CN105174677A - Potassium ferrate slow-release composite material as well as preparation method and use thereof - Google Patents
Potassium ferrate slow-release composite material as well as preparation method and use thereof Download PDFInfo
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- CN105174677A CN105174677A CN201510700180.9A CN201510700180A CN105174677A CN 105174677 A CN105174677 A CN 105174677A CN 201510700180 A CN201510700180 A CN 201510700180A CN 105174677 A CN105174677 A CN 105174677A
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Abstract
The invention discloses a potassium ferrate slow-release composite material as well as a preparation method and use thereof, belonging to the technical field of environment protection. The preparation method of the potassium ferrate slow-release composite material comprises the following steps: firstly, uniformly stirring and mixing quartz sand with potassium ferrate powder, so as to form a quartz sand-potassium ferrate mixture; then adding the quartz sand-potassium ferrate mixture into molten paraffin while heating, rapidly stirring until the mixture is completely infiltrated by the molten paraffin, so as to form a quartz sand-potassium ferrate-paraffin mixture; finally, rapidly pouring the quartz sand-potassium ferrate-paraffin mixture into a mold when the mixture is hot, carrying out compaction, and cooling, so as to obtain the potassium ferrate slow-release composite material. The potassium ferrate slow-release composite material has the advantages of high utilization rate, good processing effect, low cost, long duration time, easiness in acceptation by the public and the like. The preparation method is simple, convenient and rapid, and the raw materials are low in cost and easily available; the potassium ferrate slow-release composite material has the multiple effects in the removal process of organic pollutants in bottom mud and is also nontoxic and harmless to the environment.
Description
Technical field
The invention belongs to environmental technology field, particularly a kind of potassium ferrate slow-releasing composite material and its production and use.
Background technology
Bed mud in water surrounding is the important component part of water ecosystem, is also carrier and the accumulation storehouse of various organism Transport And Transformation in water surrounding simultaneously.Along with the fast development of China's industrial or agricultural, unprocessed or deal with improperly the discharge of trade effluent, the discharge of waste gas, the excessive use of agricultural chemicals, the discharge of Vehicular exhaust, the burnings of solid waste etc. all create a large amount of organic pollutants, these pollutents enter water body by the approach such as atmosphere dried wet deposition and rainwash, are accumulated in bed mud greatly.Under certain conditions, the organic pollutant in bed mud may be transferred in water body, endangers the whole ecosystem.
The treatment technology of current bed mud organic pollutant mainly contains three kinds: physical treatment, chemical treatment and biological treatment.Physical treatment is the physical condition changing bed mud by project slash, comprises dredging, diversion and shelters.Although physical treatment has the advantage of instant effect, quantities is large, consumption wealth effort, and is difficult to make bed mud reach the requirement of cleanup standard.Biological treatment refers to the vital movement of microorganism of the plant that utilizes and cultivate or cultivation, inoculation, shifts, transforms and degrades, thus reach the object of repairing bed mud to the organic pollutant in bed mud.Its advantage be easy and simple to handle, few to ambient interference, cost is low, but is only suitable for the remedying sludge of big area, low stain load, and repair time is long, degradation process to a great extent by envrionment conditions as the impact of organic concentration, anoxic and low temperature.Compared to physics and biological treatment, in bed mud, add chemical agent carry out being oxidized the chemical treatment method of organic pollutant, then there is high, the easy and simple to handle and low cost and other advantages of instant effect, repair rate.Current chemical treatment method is at home and abroad used widely in sludge handling engineering.
Traditional chemical in situ treatment, is generally disposablely in Amounts of Mercury in Sediments, add the medicament such as oxygenant or flocculation agent, and repeatedly adds for a long time.But disposable add can cause that utilization ratio is low, action time is short, ecological damage, long-time running high in cost of production problem, therefore and be not suitable for the long-term disposal of bed mud organic pollutant.
