CN1915849A - Method for preparing composite assembled object of magnetic ferriferous oxide/ molecular sieve of Nano zeolite - Google Patents
Method for preparing composite assembled object of magnetic ferriferous oxide/ molecular sieve of Nano zeolite Download PDFInfo
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- CN1915849A CN1915849A CN 200610030899 CN200610030899A CN1915849A CN 1915849 A CN1915849 A CN 1915849A CN 200610030899 CN200610030899 CN 200610030899 CN 200610030899 A CN200610030899 A CN 200610030899A CN 1915849 A CN1915849 A CN 1915849A
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Abstract
This invention relates to a method for preparing magnetic iron oxide/nanoscale zeolite molecular sieve composite. The method comprises: (1) selecting nanoscale zeolite crystal material; (2) introducing Fe2+/Fe3+ as active reaction sites through ion exchange under the action of electrostatic attraction; (3) dropping 25% ammonia solution for reaction of the active sites in an alkaline medium, washing with water and drying; (4) removing phosphate ions and arsenate ions from water by using a dynamic adsorption apparatus. The method has such advantages as low cost, simple operation and high adsorption rate, and can be widely used for water purification.
Description
Technical field
That the present invention relates to is a kind of preparation method who is used for the water body purification of environmental technology field, the composite assembled preparation method of particularly a kind of magnetic iron oxide/molecular sieve of Nano zeolite.
Background technology
Body eutrophication will cause aquatic plant, algal bloom, and oxygen level descends, serious consequences such as water quality deterioration.Wherein phosphorus has special effect for the eutrophication of water body.At present, inorganic phosphorus pollution problem in the southeastern coastal areas seawater such as China Taizhou has caused that government concerned pays much attention to.A large amount of uses of phosphorous washing powder, phosphorous nitride fertilizer are main " killers " who causes water body system phosphorus to pollute.Because phosphorus is all required important elements of biological growth, so phosphorus not only can cause in the water algae overgrowing, but also can cause that bacterium breeds in a large number in the lake.Phosphorus also is the killer in fish even lake, and the bacterium of a large amount of propagation has consumed the oxygen in the water, makes the fish kills that relies on oxygen existence, and bacterium also can be dead because of anoxic subsequently, finally causes serious disastrous effects such as the lake is aging, death.Phosphorus also can cause the threat of the body eutrophication similar to above-mentioned situation to the waters, beach of torrid areas.
Simultaneously, significant is that the compound of arsenic has biological effect widely as a kind of protoplasma poisonous substance of metalloid, is defined as first kind carcinogens by the Center for Disease Control and the international research institution that gives protection against cancer.In recent years, along with the fast development of industries such as mining and metallurgy, pottery, leather, agricultural chemicals, the pollution of arsenic is serious day by day in the groundwater environment.In the water there be the source of arsenic contamination: (1) natural source: the last spilling water of mineral and atmospheric disintegration of rocks, volcanic eruption, hot spring; (2) artificial source: the exploitation of arsenide and smelting.These factors have all caused very big pollution to underground water and tap water.High arsenic drinking-water is mainly underground water.
At present, traditional fractionation by adsorption mode is as a kind of water technology commonly used, relatively be widely used in phosphorus in the environment water the removal process of typical pollutant such as arsenic.Find according to comprehensive retrieval, utilize phosphate radical in the tailings planar water of ferriferous oxide ore deposit in order to solve body eutrophication problem " Water Research, 2004,38:1318-1326 " report to existing domestic and international correlation technique document.But it is pointed out that materials such as utilizing ferriferous oxide ore deposit tailings as sorbent material, in water body, introduce a large amount of new source of pollution such as metal hetero-ion easily, have the potential problems that water body constituted secondary pollution again.
