CN106277672B - A kind of preparation method and application of Phosphorus Exchange at Sediment-water Interface release control material - Google Patents
A kind of preparation method and application of Phosphorus Exchange at Sediment-water Interface release control material Download PDFInfo
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- CN106277672B CN106277672B CN201610797808.6A CN201610797808A CN106277672B CN 106277672 B CN106277672 B CN 106277672B CN 201610797808 A CN201610797808 A CN 201610797808A CN 106277672 B CN106277672 B CN 106277672B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/008—Sludge treatment by fixation or solidification
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
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Abstract
The present invention provides the preparation methods and application of a kind of Phosphorus Exchange at Sediment-water Interface release control material, the material is initiatively using lake sediment and kaolin mixture as base stock, through treatment processes such as oxidation, modification with Fe, granulation and roastings, material is significantly reduced to phosphatic adsorption-desorption equilibrium concentration EPC0Value, improves its linear distribution factor KdValue, so that material of the invention can effectively cut down sediment interstitial water phosphate concn, inhibit the release of Phosphorus Exchange at Sediment-water Interface hydrochlorate, since the phosphatic desorption ability of material itself is weaker, adsorption capacity and buffer capacity are relatively strong, therefore material of the present invention can really realize effective resistance control to Phosphorus Exchange at Sediment-water Interface release.And material materials of the invention are cheap, and social and economic benefits and good is highly-safe, does not have ecological risk to water body in lake, energy conservation and environmental protection releases the control significant effect to Dian Chi difference lake region Phosphorus Exchange at Sediment-water Interface in application process.
Description
Technical field
The present invention relates to the preparation methods and application of a kind of Phosphorus Exchange at Sediment-water Interface release control material, belong to water environment
Contamination control field.
Background technique
Over nearly more than 30 years, due to the development of social economy and the influence of mankind's activity, a large amount of xenobiotic pollutants enter lake
It moors and is enriched in deposit, be stained significantly China's majority lake surface sediments.The survey showed that, and many lakes are especially
The substrate pollution of urban lakes is surprising, such as Taihu Lake, Dian Chi, total phosphorus content is up to 3000- in many waters deposits in Chaohu
4000mg/kg.Deposit is not only the important home to return to and accumulation library of pollution of water object, but also is the weight of overlying water pollution
Want endogenous, this is because there is the homeostasis process of sedimentation absorption and desorption release, water bodys between deposit and overlying water
In phosphorus concentration be heavily dependent on the movement of this dynamic equilibrium, that is to say, that sediment phosphorus migration and release are depended on
In on the horizontal or vertical direction of column shaped deposit between adjacent two layers Interstitial Water concentration gradient.In same vertical section, when upper
When surface sediments Interstitial Water phosphorus concentration is higher than lower layer, Phosphorus in Sediments hydrochlorate between high concentration region to vertically expanding between low concentration region
It dissipates, forms the trend that phosphate is migrated from surface deposit to layer deposition object.On the contrary, when seabed sediment Interstitial Water phosphorus is dense
When degree is higher than upper layer, phosphate is then migrated from layer deposition object to surface deposit.Under normal conditions, sediment interstitial water phosphoric acid
Salinity is higher than overlying water phosphate concn, it is considered that, it just may cause water when the concentration of phosphorus reaches 0.02mg/L in water body
Body eutrophication.Therefore, sediment interstitial water phosphate concn is effectively cut down, control sediment phosphorus hydrochlorate is to overlying water diffusion
The important content of eutrophic lake internal loading control.
Improvement and reparation to eutrophication water quality focus mostly in reduction external loadings, and in the release of Phosphorus in Sediments i.e.
Source phosphorus discharges the actual effect that can but delay or offset above-mentioned measure, so the premise being effectively controlled in external pollution sources
Under, the research of deposit internal loading becomes the key of pollution control of water.Soverlay technique in situ is current control internal loading
One of effective measures, because it is good on endogenous contamination control effect and on water ecological setting influence it is smaller due to receive extensive pass
Note.The core of soverlay technique in situ is the selection of covering material, has untainted bed mud, clear using more covering material at present
Clean river sand, gravel, calcium bentonite, lime-ash, artificial zeolite, cement, there are also such as calcite, flyash, geotextile or one
A little complicated artificial foundation materials etc..For example, Chinese patent literature CN102775030A disclose it is a kind of using clean water sludge as
The method of covering material, this method by dewatered clean water sludge is dry, pulverize, be sieved, then at 500-600 DEG C of temperature
Lower calcination, obtains regenerated clean water sludge.Regenerated clean water sludge by being covered on the pollution bottom of water body to be repaired by the technology
Above mud so that polluted bed mud with overlying water is physical separates, on the one hand inhibit polluted bed mud endogenous pollution releasing to water body
It puts, the inorganic particle substance based on metal oxide contained in another aspect clean water sludge can also be to the nitrogen phosphorus etc. in water body
Polluter generates absorption, accelerates migration of the polluter in water body to bed mud, can be realized counterweight to a certain extent
The water remediation of polluted river channel.