Summary of the invention
The invention provides a kind of potassium ferrate slow-releasing composite material and its production and use.This slow-releasing composite material adopts potassium ferrate, paraffin and quartz sand three kinds of materials to make, wherein potassium ferrate is oxidative active ingredients, the coated object that can reach slow releasing potassium ferrate of paraffin, quartz sand then makes this slow-releasing composite material have certain physical strength.This material of definite shape is dropped in the bed mud of rivers and lakes, can slowly, the high ferro acid group of sustained release strong oxidizing property, be specially adapted to the removal of Organic Pollutants in Sedimentary Mud.
The technical solution adopted in the present invention is as follows:
A preparation method for potassium ferrate slow-releasing composite material, comprises the steps:
(1) quartz sand and potassium ferrate powder are uniformly mixed, form quartz sand-potassium ferrate mixture;
(2) under the condition of heating, quartz sand-potassium ferrate mixture step (1) prepared joins in the paraffin of fusing, and mixture all infiltrates by the paraffin being stirred to rapidly fusing, forms quartz sand-potassium ferrate-mineral wax mixture;
(3) quick quartz sand-potassium ferrate-mineral wax mixture step (2) prepared compacting in mould while hot, cooling, obtains potassium ferrate slow-releasing composite material.
The purity of the potassium ferrate powder in described step (1) is more than 90%.
Potassium ferrate powder in described step (1) and the mass ratio of quartz sand are 1:2-1:10.
Quartz sand in described step (1) is analytical pure, and its order number is 40-70 order.
Paraffin in described step (2) is paraffin wax, and its temperature of fusion is 54-56 DEG C.
Heating condition in described step (2) is heating in water bath, and the temperature of heating in water bath is 70 DEG C.
The mass ratio of described paraffin and quartz sand is 1:3-1:5.
In described step (3), mould is cylinder shape mould or cake mould.
The size range of described cylinder shape mould is φ 20mm × 50mm-φ 400mm × 1000mm; The size range of cake mould is φ 50mm × 10mm-φ 200mm × 40mm.
The potassium ferrate slow-releasing composite material utilizing aforesaid method to prepare, its shape is cylinder shape or cake type.
Above-mentioned potassium ferrate slow-releasing composite material is removing the application in the organic pollutant in bed mud.
First the quartz sand of certain order number and potassium ferrate are uniformly mixed in a reservoir, the method melted paraffin of heating in water bath is adopted again in water-bath, then the quartz sand potassium ferrate mixture mixed is poured into, rapid stirring makes melted paraffin all be infiltrated by mixture, pour compacting in mould fast into while hot again, cooling forming is potassium ferrate slow-releasing composite material.
Described potassium ferrate to be commercially available purity be more than 90% black powder reagent.
Described paraffin is paraffin wax, and temperature of fusion is 54-56 DEG C.
Described quartz sand is analytical pure, and order number is 40-70 order.
The mass ratio of described paraffin and quartz sand is between 1:3-1:5, and the mass ratio of potassium ferrate and quartz sand is between 1:2-1:10.
Described potassium ferrate slow-releasing composite material can be made into cylinder shape, is applicable to the rivers and lakes that bed mud is darker.After can accomplishing fluently the suitable cylindrical hole of size in advance in bed mud, this slow-releasing composite material is put into; Also can directly be inserted in bed mud.Cylinder shape potassium ferrate slow-releasing composite material can reach different depths on bed mud longitudinal section simultaneously, even processing organic pollutant, prevent the effect that lower floor's Organic Pollutants in Sedimentary Mud spreads to upper strata.
Described potassium ferrate slow-releasing composite material also can be made into cake type, is applicable to the rivers and lakes that bed mud is more shallow.This cake type slow-releasing composite material of suitable number is evenly thrown in riverbed or lakebed, can reach and carry out covering and the effect processing organic pollutant to bed mud top layer.
Potassium ferrate is a kind of novel High-efficient Water treatment agent, and its pH scope be suitable for is wide.Under acidity and alkaline condition, its redox potential is respectively+2.20V and+0.72V, higher than conventional oxygenant as chlorine, hypochlorous acid, ozone, hydrogen peroxide, potassium permanganate etc., therefore has strong oxidizing property.Novel strong oxidizer potassium ferrate is carried in slow-releasing composite material, make its slowly, sustained release potassium ferrate, be a kind of novel method of chemical in-situ treatment bed mud organic pollutant.