But so far for extremely, existing relevant adsorption separation technology is ubiquity still: adsorption efficiency is on the low side; The manufacturing cost height of sorbing material, process is removed in relevant absorption, problems such as complex operation step, therefore the environment water system purification problem that makes typical pollutants such as above-mentioned phosphorus and arsenic cause can not get effective solution always.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, provide a kind of magnetic iron oxide/molecular sieve of Nano zeolite composite assembled preparation method.Make that it is with low cost, operating process is easy, adsorption efficiency is high,, and be easy to the characteristics of recycling use, the scavenging process of large-scale application water body in environment according to its good magnetic properties that has.
The present invention is achieved by the following technical solutions, and method concrete steps of the present invention are as follows:
1. select nano level zeolite crystal material for use;
2. utilize the electrostatic attraction effect, by the fixing Fe that introduces of ion-exchange method
2+/ Fe
3+As follow-up active reaction sites.
3. dropwise add 25% strong aqua, make corresponding Fe
2+/ Fe
3+Specific chemical reaction takes place in avtive spot in alkaline medium, after through the washing, drying process, the composite assembled material of magnetic iron oxide/molecular sieve of Nano zeolite of making.
4. above-mentioned materials is utilized Dynamic gas-mixing and adsorption devices, phosphate radical, arsenate pollutent in the water are removed in absorption.
Described Fe
2+/ Fe
3+Avtive spot is meant the alumina negative potential that utilizes in the molecular sieve of Nano zeolite skeleton structure, utilizes the electrostatic attraction effect, by the Fe of ion-exchange method introducing
2+/ Fe
3+Avtive spot.
Described ion-exchange method by ion-exchange method, is introduced Fe in relevant nanometer zeolite molecular sieve skeleton structure
2+/ Fe
3+The operating process of avtive spot, utilize following dual mode to finish:
A: make the molecular sieve of Nano zeolite material place a certain proportion of Fe
2+/ Fe
3+In the solution (1: 2～2: 3), 60 ℃ of oil bath reflux a few hours (8～14 hours), after filter fast.
B: with the Fe of molecular sieve of Nano zeolite material with certain proportion
2+/ Fe
3+Solution (1: 2～2: 3) thorough mixing is even, is placed on to have in the teflon-lined stainless steel autoclave, and 60 ℃ of heating a few hours (8～14 hours) are closely dried to solution.
Described ion-exchange method is by the fixing Fe that introduces of ion-exchange method
2+/ Fe
3+The molecular sieve of Nano zeolite material of avtive spot need be under the inert atmosphere of nitrogen protection, and dropwise ammoniacal liquor forms assembly.
This material has carried out the sign of infrared and magnetic hysteresis loop, FT-IR collection of illustrative plates, 580cm
-1Near be the characteristic peak of γ-Fe2O3; 1100,1390cm
-1Near be the charateristic avsorption band of Fe3O4, as can be seen in zeolite surface success load the oxide compound of iron.The result of follow-up magnetic hysteresis loop as can be seen in the assembly materials structure oxide compound saturation magnetization of the iron of load be 3.9emu/g.Therefore, the above-mentioned characterization result of analysis-by-synthesis illustrates to have prepared the composite assembled material of magnetic iron oxide/molecular sieve of Nano zeolite.
That selected material has is with low cost, be easy to regenerate, stable in properties and satisfy the requirement of the fractionation by adsorption of water pollutant.Can be used for phosphorous, the purification of arsenic water body and the processing of sewage.Utilize alumina negative potential abundant in the synthetic molecular sieve of Nano zeolite structure voluntarily, introduce a certain proportion of Fe by ion-exchange method
2+/ Fe
3+After, select suitable chemical reaction process, the synthetic composite assembled material of a kind of novel magnetic iron oxide/molecular sieve of Nano zeolite that obtains.And utilize some material such as the interactional characteristic of specificity between phosphate radical, arsenate and Fe, under the externally-applied magnetic field of certain intensity, make the novel magnetic ferriferous oxide/molecular sieve of Nano zeolite of pollutents such as above-mentioned saturated absorption phosphate radical, arsenate composite assembled from corresponding polluted-water sharp separation.This regneration of adsorbent material process is simple to operation, can satisfy the needs of extensive environment water systemic contamination governance process.