But above-mentioned technology using waterworks clean water sludge as covering material, the introducing of this allogene to water body and
There are certain ecological risks for speech, and since the phosphate concn in water body is much smaller than the phosphate concn in clean water sludge,
Thus the phosphate in clean water sludge necessarily can also be migrated to water body, cause above-mentioned covering material to the logical of its overlying water release phosphorus
Amount is big, thus the technology may not effectively remove the phosphorus in water body, that is to say, the prior art can not still be covered using in situ
Lid technology really realizes the reparation to polluted water body, this is a technology urgently to be resolved to those skilled in the art
Problem.
Summary of the invention
Technical problem to be solved by the present invention lies in overcome the prior art using clean water sludge as present in covering material
Material ecological risk itself is high, the defects of phosphorus release risk is big, and then provide a kind of materials cheap, highly-safe, practicability
By force and there is the preparation method of the Phosphorus Exchange at Sediment-water Interface release control material of stronger removal effect to low phosphorus hydrochlorate and answer
With.
For this purpose, the present invention realizes above-mentioned purpose technical solution are as follows:
A kind of preparation method of Phosphorus Exchange at Sediment-water Interface release control material, comprising:
(1) lake sediment is acquired, it is freeze-dried, it is ground up, sieved, obtains deposition powder, it is spare；
(2) kaolin is taken, through drying, is ground up, sieved, kaolin powder is obtained, it is spare；
(3) the deposition powder and the kaolin powder are uniformly mixed and form mixed powder, it is spare；
(4) oxidation processes are carried out to the mixed powder, then dried, it is spare；
(5) processing is modified to the mixed powder after step (4) oxidation using iron salt solutions, then dried, it is spare；
(6) step (5) modified mixed powder is added into water infiltration, then extrusion forming, moulding material are fired processing
Afterwards up to Phosphorus Exchange at Sediment-water Interface release control material.
In the step (3), the quality of the kaolin powder accounts for the 10%-90% of the mixed powder gross mass, excellent
It is selected as 40%-60%, more preferably 50%.
The granularity of the deposition powder and the kaolin powder is not less than 100 mesh.
5molL is used in step (4)-1HNO3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3
The mass ratio of aqueous solution and the mixed powder is 50:1.
Iron salt solutions described in step (5) are 0.20molL-1FeSO4Aqueous solution, the FeSO4Aqueous solution and institute
The mass ratio for stating mixed powder is 100:1.
In step (6), the temperature of the calcination process is 120-800 DEG C, preferably 120-700 DEG C, more preferably 700
℃；The time of the calcination process is 0.5-3h, preferably 1h.
In step (6), the additive amount of water accounts for the 5-30wt% of the mixed powder quality, preferably 10wt%.
The Phosphorus Exchange at Sediment-water Interface release control material is the particle with 3-5mm partial size.
Phosphorus Exchange at Sediment-water Interface release control material is as deposit situ capping materials as made from above-mentioned preparation method
Purposes.
The Phosphorus Exchange at Sediment-water Interface release control material is laid on to the surface of contaminated sediment remediation, Polluted water area
Every square metre of contaminated sediment remediation corresponding to the every reduction 0.10mg/L of the content of surface deposit total phosphorus is annual required
The dosage of the Phosphorus Exchange at Sediment-water Interface load control system material is 0.23-19.71kg；
Phosphate concn in the Interstitial Water of the contaminated sediment remediation is 0.02-1.0mg/L.