The principle of process Organic Pollutants in Sedimentary Mud of the present invention is as follows:
The constituent material of potassium ferrate slow-releasing composite material is paraffin, quartz sand and potassium ferrate.Paraffin is as the coated oxidative active ingredients potassium ferrate of coated material, and quartz sand then plays whole material as skeletal support, makes this slow-releasing composite material have certain physical strength.
Ferric acid Potassium release is a diffusion process along concentration difference.When slow-releasing composite material contacts with water, the potassium ferrate concentration of solid-liquid interface both sides is different thus produce concentration difference, and first the potassium ferrate on slow-releasing composite material top layer is released and diffuses into liquid phase.After outer field potassium ferrate is released, its original position produces hole, the water molecules in liquid phase environment along hole gradually ecto-entad enter the inside of slow-releasing composite material, thus impel inner potassium ferrate to spread gradually from inside to outside.But because paraffin has coating function to potassium ferrate, the potassium ferrate of internal layer can be subject to friction resistance to during external diffusion simultaneously, and diffusion length is longer, resistance is larger, therefore determining ferric acid Potassium release with diffusion is not a rapid and temporary transient process, but one slowly and the process continued.
The potassium ferrate that slow sustained release goes out contacts with the organic pollutant in bed mud, is oxidized to CO
2, H
2o, NO
3 -, PO
4 3-deng mineral products, thus reach the object removing organic pollutant.
While high ferro acid group oxidation of organic compounds, self be reduced to the ferric ion of lower valency.Ferric ion can with sediment release or phosphate anion that high ferro acid group oxidation of organic compounds produces form tertiary iron phosphate and precipitate, reduce the phosphate content in bed mud and overlying water.Reaction equation is as follows:
Fe
3++PO
4 3-=FePO
4↓(1)
Secondly, ferric ion hydrolyzable produces ironic hydroxide flock, is removed the phosphoric in overlying water by reactions such as absorption, coagulation and complexings, simultaneously also can purifying water body.Flock is deposited on bed mud top layer, can form the cotton-shaped film of one deck and cover bed mud, suppress it to release phosphorus further, the eutrophication of anti-water-stop body.
In addition, potassium ferrate also can react with water and produce oxygen, and reaction equation is as follows:
2FeO
4 2-+5H
2O=2Fe(OH)
3+4OH
-+3/2O
2↑(2)
The oxygen produced can increase the dissolved oxygen in bed mud and overlying water, for aerobic microbiological creates good life condition, the population quantity of amplification aerobic microbiological, impels it more efficiently to decompose organic pollutant in bed mud, improves the water body self-purification ability of rivers and lakes.
The present invention is compared to the material of traditional chemical in-situ treatment bed mud and method, and its advantage is:
(1) the present invention adopts slow-releasing composite material supported active medicament potassium ferrate, compared to the disposable method adding chemical agent of tradition, has the advantages such as utilization ratio is high, treatment effect good, cost is low, the time length is long, the public easily accepts.Traditional chemical in situ treatment, no matter add oxygenant or flocculation agent, be all repeatedly throw in for a long time, easily cause that topical agent utilization ratio is low, any excess drug affects environmental ecology, the single delivering medicament time length is short, long-time running cost is high thus and the public such as not easily to accept at the problem.And the present invention adopts slow-releasing composite material, avoiding the problems such as the medicament utilization ratio caused because once adding is not high, organism treatment effect is bad, slow, the sustained release of medicament can be reached.This slow-releasing composite material of disposable input, can reduce and even eliminate long-time running cost, is also easy to the public simultaneously and accepts, be suitable for the long-term disposal of organic pollutant in Amounts of Mercury in Sediments.