Fully, select the fixing Fe of introducing of nanosized zeolitic material of different-shape character according to the abundant ion-exchange performance of nano zeolite
2+/ Fe
3+Avtive spot, thereby, under suitable alkaline reactive medium condition, prepare the composite assembled material of novel magnetic ferriferous oxide/molecular sieve of Nano zeolite easily.In the corresponding composite assembled material structure of later use iron with phosphate radical specificity between arsenate interact, with selective adsorption efficiently separate in the water body system phosphate radical typical pollutant such as arsenate.
The present invention has the method for the solid adsorption material of ferromegnetism character as a kind of efficient, quick, separation easy economy, the suitable pattern that screening is obtained and the molecular sieve of Nano zeolite of character carry out modification, make the composite assembled material of magnetic iron oxide/molecular sieve of Nano zeolite, both bring into play the good absorption property of molecular sieve of Nano zeolite and also made full use of this advantage of magnetic, can under externally-applied magnetic field, make sorbing material and water body system sharp separation, thereby scientifically solve the recycling problem of corresponding sorbing material.In a word, the certain pattern that screening obtains and the molecular sieve of Nano zeolite material of character, through a series of chemical technology means, the composite assembled material of novel magnetic ferriferous oxide/molecular sieve of Nano zeolite for preparing, can develop into from now in the extensive improvement environment water system phosphate radical typical pollutant aspect such as arsenate, a kind of new environmentally friendly adsorption functional material.
Embodiment
The present invention is applied to the composite assembled preparation method of novel magnetic ferriferous oxide/molecular sieve of Nano zeolite in water body purification field, utilize alumina negative potential abundant in the synthetic molecular sieve of Nano zeolite structure voluntarily, introduce a certain proportion of Fe by ion-exchange method
2+/ Fe
3+After, drip 25% strong aqua and divalence and the effect of ferric ion avtive spot, at the magnetic oxide of zeolite surface generation iron, washing afterwards, drying, the synthetic composite assembled material of a kind of novel magnetic iron oxide/molecular sieve of Nano zeolite that obtains.Related experiment result shows, the composite assembled material of magnetic iron oxide/nano zeolite can effectively purify phosphate radical in the adsorbed water body, typical pollutants such as arsenate, and have easy and simple to handlely, be easy to reclaim and unique advantage such as renewable recycle.In the operating process, make sharp separation between composite assembled material of magnetic iron oxide/molecular sieve of Nano zeolite and water body system by externally-applied magnetic field, later use 0.5mol/L NaOH handles iterative regenerable.
Embodiment 1
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.3mol/L FeCl
2.4H
2O is 100mL airtight stirring and refluxing 12 hours in 60 ℃ of oil baths altogether, filters.
3. in 60 ℃ of water-baths, the inert atmosphere of nitrogen protection down on filter cake with speed Dropwise 5 0mL 25% strong aqua of 2 of per seconds and stirred one hour fast, generate the chocolate material, be washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. (analytically pure potassium primary phosphate KH2PO4 is mixed with the standardized solution of 1000mg/L (in P), and the pH value is regulated by HCl or the NaOH solution of 1mol/L the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example to be put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL.Being diluted to corresponding suitable concentration) the pH value of modulation water solution system is 3-5, and absorption is 12 hours under room temperature, and maximum adsorption capacity (total P) is 600-900 μ g/g, and adsorption efficiency is 70%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g put into concentration is the arsenate solution of 80ng/mL 10mL, the pH value is 6 in the water, absorption is 12 hours under room temperature, maximum adsorption capacity is 9 μ g/g (total As), and adsorption efficiency is 64%.
Embodiment 2
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.25mol/L FeCl
2.4H
2O is 100mL airtight stirring and refluxing 12 hours in 60 ℃ of oil baths altogether, filters.
