CN106311129B - A kind of preparation method of the efficient material removal of sediment interstitial water phosphate and application - Google Patents
A kind of preparation method of the efficient material removal of sediment interstitial water phosphate and application Download PDFInfo
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- CN106311129B CN106311129B CN201610798384.5A CN201610798384A CN106311129B CN 106311129 B CN106311129 B CN 106311129B CN 201610798384 A CN201610798384 A CN 201610798384A CN 106311129 B CN106311129 B CN 106311129B
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The present invention provides a kind of preparation method of efficient material removal of sediment interstitial water phosphate and applications, the material is initiatively using lake sediment as base stock, it is mixed again with kaolin after fired and alkaline washing, gained mixed powder adds pore creating material again after modification with Fe and is granulated and roasts molding, and relatively low EPC is had both to which one kind be made0Value and higher QmaxThe efficient material removal of sediment interstitial water phosphate of value.The material of the present 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, and adsorption capacity is larger, therefore material of the present invention can really realize the effective resistance control discharged to Phosphorus Exchange at Sediment-water Interface.And the material materials of the present invention are cheap, and social and economic benefits and good is safe, does not have ecological risk, energy conservation and environmental protection, in application process to Dian Chi difference lake region Phosphorus Exchange at Sediment-water Interface release control significant effect to water body in lake.
Description
Technical field
The present invention relates to a kind of preparation method of efficient material removal of sediment interstitial water phosphate and applications, belong to water ring
Border contamination control field.
Background technology
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, China's majority lake surface sediments is made to be stained significantly.The survey showed that, and many lakes are especially
The substrate pollution of urban lakes is surprising, such as total phosphorus content is up to 3000- in Taihu Lake, Dian Chi, many waters deposits in Chaohu
4000mg/kg.Deposit is not only important home to return to and the 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 migrates and release is depended on
The concentration gradient of Interstitial Water between adjacent two layers on the horizontal or vertical direction of column shaped deposit.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, water can be caused 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 release can but delay or offset the actual effect of 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, 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 in 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 realize counterweight to a certain extent
The water remediation of polluted river channel.
But above-mentioned technology using the clean water sludge of waterworks 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, and above-mentioned covering material is caused to discharge the logical of phosphorus to its overlying water
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 use in situ cover
Lid technology really realizes the reparation to polluted water body, this is a technology urgently to be resolved hurrily to those skilled in the art
Problem.
Invention content
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 cheap, the safe, practicability of materials
By force and to sediment interstitial water low phosphorus hydrochlorate there is the sediment interstitial water phosphate of stronger removal effect efficiently to remove material
The preparation method of material and application.
For this purpose, the present invention realizes that above-mentioned purpose technical solution is:
A kind of preparation method of the efficient material removal of sediment interstitial water phosphate, including:
(1) acquire lake sediment, it is freeze-dried, be ground up, sieved, obtain deposition powder, to the deposition powder according to
It is secondary to carry out roasting and alkaline washing process, it then dries, obtains activated deposition object, it is spare;
(2) it is uniformly mixed the activated deposition object to form mixed powder with kaolin, it is spare;
(3) processing is modified to the mixed powder using iron salt solutions, then dried, it is spare;
(4) pore creating material is added into the modified mixed powder of step (3), adds water infiltration after mixing, is squeezed into
Type, to get the efficient material removal of sediment interstitial water phosphate after molding mass is fired.
Calcination temperature in step (1) is 450-800 DEG C, preferably 600 DEG C.
Washing process is carried out using sodium hydrate aqueous solution in step (1), the sodium hydrate aqueous solution it is a concentration of
0.05-0.3mol/L, preferably 0.1mol/L.
The kaolinic dosage accounts for the 50-90wt% of the mixed powder gross mass, preferably 50wt%.
The iron salt solutions are 0.20molL-1FeSO4Aqueous solution, the FeSO4Aqueous solution and the mixed powder
Mass ratio be 100:1.
The additive amount of the pore creating material is the 0.2-1.5wt%, preferably 0.5wt% of the mixed powder gross mass;Institute
It is corncob to state pore creating material.
The additive amount of water accounts for the 5-30wt% of the mixed powder quality, preferably 10wt% in step (4).