(2) the present invention adopts novel environment friendly oxygenant potassium ferrate, can reach the effect of " medicine is multiplex ", simultaneously nontoxic to environment.Potassium ferrate is as the organic pollutant in reactant oxidation bed mud, its reduzate ferric ion can be combined with phosphate anion as new reactant again and to precipitate, or produce ironic hydroxide flock absorption and coagulation phosphoric and bed mud top layer is covered, prevent body eutrophication, achieve the circulation that reaction product becomes new reaction thing again, " medicine is multiplex ".Heavy metal free pollutes simultaneously, belongs to environmentally friendly medicament.
(3) the present invention can realize the associated treatment to bed mud organic chemical contaminant and biological process.Potassium ferrate can react with water and produce oxygen, add dissolved oxygen, facilitate the degraded of aerobic microbiological to organic pollutant, therefore, add the effect that this potassium ferrate slow-releasing composite material can reach chemical process and biological method associated treatment Organic Pollutants in Sedimentary Mud.
(4) preparation method of the present invention is simple and efficient, and cheaper starting materials is easy to get.
Accompanying drawing explanation
Fig. 1 is the ferro element concentration release profiles of S1-S3 tri-groups in embodiment 1.
Fig. 2 is the ferro element concentration release profiles of G4 group in embodiment 2.
Fig. 3 is G1-G5 five groups ferro element rate of release in early stage and potassium ferrate initial mass graph of a relation in embodiment 2.
Embodiment
Below in conjunction with accompanying drawing 1-3 and embodiment, technical scheme of the present invention is specifically addressed.
The purity of the potassium ferrate that following examples are used is more than 90%; Quartz sand used is its order number of analytical pure is 40-70 order; Paraffin in described step (2) is paraffin wax, and its temperature of fusion is 54-56 DEG C.
Embodiment 1
The quality of fixing paraffin and potassium ferrate is respectively 2g and 4g.
Take 6g, 8g, 10g quartz sand respectively, it is joined respectively and fills in the container of potassium ferrate, be uniformly mixed.The beaker filling paraffin is heated in 70 DEG C of thermostat water baths, after paraffin all melts, pour the quartz sand potassium ferrate mixture mixed into, be stirred to mixture all to be infiltrated by paraffin, pour compacting in the cylinder shape mould of φ 20mm × 50mm while hot fast into, take out after its cooling forming, namely the potassium ferrate slow-releasing composite material that obtained quartz sand content is different, is numbered slow-releasing composite material S1 (6g quartz sand), S2 (8g quartz sand), S3 (10g quartz sand).
This slow-releasing composite material containing different mass quartz sand for checking has slow release effect, monitors the ferro element rate of release of potassium ferrate slow-releasing composite material by experiment continuously.In three containers, inject 1.5L deionized water respectively, S1-S3 tri-groups of slow-releasing composite materials are dropped in three containers respectively, airtight lucifuge room temperature preservation, sampling every day (during sampling, disturbance solution, makes the iron hydroxide of suspension also can be obtained).Get 2mL sample inject colorimetric cylinder, add (1+1) hydrochloric acid (massfraction be 37.5% concentrated hydrochloric acid and deionized water equal-volume mixed configuration form, concentration 12.1mol/L.Lower same.) produce to sample bubble-free, add one again, add 1mL100g/L oxammonium hydrochloride, 2mL1.5g/L phenanthroline and 5mL1mol/L sodium acetate soln afterwards successively, shake up rear standing 10min, with ultraviolet spectrophotometer in 510nm place working sample absorbance, try to achieve the iron level in institute's water sampling.Set up the relation of total iron content and time in water.Three groups of potassium ferrate slow-releasing composite material ferro element concentration release profiles as shown in Figure 1.
Monitoring result shows, and in 100h, the ferro element concentration of slow-releasing composite material release substantially linearly increases, and during 100h, S1-S3 tri-groups of potassium ferrate burst sizes account for 1.3%, 1.9% and 2.2% of total amount respectively.Meanwhile, under the condition of fixing potassium ferrate mass conservation, in slow-releasing composite material, initial quartz sand quality is larger, then the total concentration of iron discharged is larger.Illustrate thus, the slow-releasing composite material containing different mass quartz sand reaches the slow releasing of potassium ferrate medicament really.