Above-mentioned technical proposal of the invention has the advantage that
1, the preparation method of Phosphorus Exchange at Sediment-water Interface release control material of the present invention, it is contemplated that lake sediment
With dual role, it is both " remittance " of phosphorus and " source " of phosphorus, since the source-sink transition process of deposit is difficult to control, especially
, when the initial phosphate concentration in water body is lower, deposit can show to lead to using heavy phosphorus " negative absorption " phenomenon for it
There is the phosphate entrained by material itself can cover water-soluble risk out upwards as phosphorus controlled-release material for product object, easily causes water
The secondary pollution of body, ecological security is poor, this is also exactly that the prior art can not directly prepare phosphorus control using lake sediment
Material reason for it is released, and in order to overcome drawbacks described above, the present invention is for the first time basic with deposit and kaolinic mixture
Raw material, successively after oxidation, modification with Fe and calcination process, being formed a kind of as shown in Figure 1 has lower absorption-desorption balance
Concentration (EPC0) and higher distribution coefficient (Kd) Phosphorus Exchange at Sediment-water Interface release control material.Research has shown that, EPC0It is worth and heavy
The relative size of product object-water termination soluble phosphate (SRP) content determines phosphatic migratory direction, EPC0Be worth it is smaller,
Show that the flux for discharging phosphorus to overlying water from material is also smaller, and KdIt is gentle to phosphatic adsorption strength that value then reflects material
Rush ability, KdValue is bigger, shows that material is stronger to phosphatic buffer capacity, adsorption strength is also bigger, is less susceptible to that phosphorus occurs
Desorption.It can be seen that Phosphorus Exchange at Sediment-water Interface release control material of the present invention can really be realized to deposit-
Effective resistance control of water termination phosphorus release, thus solves covering material in the prior art and ignores because pursuing phosphorus adsorbance simply
Caused by material itself phosphorus burst size is big the problem of can not effectively controlling sediment phosphorus endogenous pollution.
In particular, preparation method of the present invention by using kaolin as phosphorus release control material raw material it
One, the characteristic that on the one hand aluminium oxide of high-content in kaolin can be utilized strong to phosphatic large amount of adsorption, crystallized ability, significantly
The adsorption-desorption equilibrium concentration for reducing material itself, improves distribution coefficient, to be advantageously implemented between lake sediment
Effective control of the phosphatic removal of low concentration and Phosphorus Exchange at Sediment-water Interface release in gap water；On the other hand certainly using kaolin
The caking property of body is to ensure the molding of phosphorus release control material；The third aspect is drawn materials cheap, highly-safe, practical using kaolin
The strong feature of property, can reduce the production cost and ecological risk of phosphorus release control material.In addition, preparation method of the present invention
By carrying out oxidation and modification to mixed raw material, then cooperates high-temperature roasting, thus can greatly improve active iron oxygen in material
The content of compound, to promote material to phosphatic adsorption capacity and adsorption strength, to be more advantageous to realization to sediment-water
Effective control of interface phosphorus release.
2, the preparation method of Phosphorus Exchange at Sediment-water Interface release control material of the present invention, preferably optimum calcination temperature
It is 700 DEG C, the carbonate and organic matter that can not only be removed the moisture in deposit hole in this way and be adsorbed on deposit increase
The big porosity and specific surface area of deposit, is conducive to improve deposit to the adsorption capacity of phosphorus, and can also activated deposition
The phosphorus of more difficult movement in object, subsequent deposit are fixed the phosphorus of activation once again by the way that a degree of Mineral Transformation occurs,
Advantageously reduce the internal loading amount of sediment phosphorus.
3, the preparation method of Phosphorus Exchange at Sediment-water Interface release control material of the present invention, by making mixed powder
Grain is shaped to the particle that partial size is 3-5mm, then by material-paving of the invention after contaminated deposit surface, can be effective
Reduce bottom water body answers the disturbance of shear force and water body flow to deposit, and then the phosphorus for advantageously reducing sediment resuspension is released
It puts.
4, the preparation method of Phosphorus Exchange at Sediment-water Interface release control material of the present invention, final material pair obtained
0.02-1.0mg/L sediment interstitial water removal rate of phosphate has reached 80%-98%；For Dian Chi difference lake region deposit, open
Show an insitu analog lake sediment-water interface phosphorus release process, after simulation test 90 days, control of material group overlying water total phosphorus
Concentration reduces 7 to 36 times than control group, and material covering control group Phosphorus Exchange at Sediment-water Interface burst size is cut than control group as a result,
73%-97% is subtracted.
By taking Caohai of Dianchi Lake as an example, the content of surface deposit total phosphorus (TP) is 0.30mg/L, sediment-water in water body at present
The release iron of interface solubility total phosphorus (DTP) is 1.091mg/ (m2D), then TP value to be made to be reduced to 0.20mg/L, if
The further conversion that phosphorus is moved in deposit is not considered, then the amount that 1 year domestic demand adds material of the present invention is
0.23Kg/m2If considering that removable phosphorus largely enters whole mineralisings during entire biogeochemical cycle above to cover
In water body, then it is 19.71Kg/m that 1 year domestic demand, which adds the amount of material of the present invention,2.As it can be seen that by will be of the present invention
Material-paving can be realized effective resistance control to Phosphorus Exchange at Sediment-water Interface release in contaminated deposit surface.