3. in 60 ℃ of water-baths, the inert atmosphere of nitrogen protection down on filter cake with the speed Dropwise 5 0mL25% strong aqua of 2 of per seconds and stirred one hour fast, generate the chocolate material, be washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, the pH value of modulation water solution system is 3-5, absorption is 12 hours under room temperature, and adsorption efficiency is 64%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 50%.
Embodiment 3
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.33mol/L FeCl
2.4H
2O is 100mL airtight stirring and refluxing 12 hours in 60 ℃ of oil baths altogether, filters.
3. in 60 ℃ of water-baths, the inert atmosphere of nitrogen protection down on filter cake with speed Dropwise 5 0mL 25% strong aqua of 2 of per seconds and stirred one hour fast, generate the chocolate material, be washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, the pH value of modulation water solution system is 3-5, absorption is 12 hours under room temperature, and adsorption efficiency is 62%
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 58%.
Embodiment 4
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.3mol/L FeCl
2.4H
2O is 100mL airtight stirring and refluxing 8 hours in 60 ℃ of oil baths altogether, filters.
3. in 60 ℃ of water-baths, the inert atmosphere of nitrogen protection down on filter cake with speed Dropwise 5 0mL 25% strong aqua of 2 of per seconds and stirred one hour fast, generate the chocolate material, be washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, adsorption efficiency is 61%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 54%.
Embodiment 5
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.3mol/L FeCl
2.4H
2O is 100mL airtight stirring and refluxing 14 hours in 60 ℃ of oil baths altogether, filters.
3. in 60 ℃ of water-baths, the inert atmosphere of nitrogen protection down on filter cake with the speed Dropwise 5 0mL25% strong aqua of 2 of per seconds and stirred one hour fast, generate the chocolate material, be washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
The composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, and adsorption efficiency is 60%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 53%.
Embodiment 6
1. select homemade BEAT nanosized zeolitic material 1g for use
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.25mol/L FeCl
2.4H
210mL is in having the teflon-lined stainless steel cauldron altogether for O, and reaction is 12 hours under the 333K autogenous pressure, is warmed up to 373K, reacts 12 hours.
3. inert atmosphere of nitrogen protection added 20mL 25% strong aqua down and reacted under 333K 12 hours again, is washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, the pH value of modulation water solution system is 3-5, absorption is 12 hours under room temperature, maximum adsorption capacity (total P) is 600-900 μ g/g, and adsorption efficiency is 83%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g put into concentration is the arsenate solution of 80ng/mL 10mL, the pH value is 6 in the water, absorption is 12 hours under room temperature, maximum adsorption capacity is 9 μ g/g (total As), and adsorption efficiency surpasses 74%.
Embodiment 7
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.29mol/L FeCl
2.4H
210mL is in having the teflon-lined stainless steel cauldron altogether for O, and reaction is 12 hours under the 333K autogenous pressure, is warmed up to 373K, reacts 12 hours.
3. inert atmosphere of nitrogen protection added 20mL 25% strong aqua down and reacted under 333K 12 hours again, is washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, adsorption efficiency is 61%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 54%.
Embodiment 8
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.33mol/L FeCl
2.4H
210mL is in having the teflon-lined stainless steel cauldron altogether for O, and reaction is 12 hours under the 333K autogenous pressure, is warmed up to 373K, reacts 12 hours.
3. inert atmosphere of nitrogen protection added 20mL 25% strong aqua down and reacted under 333K 12 hours again, is washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, adsorption efficiency is 63%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 53%.
Embodiment 9
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.25mol/L FeCl
2.4H
210mL is in having the teflon-lined stainless steel cauldron altogether for O, and reaction is 8 hours under the 333K autogenous pressure, is warmed up to 373K, reacts 12 hours.
3. inert atmosphere of nitrogen protection added 20mL 25% strong aqua down and reacted under 333K 12 hours again, is washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, adsorption efficiency is 65%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 50%.
Embodiment 10
1. select homemade BEAT nanosized zeolitic material 1g for use.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.25mol/L FeCl
2.4H
210mL is in having the teflon-lined stainless steel cauldron altogether for O, and reaction is 14 hours under the 333K autogenous pressure, is warmed up to 373K, reacts 12 hours.