Calcination temperature in step (4) is 550-800 DEG C, preferably 700 DEG C.
The efficient material removal of sediment interstitial water phosphate is the particle with 3-5mm grain sizes.
The efficient material removal of sediment interstitial water phosphate made from above-mentioned preparation method covers in situ as deposit
The purposes of material, the phosphate concn in the sediment interstitial water are 0.02-1.0mg/L.
The above-mentioned technical proposal of the present invention has the following advantages:
1, the preparation method of the efficient material removal of sediment interstitial water phosphate of the present invention, it is contemplated that lacustrine deposit
Object has 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 relatively low, deposit can show, to phosphorus " negative absorption " phenomenon, to cause to use
Deposit as phosphorus controlled-release material there is the phosphate entrained by material itself can to overlying it is water-soluble go out risk, easily cause
The secondary pollution of water body, ecological security is poor, this, which is also exactly the prior art, directly to prepare phosphorus using lake sediment
Where the reason of controlled-release material, and in order to overcome drawbacks described above, the present invention is for the first time using deposit and kaolinic mixture as base
This raw material, after modification with Fe and shaping and roasting, being formed a kind of as shown in Figure 3 has relatively low adsorption-desorption equilibrium concentration
(EPC0) and compared with high-adsorption-capacity (Qmax) the efficient material removal of sediment interstitial water phosphate.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 that phosphorus is discharged from material to overlying water is also smaller, and QmaxValue then reflects material to phosphatic adsorption capacity,
QmaxValue is bigger, shows that material is also bigger to phosphatic adsorption capacity, it can be seen that, sediment interstitial water of the present invention
The efficient material removal of phosphate can really realize the effective resistance control discharged to Phosphorus Exchange at Sediment-water Interface, thus solve existing
Covering material in technology ignore because pursuing phosphorus adsorbance simply material itself phosphorus burst size it is big caused by can not effectively control
The problem of sediment phosphorus endogenous pollution processed.
In particular, preparation method of the present invention is efficient as sediment interstitial water phosphate by using kaolin
Material removal prepares one of raw material, on the one hand can utilize kaolin in high-content aluminium oxide to phosphatic large amount of adsorption,
The strong characteristic of crystallized ability, greatly reduces the adsorption-desorption equilibrium concentration of material itself, improves adsorption capacity, to have
Conducive to realizing to the phosphatic removal of low concentration in lake sediment Interstitial Water, the effective of Phosphorus Exchange at Sediment-water Interface release is realized
Resistance control;On the other hand using the caking property of kaolin itself to ensure the molding of phosphorus release control material;The third aspect utilizes height
Ridge soil is drawn materials cheap, safe, highly practical feature, and the production cost of phosphorus release control material and ecological wind can be reduced
Danger.Also, the preparation method of the present invention has also individually carried out calcination process to deposit, can not only remove deposit hole in this way
Moisture in gap and the carbonate and organic matter being adsorbed on deposit, increase the porosity and specific surface area of deposit, have
Conducive to improving deposit to the adsorption capacity of phosphorus, and can also in activated deposition object more difficult movement phosphorus, subsequent deposit passes through
A degree of Mineral Transformation, which occurs, makes the phosphorus of activation be fixed once again, advantageously reduces the internal loading amount of sediment phosphorus;
Since roasting can make the structure and composition of deposit change, adsorption capacity is enhanced, but roasting can also cause in deposit
Phosphatic locomotivity enhancing, moves in phosphorus based on iron aluminium oxidation state phosphorus, therefore the preparation method of the present invention also uses
Alkaline solution cleans the deposit after roasting, so as to effectively reduce phosphatic background values in material, further carries
Material is risen to phosphatic removal effect.