Detailed description of the invention
It, below will be in specific embodiment in order to illustrate more clearly of the technical solution in the specific embodiment of the invention
The required attached drawing of description be briefly described, it should be apparent that, the accompanying drawings in the following description is of the invention some
Embodiment for those of ordinary skill in the art without creative efforts, can also be according to these
Attached drawing obtains other attached drawings.
Fig. 1 is control material of the present invention to phosphatic absorption-desorption curve graph；
Fig. 2 is control material of the present invention to phosphatic adsorption-desorption equilibrium concentration (EPC0) and distribution coefficient
(Kd) with the curve graph of kaolin percentage variation in material；
Fig. 3 a~3f respectively represents maturing temperature and is followed successively by 120 DEG C, 200 DEG C, 300 DEG C, 450 DEG C, 550 DEG C of 700 DEG C of when systems
The curve graph that standby control material changes phosphatic removal rate with initial phosphate concentration；
Fig. 4 a~4d respectively corresponds the live insitu analog condition material in experimental group 1~4 and releases Phosphorus Exchange at Sediment-water Interface
Put control effect figure.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
In addition, technical characteristic involved in invention described below different embodiments is as long as they do not conflict with each other
It can be combined with each other.
Deposition feedstock in following embodiments picks up from Dian Chi 24 ° 53 ' 55.31 " N and 102 ° 40 ' 35.92 " E, with Dian Chi
The quality meter of deposit, the loss on ignition of the Phosphorus in Sediment of Dianchi Lake are 20.23wt%, are contained in the Phosphorus in Sediment of Dianchi Lake
The SiO of 30.07wt%2, 23.93wt% Al2O3, 20.51wt% Fe2O3, 0.32wt% CaO, 0.93wt% MgO,
The Na of 0.18wt%2O, the K of 3.08wt%2The TiO of O and 0.75wt%2；
Kaolin is purchased from Zhengzhou West Germany benefit chemical plant；
Muffle furnace is purchased from Germany's Na Bore Muffle furnace, model: L5/11/P330+.
Embodiment 1
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be not less than 100 mesh deposition
Powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, it is spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 10wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
5wt% is then squeezed into graininess, and molding mass obtains the Phosphorus Exchange at Sediment-water Interface that partial size is 3-5mm in 120 DEG C of roasting 2h
Release control material.
Embodiment 2
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 150~200 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 150~200 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 80wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
10wt% is then squeezed into graininess, and molding mass obtains the water/sediment interface that partial size is 3-4mm in 200 DEG C of roasting 3h
Phosphorus release control material.
Embodiment 3
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 120~300 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 120~300 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 70wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
15wt% is then squeezed into graininess, and molding mass obtains the water/sediment interface that partial size is 3-4mm in 300 DEG C of roasting 1h
Phosphorus release control material.
Embodiment 4
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 100~300 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 100~300 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 60wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
20wt% is then squeezed into graininess, and molding mass obtains sediment-water circle that partial size is 4-5mm in 450 DEG C of roasting 1.5h
Face phosphorus release control material.
Embodiment 5
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 100~200 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 100~200 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 50wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
20wt% is then squeezed into graininess, and molding mass obtains the water/sediment interface that partial size is 3-4mm in 700 DEG C of roasting 1h
Phosphorus release control material.
Embodiment 6
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 100~250 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 100~250 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 40wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
15wt% is then squeezed into graininess, and molding mass obtains the water/sediment interface that partial size is 3-5mm in 550 DEG C of roasting 1h
Phosphorus release control material.
Embodiment 7
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 150~200 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 150~200 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 30wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
30wt% is then squeezed into graininess, and molding mass obtains sediment-water circle that partial size is 3-4mm in 700 DEG C of roasting 0.5h
Face phosphorus release control material.
Embodiment 8
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 100~200 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 100~200 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 20wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
15wt% is then squeezed into graininess, and molding mass obtains the water/sediment interface that partial size is 3-4mm in 800 DEG C of roasting 1h
Phosphorus release control material.