Embodiment 2
Fixing paraffin and quartz sand quality are respectively 2g and 10g.
Take 1g, 2g, 3g, 4g, 5g potassium ferrate respectively, it is joined respectively and fills in the container of quartz sand, be uniformly mixed.Beaker 70 DEG C of heating in water bath in thermostat water bath of paraffin will be filled, after paraffin all melts, pour the quartz sand potassium ferrate mixture mixed into, be stirred to mixture all to be infiltrated by paraffin, pour compacting in the cylinder shape mould of φ 20mm × 50mm while hot fast into, take out after its cooling forming, i.e. the obtained potassium ferrate slow-releasing composite material containing different mass potassium ferrate.Get and be numbered G1 (1g potassium ferrate), G2 (2g potassium ferrate), G3 (3g potassium ferrate), G4 (4g potassium ferrate), G5 (5g potassium ferrate).
This slow-releasing composite material containing different mass potassium ferrate for checking has slow release effect, monitors the iron rate of release of potassium ferrate slow-releasing composite material by experiment continuously.In five containers, inject 1.5L deionized water respectively, G1-G5 five groups of slow-releasing composite materials are dropped in corresponding container respectively, airtight lucifuge room temperature preservation, sampling every day (during sampling, disturbance solution, makes the iron hydroxide of suspension also can be obtained).Get 2mL sample and inject colorimetric cylinder, add (1+1) hydrochloric acid to produce to sample bubble-free, add one again, add 1mL100g/L oxammonium hydrochloride, 2mL1.5g/L phenanthroline and 5mL1mol/L sodium acetate soln afterwards successively, shake up rear standing 10min, with ultraviolet spectrophotometer in 510nm place working sample absorbance, try to achieve the iron level in institute's water sampling.Set up the relation of total iron content and time in water.
For G4 slow-releasing composite material, monitoring data shows (as shown in Figure 2), and in early stage 200h, the ferro element concentration of slow-releasing composite material release substantially linearly increases, and reduces gradually to later stage ferro element rate of release, and concentration increases slower.When 885h, potassium ferrate burst size accounts for 5.7% of total amount.Illustrate thus, the slow-releasing composite material containing different mass potassium ferrate reaches the object of potassium ferrate medicament slow releasing really.
By the monitoring result comparing five groups of potassium ferrate slow-releasing composite materials known (rate of release and potassium ferrate initial mass relation are as shown in Figure 3), in slow-releasing composite material, potassium ferrate initial mass is larger, the ferro element concentration then recorded is larger, and early stage, rate of release became certain linear relationship with potassium ferrate initial mass.Can find out, different material compositions, can control the speed of potassium ferrate slow-releasing composite material release potassium ferrate.
Embodiment 3
In bed mud, organic components is complicated, huge number, and the present embodiment selects organic pollutant trieline (TCE) that is comparatively common and easily its content of mensuration as the handling object of potassium ferrate slow-releasing composite material.In view of the numerous not easily single mensuration of organism kinds in bed mud and the needs safeguarding determining instrument, be therefore subject to the Amounts of Mercury in Sediments of Organic pollutants with the aqueous solution simulation containing TCE, probe into the treatment effect of potassium ferrate slow-releasing composite material to TCE.
Taking 2.5g potassium ferrate powder input 250mLTCE starting point concentration is in the Erlenmeyer flask of 20mg/L, and stirring reaction in magnetic stirring apparatus also gets a sample every 1h, remains content with high effective liquid chromatography for measuring TCE.Experimental result display 1.5h clearance is 15%, 2.5h clearance is 33%, illustrates that potassium ferrate has treatment effect to TCE really.
Fixing paraffin and quartz sand quality are respectively 1g and 5g.
