is 200-450 μm.
The preparation method of expanded vermiculite is: after vermiculite mineral being ground to granularity 20-50 μm, carries out roasting, and sintering temperature is 600 DEG C, and roasting time is 1-2min.
Mixing speed in step (3) is 1400-2000r/min.
Embodiment 5
A preparation method for the expanded vermiculite sorbing material of loaded with nano ZnO, comprises the following steps:
(1), by two water zinc acetate Zn (Ac) 22H 2o, is dissolved in ethanol, forms Zn (Ac) 22H 2o ethanolic solution, adds the equimolar polyethylene glycol with zinc ion, obtains two water zinc acetate mixed liquors;
(2), expanded vermiculite is added two water zinc acetate mixed solutions to stir, the ratio of two water zinc acetates and expanded vermiculite is 10mmol/g, obtain the zinc acetate mixed solution that zinc acetate concentration is 0.4-0.8mol/L, again oxalic acid ethanolic solution is added drop-wise in zinc acetate mixed solution, the mol ratio of oxalic acid and two water zinc acetates is 1:1-1:5, regulate the pH value of zinc acetate mixed solution to 6-10 with NaOH ethanolic solution, then filter after being placed in the thermostat water bath stirring reaction 0.5-4h of 60-90 DEG C, obtain gel;
(3), by after gel detergent twice, after 80-110 DEG C of heating 0.4-1h, then after 600 DEG C of roasting 1.5-3h, the expanded vermiculite sorbing material that namely room temperature obtains load 5wt% nano-ZnO is cooled to.
Sintering temperature is 650 DEG C, and roasting time is 1-2min.
The granularity of expanded vermiculite is 1400-1500 μm.
The preparation method of expanded vermiculite is: after vermiculite mineral being ground to granularity 130-150 μm, carries out roasting, and sintering temperature is 850 DEG C, and roasting time is 0.5-1min.
Mixing speed in step (3) is 1400-2000r/min.
Embodiment 6
2g granularity be the vermiculite of 1400 μm, the expanded vermiculite of the loaded with nano ZnO of embodiment 1-embodiment 5 is placed in 6 250mL beakers respectively.Then the heavy metal Cd prepared by deionized water is added respectively 2+, Pb 2+, Ni 2+, Cu 2+concentration is the 100mL mixed solution of 10.0mg/L, and solution is adjusted to pH=7 by the salpeter solution with 5% or 5% ammoniacal liquor.Then stir (300r/min) 3h at 40 DEG C with thermostatic electromagnetic agitator, after sorbing material being separated 5min with absorption raffinate with centrifuge under 7000r/min condition, getting supernatant, measure Cd in solution by ICP-OES method 2+, Pb 2+, Ni 2+, Cu 2+residual ion mass concentration, and calculate Cd 2+, Pb 2+, Ni 2+, Cu 2+adsorption rate.Wherein, adsorption rate=(heavy metal ion initial concentration C 0concentration of heavy metal ion C after ﹣ absorption)/heavy metal ion initial concentration C 0× 100%.Filter, the metal ion content in rear mensuration filtrate, its result is as shown in table 1.
Take Escherichia coli as the anti-microbial property of expanded vermiculite that experimental strain tests vermiculite, loaded with nano ZnO.Step is as follows: (1) agar medium: take 10g agar powder, dusty yeast 1.5g, peptone 3g, sodium chloride 1.5g, sterilized water 300mL, regulate pH=7.6 with NaOH, after heating for dissolving, high-temperature sterilization 2h, for subsequent use, (2) expanded vermiculite of the vermiculite and loaded with nano ZnO that are all 2g same particle sizes is placed in two culture dishes respectively, add appropriate amounts of sterilized water mixing, add the agar medium that 20mL is cooled to 45 DEG C, 2mL Escherichia coli solution is pipetted with Sterile pipette, keep flat and fully shake up on the table, become dull and stereotyped after condensation, be inverted in the insulating box of 37 DEG C and cultivate 24h, meter total plate count, do antibacterial group and the experiment of blank group simultaneously, bacteriostasis rate (R) is by following formulae discovery: R=(control group average colony number-experimental group average colony number)/experimental group average colony number × 100% experimental result shows, vermiculite does not have anti-microbial property to Escherichia coli, and the expanded vermiculite of loaded with nano ZnO all can reach 96.5% to colibacillary effective killing rate.
Be embodiments of the invention as mentioned above.The present invention is not limited to above-mentioned embodiment, and anyone should learn the structure change made under enlightenment of the present invention, and every have identical or close technical scheme with the present invention, all falls within protection scope of the present invention.

Claims (8)

1. a preparation method for the expanded vermiculite sorbing material of loaded with nano ZnO, is characterized in that: comprise the following steps:
(1), by two water zinc acetate Zn (Ac) 22H 2o, is dissolved in suitable ethanol, forms Zn (Ac) 22H 2o ethanolic solution, adds the equimolar polyethylene glycol with zinc ion, obtains two water zinc acetate mixed liquors;
(2), expanded vermiculite is added two water zinc acetate mixed solutions to stir, obtain the zinc acetate mixed solution that zinc acetate concentration is 0.4-0.8mol/L, the ratio of two water zinc acetates and expanded vermiculite is 4-40mmol/g, again oxalic acid ethanolic solution is added drop-wise in zinc acetate mixed solution, regulate the pH value of zinc acetate mixed solution to 6-10 with NaOH ethanolic solution, then filter after being placed in the thermostat water bath stirring reaction 0.5-4h of 60-90 DEG C, obtain gel;
(3), by after gel detergent twice, after 80-110 DEG C of heating 0.4-1h, then after 450 DEG C-600 DEG C roasting 1.5-3h, the expanded vermiculite sorbing material that namely room temperature obtains loaded with nano ZnO is cooled to.
2. preparation method according to claim 1, is characterized in that: the granularity of expanded vermiculite is 9-1500 μm.
3. preparation method according to claim 1, is characterized in that: the preparation method of expanded vermiculite is: after vermiculite mineral being ground to granularity 1.5-150 μm, carries out roasting, and sintering temperature is 500-850 DEG C, and roasting time is 0.5-5min.
4. preparation method according to claim 3, is characterized in that: sintering temperature is 550-650 DEG C, and roasting time is 1-3min.
5. preparation method according to claim 1, is characterized in that: the mol ratio of step (2) mesoxalic acid and two water zinc acetates is 1:1-1:5.
6. preparation method according to claim 1, is characterized in that: the sintering temperature in step (3) is 550-600 DEG C.
7. preparation method according to claim 1, is characterized in that: the mixing speed in step (3) is 1400-2000r/min.
8. the expanded vermiculite sorbing material of the loaded with nano ZnO that the preparation method as described in claim 1-7 obtains, is characterized in that, the weight being loaded into nano-ZnO is the 5-40wt% of the expanded vermiculite sorbing material weight of loaded with nano ZnO.
CN201510833285.1A 2015-11-25 2015-11-25 Nanometer-ZnO-loaded expanded vermiculite adsorbing material and preparation method thereof Pending CN105327675A (en)

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