Embodiment 9
Phosphorus Exchange at Sediment-water Interface release control material described in the present embodiment is prepared by the following method:
(1) acquisition bottom mud in lake be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be 150~200 purposes sink
Product powder, it is spare；Kaolin is taken, through drying, is ground up, sieved, obtaining granularity is 150~200 mesh kaolin powders, spare；
(2) the deposition powder and kaolin powder are thoroughly mixed to form mixed powder, the kaolin in proportion
Dosage account for the 90wt% of mixed powder gross mass, it is spare；
(3) HNO of 5mol/L is utilized3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution and institute
The mass ratio for stating mixed powder is 50:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to room temperature；
Then the FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing to oxidized mixed powder, described
FeSO4The mass ratio of aqueous solution and the mixed powder is 100:1, and is placed in air dry oven and is evaporated, and taking-up is cooled to
Room temperature is spare；
(4) step (3) modified mixed powder is added into water infiltration, the additive amount of water accounts for the mixed powder quality
10wt% is then squeezed into graininess, and molding mass obtains sediment-water circle that partial size is 4-5mm in 700 DEG C of roasting 0.5h
Face phosphorus release control material.
Experimental example
The present invention is respectively provided with absorption-desorption experiment and the experiment of water/sediment interface scene in-situ control, to investigate this
Invent the using effect of Phosphorus Exchange at Sediment-water Interface release control material obtained.
1, absorption-desorption is tested
Configuration is that 0~1.0mg/L (is respectively set close to sediment interstitial water phosphorus concentration range under the natural conditions of lake
For the water sample of 0,0.02,0.05,0.10,0.20,0.30,0.50 and 1.0mg/L)；Material dry sample 0.5g is weighed to be centrifuged in 100mL
Guan Zhong is separately added into the water sample solution of the above-mentioned various concentration of 50mL, vibrates under 25 DEG C of environment flat to adsorbing for 24 hours (200rpm)
Weighing apparatus；Centrifuge tube is taken out, is centrifuged 15min at 5000rpm, supernatant is taken to filter to obtain filtrate by 0.45 μm of filter membrane, measurement SRP is dense
Degree；It takes appropriate filtrate in 25mL colorimetric cylinder, is settled to 25mL with distilled water, 10% ascorbic acid of 0.5mL is added, shakes up,
1mL molybdate solution is added after 30s to mix well, develop the color 15min, makees reference with ultrapure water, and the colorimetric under 700nm wavelength is surveyed
Determine phosphorus concentration in solution.
It is calculated by experimental data, obtains the material of different kaolin contents as shown in Figure 1 to phosphatic absorption-solution
Inhale curve；Linear distribution model fitting operation is recycled, each material is obtained to phosphatic adsorption-desorption equilibrium concentration, sees figure
2, wherein linear equation is as follows:
Q=b+KdC
EPC0=(- b)/Kd
In above formula, Q is material to phosphatic equilibrium adsorption capacity, mg/kg；C is balance solution concentration, mg/L；EPC0For
Adsorption-desorption equilibrium concentration, KdFor linear distribution factor.
From figure 2 it can be seen that the kaolinic material containing 10wt% is to phosphatic adsorption-desorption equilibrium concentration
0.03mg/L, distribution coefficient KdValue is 5.6L/g, with the increase of kaolin proportion, EPC0Downward trend, minimum is presented
It is 0.0035, reduces nearly 10 times, but KdDownward trend after first raising is but presented in value, and peak appears in kaolin containing 50wt%
Material in, be 33.6L/g, improve 5 times or more, therefore deduce that the optimum proportioning of material of the present invention, i.e., deposit with
Kaolinic mass ratio is 1:1.
Fig. 3 a~3f show the material as made from different maturing temperatures to the sediment interstitial water with different phosphorus concentrations
In phosphatic removal effect, from Fig. 3 a~3f can be seen that through 700 DEG C roasting obtained by material there is very high phosphoric acid always
Salt removal rate thereby determines that the optimum calcination temperature of preparation method of the present invention is 700 DEG C.