Take 0.5g, 1g, 1.5g, 2g, 2.5g potassium ferrate respectively, it is joined respectively and fills in the container of quartz sand, be uniformly mixed.Beaker 70 DEG C of heating in water bath in thermostat water bath of paraffin will be filled, after paraffin all melts, pour the quartz sand potassium ferrate mixture mixed into, be stirred to mixture all to be infiltrated by paraffin, pour compacting in the cylinder shape mould of φ 20mm × 50mm while hot fast into, take out after its cooling forming, be the potassium ferrate slow-releasing composite material containing different potassium ferrate content, get and be numbered R1 (0.5g potassium ferrate), R2 (1g potassium ferrate), R3 (1.5g potassium ferrate), R4 (2g potassium ferrate), R5 (2.5g potassium ferrate).
In five containers, add TCE saturated aqueous solution and deionized water respectively, making its cumulative volume be 1.5L, TCE starting point concentration is 20mg/L.R1-R5 five groups of slow-releasing composite materials are dropped in corresponding container respectively, blank experimental group is set simultaneously.Six groups of container closure lucifuge room temperature preservation, every day, sampling and measuring TCE remained content.Experimental result display blank group TCE concentration is substantially unchanged, and five groups of experimental group TCE concentration slowly decline, and this potassium ferrate being slow-releasing composite material discharges progressively is oxidized caused by TCE.Also find, the slow-releasing composite material process TCE speed containing potassium ferrate initial mass larger (i.e. R4, R5) is faster simultaneously.
To sum up, potassium ferrate can rapid oxidation TCE, simultaneously slow-releasing composite material can continue, slow releasing active agents potassium ferrate, the effect of long-term disposal Organic Pollutants in Sedimentary Mud can be reached.
Claims (10)
1. a preparation method for potassium ferrate slow-releasing composite material, is characterized in that comprising the steps:
(1) quartz sand and potassium ferrate powder are uniformly mixed, form quartz sand-potassium ferrate mixture;
(2) under the condition of heating, quartz sand-potassium ferrate mixture step (1) prepared joins in the paraffin of fusing, and mixture all infiltrates by the paraffin being stirred to rapidly fusing, forms quartz sand-potassium ferrate-mineral wax mixture;
(3) quick quartz sand-potassium ferrate-mineral wax mixture step (2) prepared compacting in mould while hot, cooling, obtains potassium ferrate slow-releasing composite material.
2. the preparation method of a kind of potassium ferrate slow-releasing composite material according to claim 1, is characterized in that: the purity of the potassium ferrate powder in described step (1) is more than 90%; Quartz sand is analytical pure, and its order number is 40-70 order.
3. a kind of preparation method of potassium ferrate slow-releasing composite material according to claim 1 or 2, is characterized in that: the potassium ferrate powder in described step (1) and the mass ratio of quartz sand are 1:2-1:10.
4. the preparation method of a kind of potassium ferrate slow-releasing composite material according to claim 1, it is characterized in that: the paraffin in described step (2) is paraffin wax, its temperature of fusion is 54-56 DEG C.
5. a kind of preparation method of potassium ferrate slow-releasing composite material according to claim 1 or 2, it is characterized in that: the heating condition in described step (2) is heating in water bath, the temperature of heating in water bath is 70 DEG C.
6. a kind of preparation method of potassium ferrate slow-releasing composite material according to claim 1 or 4, is characterized in that: the mass ratio of described paraffin and quartz sand is 1:3-1:5.
7. a kind of preparation method of potassium ferrate slow-releasing composite material according to claim 1 or 2 or 4, is characterized in that: in described step (3), mould is cylinder shape mould or cake mould.
8. the preparation method of a kind of potassium ferrate slow-releasing composite material according to claim 7, is characterized in that: the size range of described cylinder shape mould is φ 20mm × 50mm-φ 400mm × 1000mm; The size range of cake mould is φ 50mm × 10mm-φ 200mm × 40mm.
9. utilize a potassium ferrate slow-releasing composite material prepared by method described in any one of claim 1-8, its shape is cylinder shape or cake type.
10. potassium ferrate slow-releasing composite material according to claim 9 is removing the application in Organic Pollutants in Sedimentary Mud.
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CN106430365B (en) * | 2016-11-28 | 2019-11-12 | 辽宁石油化工大学 | A kind of Zero-valent Iron activator sustained release candle for in-situ remediation of underground water |
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