In addition, the preparation method of the present invention also added pore creating material in the forming process of material, to be existed using pore creating material
Volatilization under roasting condition can make material form the characteristic of uniform tiny cavernous structure, contribute to the specific surface area for increasing material,
To further increase adsorption capacity of the present invention control phosphate material to phosphorus, as shown in Fig. 4 a~4d, when initial phosphate in solution
When concentration is relatively low, material 4 is significantly higher than material 1,2 and 3 to phosphatic adsorption capacity, this is primarily due to the material before pore-creating
The aperture of material is less, and when phosphate concn is relatively low, phosphatic diffusivity is weaker in reaction system, it is more difficult to play material
Adsorption effect, after addition corncob increases the porosity of material, the phosphate of low concentration is easy to penetrate into material internal,
Still higher if thus even if the initial relatively low material of the invention of phosphate concn is to phosphatic removal rate in reaction system.
2, the preparation method of the efficient material removal of sediment interstitial water phosphate of the present invention, by by mixed powder
Granulating and forming is the particle that grain size is 3-5mm, after contaminated deposit surface, can be had by the material-paving of the present invention
Effect reduction bottom water body answers the disturbance of shear force and water body flow to deposit, and then advantageously reduces the phosphorus of sediment resuspension
Release.
3, the preparation method of the efficient material removal of sediment interstitial water phosphate of the present invention, final material obtained
2550mg/Kg is reached as high as to phosphatic adsorption capacity;By by material-paving of the present invention in contaminated deposition
Object surface can realize the effective resistance control discharged to Phosphorus Exchange at Sediment-water Interface, the removal of sediment interstitial water various concentration phosphate
Rate is up to 92%-98%.
Description of the drawings
It, below will be in specific implementation mode 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 be the present 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 the phosphatic absorption-desorption curve graph of 1~4 pair of material;
Fig. 2 is 1~4 pair of phosphatic adsorption isotherm map of material;
Fig. 3 is the phosphatic adsorption-desorption equilibrium concentration (EPC of 1~4 pair of material0) and adsorption capacity (Qmax) figure;
Fig. 4 a~4d respectively represent the phosphatic removal effect figure of 1~4 pair of sediment interstitial water various concentration of material.
Specific implementation mode
Technical scheme 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
The every other embodiment that personnel are 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 loss on ignition of the quality meter of deposit, the Phosphorus in Sediment of Dianchi Lake is 20.23wt%, is 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 profit chemical plant;
Muffle furnace is purchased from Germany's Na Bore Muffle furnaces, model:L5/11/P330+.
Embodiment 1
The efficient material removal of sediment interstitial water phosphate described in the present embodiment is prepared by the following method:
(1) acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity not less than 100 purposes sink
The deposition powder is placed in 450 DEG C of Muffle kiln roasting 2h, 0.2mol/L is used after being cooled to room temperature by product powder
Sodium hydrate aqueous solution carry out washing process, and be placed in air dry oven and be evaporated, obtain activated deposition object, it is spare;
(2) kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, by the activation
Deposit and kaolin powder are thoroughly mixed to form mixed powder in proportion, and the kaolinic dosage accounts for mixed powder gross mass
75wt%, it is spare;
(3) FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing, the FeSO to the mixed powder4Aqueous solution
Mass ratio with the mixed powder is 100:1, and be placed in air dry oven and be evaporated, taking-up is cooled to room temperature spare;
(4) corncob is added into the modified mixed powder of step (3), the additive amount of corncob is the mixed powder
The 0.2wt% of gross mass;Infiltration is added water after mixing, the additive amount of water accounts for the 20wt% of the mixed powder quality, and
After be squeezed into graininess, molding mass roasts 2h in 550 DEG C, and it is efficient to obtain the sediment interstitial water phosphate that grain size is 3-5mm
Material removal.
Embodiment 2
The efficient material removal of sediment interstitial water phosphate described in the present embodiment is prepared by the following method:
(1) acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity not less than 100 purposes sink
The deposition powder is placed in 550 DEG C of Muffle kiln roasting 1h, 0.05mol/ is used after being cooled to room temperature by product powder
The sodium hydrate aqueous solution of L carries out washing process, and is placed in air dry oven and is evaporated, and obtains activated deposition object, spare;
(2) kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, by the activation
Deposit and kaolin powder are thoroughly mixed to form mixed powder in proportion, and the kaolinic dosage accounts for mixed powder gross mass
60wt%, it is spare;
(3) FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing, the FeSO to the mixed powder4Aqueous solution
Mass ratio with the mixed powder is 100:1, and be placed in air dry oven and be evaporated, taking-up is cooled to room temperature spare;
(4) corncob is added into the modified mixed powder of step (3), the additive amount of corncob is the mixed powder
The 0.8wt% of gross mass;Infiltration is added water after mixing, the additive amount of water accounts for the 30wt% of the mixed powder quality, and
After be squeezed into graininess, molding mass roasts 2h in 800 DEG C, and it is efficient to obtain the sediment interstitial water phosphate that grain size is 3-4mm
Material removal.