2, water/sediment interface scene in-situ control is tested
The column shaped deposit for acquiring Dian Chi difference lake region, places it in indoor column simulator after transporting laboratory back,
And the thickness for adjusting deposit is about 20cm, then removes overlying water using siphon pipe；To avoid interface after material covering from generating
Differential settlement places a specific thin layer pvc filter disc on deposit surface layer immediately after removing overlying water, makes its level covering
Consolidation effect is generated on deposit surface layer and not to deposit, covers material made from the embodiment of the present invention 5 above pvc filter disc
Material selects the point of Dian Chi difference lake region 4, if four groups of parallel laboratory tests, respectively experimental group 1, experimental group 2, experimental group 3 and experiment
Group 4.This experimental example is handled by control of covering material, to be not provided with coating as control treatment.It is imitated for the control of reinforcing material
Fruit, overlying water is using the artificial lake water substitution of (adjusting water body DO is about 9.0mg/L) after aeration, and concrete configuration method is with reference to text
Offer Assessing the effectiveness of thin-layer sand caps for contaminated
sediment management through passive sampling(Lampert D J,Sarchet W V,Reible D
D, Environmental science&technology, 2011,45 (19): 8437-8443), overlying water depth is 30cm.
In the training period, water sample 100mL at the 5cm of coating (or deposit layer) top is taken to be used to measure phosphate concn,
It is dense that Fig. 4 a~4d respectively corresponds phosphate in the overlying water in experimental group 1~4 after covering material control processing and control treatment
The curve graph changed with simulated time is spent, 4 months monitoring results show the control material of the method for the invention preparation to Yunnan
Difference lake region sediment phosphorus release in pond all has significant control effect, and control of material group overlying water total phosphorus concentration is dropped than control group
7 to 36 times low, material covers control group Phosphorus Exchange at Sediment-water Interface burst size and reduces 73%-97% than control group as a result,.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of preparation method of Phosphorus Exchange at Sediment-water Interface release control material characterized by comprising
(1) lake sediment is acquired, it is freeze-dried, it is ground up, sieved, obtains deposition powder, it is spare；
(2) kaolin is taken, through drying, is ground up, sieved, kaolin powder is obtained, it is spare；
(3) the deposition powder and the kaolin powder are uniformly mixed and form mixed powder, it is spare；
(4) oxidation processes are carried out to the mixed powder using nitric acid, then dried, it is spare；
(5) processing is modified to the mixed powder after step (4) oxidation using ferrous salt solution, then dried, it is spare；
(6) step (5) modified mixed powder is added into water infiltration, then extrusion forming, moulding material is fired after processing i.e.
Obtain Phosphorus Exchange at Sediment-water Interface release control material.
2. the preparation method of Phosphorus Exchange at Sediment-water Interface release control material according to claim 1, which is characterized in that institute
It states in step (3), the quality of the kaolin powder accounts for the 10%-90% of the mixed powder gross mass.
3. the preparation method of Phosphorus Exchange at Sediment-water Interface release control material according to claim 1 or 2, which is characterized in that
The granularity of the deposition powder and the kaolin powder is not less than 100 mesh.
4. the preparation method of Phosphorus Exchange at Sediment-water Interface release control material according to claim 1 or 2, which is characterized in that
5molL is used in step (4)-1HNO3Aqueous solution carries out oxidation processes, the HNO to the mixed powder3Aqueous solution with
The mass ratio of the mixed powder is 50:1.
5. the preparation method of Phosphorus Exchange at Sediment-water Interface release control material according to claim 1 or 2, which is characterized in that
Ferrous salt solution described in step (5) is 0.20molL-1FeSO4Aqueous solution, the FeSO4Aqueous solution is mixed with described
The mass ratio of powder is 100:1.
6. the preparation method of Phosphorus Exchange at Sediment-water Interface release control material according to claim 1 or 2, which is characterized in that
In step (6), the temperature of the calcination process is 120-800 DEG C；The time of the calcination process is 0.5-3h.
7. the preparation method of Phosphorus Exchange at Sediment-water Interface release control material according to claim 1 or 2, which is characterized in that
In step (6), the additive amount of water accounts for the 5-30wt% of the mixed powder quality.
8. the preparation method of Phosphorus Exchange at Sediment-water Interface release control material according to claim 1 or 2, which is characterized in that
The Phosphorus Exchange at Sediment-water Interface release control material is the particle with 3-5mm partial size.
9. the Phosphorus Exchange at Sediment-water Interface release control material conduct as made from claim 1-8 described in any item preparation methods
The purposes of deposit situ capping materials.
10. purposes according to claim 9, which is characterized in that spread the Phosphorus Exchange at Sediment-water Interface release control material
It is located at the surface of contaminated sediment remediation, it is every corresponding to the every reduction 0.10mg/L of the content of Polluted water area surface deposit total phosphorus
The dosage of the annual required Phosphorus Exchange at Sediment-water Interface release control material of square metre contaminated sediment remediation is
0.23-19.71kg；
Phosphate concn in the Interstitial Water of the contaminated sediment remediation is 0.02-1.0mg/L.
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