3. inert atmosphere of nitrogen protection added 20mL 25% strong aqua down and reacted under 333K 12 hours again, is washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, adsorption efficiency is 64%
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 52%.
Embodiment 11
1. select the nanosized zeolitic material with BEAT zeolite different properties and pattern for use, X zeolite 1g.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.3mol/L FeCl
2.4H
2O airtight stirring in 60 ℃ of water-baths is spent the night, and filters.
3. in 60 ℃ of water-baths, the inert atmosphere of nitrogen protection dripped the 30mL25% strong aqua with the speed of 2 of per seconds down and stirred one hour fast on filter cake, generate the chocolate material, is washed to nearly neutrality then, 60 ℃ of dryings 5 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, maximum adsorption capacity is that 600 μ gP/g adsorption efficiencies are 67%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 52%.
Embodiment 12
1. select the nanosized zeolitic material with BEAT zeolite different properties and pattern for use, X zeolite 1g.
2. the FeCl that adds 0.5mol/L
3.6H
2O and 0.25mol/L FeCl
2.4H
2O is in having the teflon-lined stainless steel cauldron, and reaction is 12 hours under the 333K autogenous pressure, and little then loose kettle cover is warmed up to 373K, reacts 12 hours.
3. inert atmosphere of nitrogen protection added 30mL 25% strong aqua down and reacted under 333K 12 hours again, is washed to nearly neutrality then, 60 ℃ of dryings 2 hours.
4. the composite assembled material 0.05g of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example is put into the phosphorous Simulated Water solution that concentration is the 50 μ g/mL (total P) of 5mL, maximum adsorption capacity is that 600 μ gP/g adsorption efficiencies are 65%.
With the composite assembled material of the magnetic iron oxide/molecular sieve of Nano zeolite for preparing in the above-mentioned example, 0.05g puts into the arsenate solution that concentration is 80ng/mL 10mL, and the pH value is 6 in the water, and absorption is 12 hours under room temperature, and adsorption efficiency is 51%.
The present invention utilizes the externally-applied magnetic field of certain intensity, assemble, reclaim the composite assembled sorbing material of novel magnetic ferriferous oxide/molecular sieve of Nano zeolite that absorption reaches capacity, after be positioned in the 0.5mol/L NaOH solution, at room temperature, vibrated 12 hours, for the sorbing material after the desorb, the recirculation utilization, detailed process is as follows:
Get the 0.05g sorbent material and put into the phosphorous Simulated Water that concentration is 50 μ g/mL (total P) 5mL, the pH value is 3-5 in the water, absorption is 12 hours under room temperature, loading capacity is 843 μ g/g (total P), repeats with the loading capacity 900 μ g/g (total P) of original sorbing material under the same terms are basic.As get the 0.05g sorbing material and put into the arsenate solution that concentration is 80ng/mL 10mL, the pH value is 6 in the water, absorption is 12 hours under room temperature, and maximum adsorption capacity is 8.4 μ g/g, repeats substantially with the loading capacity 9 μ g/g of fresh sorbing material under the same terms.
Claims (4)
1, the composite assembled preparation method of a kind of magnetic iron oxide/molecular sieve of Nano zeolite is characterized in that concrete steps are as follows:
1. select nano level zeolite crystal material for use;
2. utilize the electrostatic attraction effect, by the fixing Fe that introduces of ion-exchange method
2+/ Fe
3+As follow-up active reaction sites;
3. dropwise add 25% strong aqua, make corresponding Fe
2+/ Fe
3+Chemical reaction takes place in avtive spot in alkaline medium, after through the washing, drying process, the composite assembled material of magnetic iron oxide/molecular sieve of Nano zeolite of making;
4. above-mentioned materials is utilized Dynamic gas-mixing and adsorption devices, phosphate radical, arsenate pollutent in the water are removed in absorption.