Embodiment 3
The efficient material removal of sediment interstitial water phosphate described in the present embodiment is prepared by the following method:
(1) acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity not less than 100 purposes sink
The deposition powder is placed in 600 DEG C of Muffle kiln roasting 2h, 0.1mol/L is used after being cooled to room temperature by product powder
Sodium hydrate aqueous solution carry out washing process, and be placed in air dry oven and be evaporated, obtain activated deposition object, it is spare;
(2) kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, by the activation
Deposit and kaolin powder are thoroughly mixed to form mixed powder in proportion, and the kaolinic dosage accounts for mixed powder gross mass
50wt%, it is spare;
(3) FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing, the FeSO to the mixed powder4Aqueous solution
Mass ratio with the mixed powder is 100:1, and be placed in air dry oven and be evaporated, taking-up is cooled to room temperature spare;
(4) corncob is added into the modified mixed powder of step (3), the additive amount of corncob is the mixed powder
The 0.5wt% of gross mass;Infiltration is added water after mixing, the additive amount of water accounts for the 10wt% of the mixed powder quality, and
After be squeezed into graininess, molding mass roasts 2h in 700 DEG C, and it is efficient to obtain the sediment interstitial water phosphate that grain size is 4-5mm
Material removal 4.
Embodiment 4
The efficient material removal of sediment interstitial water phosphate described in the present embodiment is prepared by the following method:
(1) acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity not less than 100 purposes sink
The deposition powder is placed in 800 DEG C of Muffle kiln roasting 1h, 0.15mol/ is used after being cooled to room temperature by product powder
The sodium hydrate aqueous solution of L carries out washing process, and is placed in air dry oven and is evaporated, and obtains activated deposition object, spare;
(2) kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, by the activation
Deposit and kaolin powder are thoroughly mixed to form mixed powder in proportion, and the kaolinic dosage accounts for mixed powder gross mass
80wt%, it is spare;
(3) FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing, the FeSO to the mixed powder4Aqueous solution
Mass ratio with the mixed powder is 100:1, and be placed in air dry oven and be evaporated, taking-up is cooled to room temperature spare;
(4) corncob is added into the modified mixed powder of step (3), the additive amount of corncob is the mixed powder
The 1.0wt% of gross mass;Infiltration is added water after mixing, and the additive amount of water accounts for the 5wt% of the mixed powder quality, then
It is squeezed into graininess, molding mass roasts 1h in 600 DEG C, obtains the sediment interstitial water phosphate that grain size is 3-5mm and efficiently goes
Except material.
Embodiment 5
The efficient material removal of sediment interstitial water phosphate described in the present embodiment is prepared by the following method:
(1) acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity not less than 100 purposes sink
The deposition powder is placed in 700 DEG C of Muffle kiln roasting 1h, 0.3mol/L is used after being cooled to room temperature by product powder
Sodium hydrate aqueous solution carry out washing process, and be placed in air dry oven and be evaporated, obtain activated deposition object, it is spare;
(2) kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, by the activation
Deposit and kaolin powder are thoroughly mixed to form mixed powder in proportion, and the kaolinic dosage accounts for mixed powder gross mass
90wt%, it is spare;
(3) FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing, the FeSO to the mixed powder4Aqueous solution
Mass ratio with the mixed powder is 100:1, and be placed in air dry oven and be evaporated, taking-up is cooled to room temperature spare;
(4) corncob is added into the modified mixed powder of step (3), the additive amount of corncob is the mixed powder
The 1.0wt% of gross mass;Infiltration is added water after mixing, the additive amount of water accounts for the 15wt% of the mixed powder quality, and
After be squeezed into graininess, molding mass roasts 3h in 650 DEG C, and it is efficient to obtain the sediment interstitial water phosphate that grain size is 3-4mm
Material removal.
Embodiment 6
The efficient material removal of sediment interstitial water phosphate described in the present embodiment is prepared by the following method:
(1) acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity not less than 100 purposes sink
The deposition powder is placed in 650 DEG C of Muffle kiln roasting 1h, 0.25mol/ is used after being cooled to room temperature by product powder
The sodium hydrate aqueous solution of L carries out washing process, and is placed in air dry oven and is evaporated, and obtains activated deposition object, spare;
(2) kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, by the activation
Deposit and kaolin powder are thoroughly mixed to form mixed powder in proportion, and the kaolinic dosage accounts for mixed powder gross mass
50wt%, it is spare;
(3) FeSO of 0.2mol/L is utilized4Aqueous solution is modified processing, the FeSO to the mixed powder4Aqueous solution
Mass ratio with the mixed powder is 100:1, and be placed in air dry oven and be evaporated, taking-up is cooled to room temperature spare;
(4) corncob is added into the modified mixed powder of step (3), the additive amount of corncob is the mixed powder
The 0.6wt% of gross mass;Infiltration is added water after mixing, the additive amount of water accounts for the 10wt% of the mixed powder quality, and
After be squeezed into graininess, molding mass roasts 3h in 750 DEG C, and it is efficient to obtain the sediment interstitial water phosphate that grain size is 3-5mm
Material removal.
Comparative example 1
Acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be not less than 100 mesh deposition
The deposition powder is placed in 600 DEG C of Muffle kiln roasting 2h, obtains material 1 by powder.
Comparative example 2
(1) acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity not less than 100 purposes sink
Product powder, it is spare;
(2) kaolin is taken, through drying, is ground up, sieved, granularity is obtained and is not less than 100 mesh kaolin powders, by the deposition
Powder and kaolin powder are thoroughly mixed to form mixed powder in proportion, and the kaolinic dosage accounts for mixed powder gross mass
50wt%, it is spare;
(3) water infiltration, the additive amount of water is added to account for the 10wt% of the mixed powder quality, then squeeze the mixed powder
It is pressed into graininess, molding mass roasts 2h in 700 DEG C, obtains material 2.
Comparative example 3
Acquisition lake sediment be raw material, it is freeze-dried, be ground up, sieved after, obtain granularity be not less than 100 mesh deposition
The deposition powder is placed in 600 DEG C of Muffle kiln roasting 2h, is cooled to after room temperature using 0.1mol/L's by powder
Sodium hydrate aqueous solution carries out washing process, and is placed in air dry oven and is evaporated, and obtains material 3.
Experimental example
The present invention is respectively provided with the phosphatic absorption-desorption experiment of 1~4 pair of material and Adsorption thermodynamics experiment, simultaneously
By simulating sediment interstitial water concentration to investigate 1~4 pair of phosphatic removal effect of sediment interstitial water various concentration of material.
1, absorption-desorption is tested
Configuration (is respectively set close to sediment interstitial water phosphorus concentration ranging from 0~1.0mg/L under the natural conditions of lake
For 0,0.02,0.05,0.10,0.20,0.30,0.50 and 1.0mg/L) water sample;Material dry sample 0.5g is weighed to centrifuge in 100mL
Guan Zhong is separately added into the water sample solution of the above-mentioned various concentrations of 50mL, is vibrated under 25 DEG C of environment flat to adsorbing for 24 hours (200rpm)
Weighing apparatus;Centrifuge tube is taken out, 15min is centrifuged at 5000rpm, supernatant is taken to filter to obtain filtrate by 0.45 μm of filter membrane, it is dense to measure SRP
Degree;It takes appropriate filtrate in 25mL colorimetric cylinders, 25mL is settled to distilled water, 10% ascorbic acid of 0.5mL is added, shakes up,
1mL molybdate solutions are added after 30s to mix well, develop the color 15min, makees reference with ultra-pure water, and the colorimetric under 700nm wavelength is surveyed
Determine phosphorus concentration in solution.