2, the composite assembled preparation method of magnetic iron oxide/molecular sieve of Nano zeolite according to claim 1 is characterized in that, described Fe
2+/ Fe
3+Avtive spot is meant the alumina negative potential that utilizes in the molecular sieve of Nano zeolite skeleton structure, utilizes the electrostatic attraction effect, by the Fe of ion-exchange method introducing
2+/ Fe
3+Avtive spot.
3, the composite assembled preparation method of magnetic iron oxide/molecular sieve of Nano zeolite according to claim 1 is characterized in that, described ion-exchange method by ion-exchange method, is introduced Fe in relevant nanometer zeolite molecular sieve skeleton structure
2+/ Fe
3+The operating process of avtive spot, utilize following dual mode to finish:
A: make the molecular sieve of Nano zeolite material place the Fe of 1: 2～2: 3 ratios
2+/ Fe
3+In the solution, 60 ℃ of oil bath reflux 8～14 hours, after filter fast;
B: with the Fe of molecular sieve of Nano zeolite material with 1: 2～2: 3 ratios
2+/ Fe
3+The solution thorough mixing is even, be placed on to have in the teflon-lined stainless steel autoclave, 60 ℃ the heating 8～14 hours closely dried to solution.
According to claim 1 or the composite assembled preparation method of 3 described magnetic iron oxide/molecular sieve of Nano zeolite, it is characterized in that 4, described ion-exchange method is by the fixing Fe that introduces of ion-exchange method
2+/ Fe
3+The molecular sieve of Nano zeolite material of avtive spot need be under the inert atmosphere of nitrogen protection, and dropwise ammoniacal liquor forms assembly.
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| CN109603785A (en) * | 2018-12-18 | 2019-04-12 | 安徽工业大学 | It is a kind of to remove arsenic, phosphorus adsorbent and preparation method thereof in water removal simultaneously |
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|---|---|---|---|---|
| SE8500668L (en) * | 1985-02-13 | 1985-12-02 | Lt Produkter Skutsker Ab | REGULATION AND CLEANING DEVICE AT AIRPORTS ORGANIZED IN THE SIDE WALL OF A PARK |
| JPH11300200A (en) * | 1998-04-24 | 1999-11-02 | Taiheiyo Tanko Kk | Absorptive filter medium consisting of zeolite ore |
| CN1087975C (en) * | 1998-07-17 | 2002-07-24 | 北京理工大学 | Catalyst for removing sulfur dioxide |
| CN1181911C (en) * | 2003-03-20 | 2004-12-29 | 复旦大学 | Preparation of zeolite modified flyash microbead assembled bodies for having affinity and separation of protein |
| WO2006059824A1 (en) * | 2004-12-01 | 2006-06-08 | Geoworks Co., Ltd. | Method of preparation of zeolite for re¬ mediating contaminated materials and method for remediating contaminated materials using thereof |
-
2006
- 2006-09-07 CN CNB2006100308997A patent/CN100391590C/en not_active Expired - Fee Related
Cited By (5)
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| CN102671641A (en) * | 2012-05-24 | 2012-09-19 | 上海交通大学 | Preparation and application for nanometer SiO2 strengthened calcium alginate-xanthan gum composite absorbent |
| CN103736449A (en) * | 2013-12-20 | 2014-04-23 | 中节能六合天融环保科技有限公司 | Method for preparing arsenic removal adsorbent from iron mud-coated zeolite and application |
| CN106268618A (en) * | 2016-08-31 | 2017-01-04 | 广州市市政集团有限公司 | A kind of preparation method and applications of active adsorbing material |
| CN109502603A (en) * | 2017-09-14 | 2019-03-22 | 北京化工大学 | A kind of magnetic molecule preparation method sieved and obtained magnetic molecule sieve |
| CN109603785A (en) * | 2018-12-18 | 2019-04-12 | 安徽工业大学 | It is a kind of to remove arsenic, phosphorus adsorbent and preparation method thereof in water removal simultaneously |
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| CN100391590C (en) | 2008-06-04 |
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