It is calculated by experimental data, obtains the phosphatic absorption-desorption curve of 1~4 pair of material as shown in Figure 1;It is sharp again
With linear distribution model fitting operation, 1~4 pair of phosphatic adsorption-desorption equilibrium concentration of material is obtained, sees Fig. 3, wherein line
Property 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 3, it can be seen that EPC0Show as material 1<Material 2<Material 3<Material 4 that is to say, deposit is through 600
DEG C roasting after gained material EPC0Maximum is 0.027mg/L;Deposit and kaolin in mass ratio 1:1 mixed is incorporated in 700
It is formed by the EPC of material after DEG C roasting0For 0.012mg/L, than deposit, the material of gained improves after 600 DEG C of roastings
1.3 again;Deposit is formed by the EPC of material after 600 DEG C of roastings and 0.1mol/L NaOH aqueous cleanings successively0For
0.0037mg/L, than deposit, the material of gained improves 6.4 times after 600 DEG C of roastings, material made from the embodiment of the present invention 3
4 EPC0For 0.0016mg/L, than deposit, the material of gained improves 16.6 times after 600 DEG C of roastings.It can be seen that according to
Material made from the method for the invention has smaller EPC0Value.
2, Adsorption thermodynamics are tested
The phosphate concn of test solution ranging from 0~15mg/L (is respectively set to 0,0.5,1.0,2.0,5.0,8.0
And 15.0mg/L);Material dry sample 0.5g is weighed in 100mL centrifuge tubes, is separately added into the KH of 50mL various concentration series2PO4It is molten
Liquid, vibrated under 25 DEG C of environment for 24 hours (200rpm) to adsorption equilibrium;Centrifuge tube is taken out, 15min is centrifuged at 5000rpm, takes
Clear liquid filters to obtain filtrate by 0.45 μm of filter membrane, measures SRP concentration;Take appropriate filtrate in 25mL colorimetric cylinders, with distilled water constant volume
To 25mL, 10% ascorbic acid of 0.5mL is added, shakes up, 1mL molybdate solutions are added after 30s and mix well, develop the color 15min,
Make reference with ultra-pure water, the colorimetric under 700nm wavelength measures phosphorus concentration in solution.
It is calculated by experimental data, obtains 1~4 pair of phosphatic adsorption isotherm of material as shown in Figure 2;It recycles
Langmuir model fitting operations obtain 1~4 pair of phosphatic adsorption capacity of material, see Fig. 3, wherein the model sides Langmuir
Journey is as follows:
Q=Qmax×C/(Kd+C)
In formula:Q is sample ammonia-nitrogen balance adsorbance, mg/kg;QmaxMaximal absorptive capacity, mg/kg;C is balance solution ammonia nitrogen
Concentration, mg/L.
From figure 3, it can be seen that QmaxShow as material 2<Material 1<Material 4<Material 3, that is to say, deposit is through 600 DEG C
Material and deposit and kaolin in mass ratio 1 are formed by after roasting:1 it is mixed be incorporated in 700 DEG C of roastings after be formed by material
The Q of materialmaxValue it is relatively low, in contrast, deposit successively through 600 DEG C roasting and 0.1mol/L NaOH aqueous cleanings after institute's shape
At material and the embodiment of the present invention 3 made from material 4 QmaxValue significantly improves.Thus illustrate, alkalinity is carried out to deposit
Washing is to improve material QmaxThe necessary technology means of value.
3, the phosphatic removal effect experiment of 1~4 pair of sediment interstitial water various concentration of material
Dian Chi 0-20cm bed muds are taken, after 5000r/min centrifuges 5-30min, take supernatant by 0.45 μm of miillpore filter,
Up to sediment interstitial water, sediment interstitial water, which is configured to phosphate concn, using phosphate standard storing solution is respectively
0.02, the gap aqueous solution of 0.05,0.1,0.2,0.3,0.5 and 1mg/L, by material 1~4 according to water:The mass ratio of material is
100:1 ratio mixing, then the mixing oscillation 16-24h in 25 DEG C, 200r/min constant temperature oscillators, tests and is calculated
1~4 pair of phosphatic removal effect of sediment interstitial water various concentration of material, as a result as shown in Fig. 4 a~4d.
It is 0.02- to phosphate concn from Fig. 4 a~4d as it can be seen that material 4 is best to the phosphatic removal effect of Interstitial Water
The removal rate of phosphorus has reached 92%-99% in the Interstitial Water of 1mg/L, is secondly material 3, is to Interstitial Water removal rate of phosphate
89%-95%, and material 1 is worst to Interstitial Water phosphate removal effect.Thus it absolutely proves, according to the method for the invention system
The material obtained has the best phosphatic removal effect of Interstitial Water.
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 (16)
1. a kind of preparation method of sediment interstitial water phosphate material removal, which is characterized in that including:
(1) acquire lake sediment, it is freeze-dried, be ground up, sieved, obtain deposition powder, to the deposition powder successively into
Row roasting and alkaline washing process, then dry, obtain activated deposition object, spare;
(2) it is uniformly mixed the activated deposition object to form mixed powder with kaolin, it is spare;
(3) processing is modified to the mixed powder using iron salt solutions, then dried, it is spare;
(4) pore creating material is added into the modified mixed powder of step (3), adds water infiltration after mixing, extrusion forming, at
To get the sediment interstitial water phosphate material removal after proximate matter material is fired.
2. the preparation method of sediment interstitial water phosphate material removal according to claim 1, which is characterized in that step
(1) calcination temperature in is 450-800 DEG C.
3. the preparation method of sediment interstitial water phosphate material removal according to claim 2, which is characterized in that step
(1) calcination temperature in is 600 DEG C.
4. the preparation method of sediment interstitial water phosphate material removal according to claim 1, which is characterized in that step
(1) washing process, a concentration of 0.05-0.3mol/L of the sodium hydrate aqueous solution are carried out using sodium hydrate aqueous solution in.
5. the preparation method of sediment interstitial water phosphate material removal according to claim 4, which is characterized in that described
A concentration of 0.1mol/L of sodium hydrate aqueous solution.
6. the preparation method of sediment interstitial water phosphate material removal according to claim 1, which is characterized in that described
Kaolinic dosage accounts for the 50-90wt% of the mixed powder gross mass.
7. the preparation method of sediment interstitial water phosphate material removal according to claim 6, which is characterized in that described
Kaolinic dosage accounts for the 50wt% of the mixed powder gross mass.
8. the preparation method of sediment interstitial water phosphate material removal according to claim 1, which is characterized in that described
Iron salt solutions are 0.20molL-1FeSO4Aqueous solution, the FeSO4The mass ratio of aqueous solution and the mixed powder is
100:1。
9. the preparation method of sediment interstitial water phosphate material removal according to claim 1, which is characterized in that described
The additive amount of pore creating material is the 0.2-1.5wt% of the mixed powder gross mass;The pore creating material is corncob.
10. the preparation method of sediment interstitial water phosphate material removal according to claim 9, which is characterized in that institute
The additive amount for stating pore creating material is the 0.5wt% of the mixed powder gross mass.
11. the preparation method of sediment interstitial water phosphate material removal according to claim 1, which is characterized in that step
Suddenly the additive amount of water accounts for the 5-30wt% of the mixed powder quality in (4).
12. the preparation method of sediment interstitial water phosphate material removal according to claim 11, which is characterized in that step
Suddenly the additive amount of water accounts for the 10wt% of the mixed powder quality in (4).
13. special according to the preparation method of claim 1-12 any one of them sediment interstitial water phosphate material removals
Sign is that the calcination temperature in step (4) is 550-800 DEG C.
14. the preparation method of sediment interstitial water phosphate material removal according to claim 13, which is characterized in that step
Suddenly the calcination temperature in (4) is 700 DEG C.
15. the preparation method of sediment interstitial water phosphate material removal according to claim 1, which is characterized in that institute
It is the particle with 3-5mm grain sizes to state sediment interstitial water phosphate material removal.
16. the sediment interstitial water phosphate material removal conduct made from claim 1-15 any one of them preparation methods
The purposes of deposit situ capping materials, the phosphate concn in the sediment interstitial water are 0.02-1.0mg/L.
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