CN110449125A - Charcoal/silicon/iron oxide composite material preparation method and application - Google Patents
Charcoal/silicon/iron oxide composite material preparation method and application Download PDFInfo
- Publication number
- CN110449125A CN110449125A CN201910745086.3A CN201910745086A CN110449125A CN 110449125 A CN110449125 A CN 110449125A CN 201910745086 A CN201910745086 A CN 201910745086A CN 110449125 A CN110449125 A CN 110449125A
- Authority
- CN
- China
- Prior art keywords
- charcoal
- composite material
- phosphate
- solution
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
Abstract
The present invention relates to charcoal/silicon/iron oxide composite material preparation method and applications, iron oxide particle is loaded into biological carbon surface by simple coprecipitation method, it forms that pore structure is good and the biggish composite material of specific surface area, and is applied to phosphatic removal in aqueous solution.By studying charcoal/ferriferous oxide synthesis condition, relatively more synthesized material removes phosphatic effect.By research charcoal/silicon/iron oxide composite material to absorption property phosphatic in water, the optimal values such as adsorbent amount, adsorption time, adsorption concentration are obtained.Charcoal has porous structure and big surface area, and from a wealth of sources, low in cost.Great amount of hydroxy group free radical is contained on ferriferous oxide surface, can be converted into positively charged adsorption site.Charcoal/silicon/iron oxide composite material of this method preparation has preferable removal ability for phosphate in water, and has stronger stability and recyclable recycling property.
Description
Technical field
The present invention relates to phosphate from sewage to pollute process field, specially charcoal/silicon/iron oxide composite material.
Background technique
As human industry's activity and the continuous expansion of urbanization range, water eutrophication problem are gradually aggravated,
Through becoming global environmental problem.Water eutrophication can lead to the characteristics algae excessive propagation such as blue-green alge, water body it is transparent
Degree reduces, and in turn results in dissolved oxygen content and sharply declines, seriously destroys the ecosystem environments such as lake, reservoir.It grinds both at home and abroad
Study carefully and shows that P elements are the key factors for causing water eutrophication.Phosphorus is very important mineral element in life entity, still
Excessive phosphorus if it exists in water body water quality will occurs and deteriorate and phenomena such as shortage of water resources.Therefore, dephosphorization process is for water
Body eutrophication control has key effect.
The method of sewage dephosphorization mainly has chemical method, physical method, bioanalysis etc..Wherein, chemical method dephosphorization function refers to
Difficultly-soluble phosphates sediment is generated using the metal ion and phosphate radical of the generations such as molysite, aluminium salt and lime to remove in waste water
Phosphorus.Physical method includes manually salvaging, making stream diversion, aeration etc..Bioanalysis dephosphorization is to be based on biting phosphorus bacterium in aerobic and anaerobic condition
Under, intake and release phosphorus realize dephosphorization by the alternate run of Aerobic-anaerobic.Wherein dephosphorization method through adsorption has high-efficient,
The features such as easy to operate, and reliable for operation, has been widely studied and has applied.
In recent years, charcoal has been widely used for the multiple fields such as pollutant removal, carbon fixation and soil remediation.Biology
Carbon feedstock abundance, cost is relatively low, has apparent porous structure and big hole area, is conducive to the progress of adsorption process.
But since there are a large amount of negative electrical charges to constrain its removal to anionic pollutant in aqueous solution for biological carbon surface.And ferriferous oxide
Multiple oxygen atoms and cation crystal binding sites are capable of forming in water environment, while fault of construction existing for its surface also can
Certain activated adoption site is enough provided for suction-operated.In addition, hydroxyl of the ferriferous oxide surface also containing high concentration is free
Base can transform into positively charged site under field conditions (factors), be conducive to the removal of anionic pollutant in aqueous solution.Iron
The surface of oxide and its hyrate also possesses the higher hydroxyl radical free radical of content, and phosphate can pass through electrostatic interaction and ligand
The forms such as exchange are attracted to its surface.
Charcoal/silicon/iron oxide composite material prepared by the present invention is a kind of novel adsorbent material, for removing waste water
In phosphate contaminants, composite material exhibits go out low cost, high efficiency, preparation method is simple and recyclable recycling etc.
Advantage.
Summary of the invention
Charcoal/silicon/iron oxide composite material, preparation step are as follows:
Step 1 prepares charcoal: the shell charcoal after being pyrolyzed at 900 DEG C is crossed 200 meshes.
Step 2 prepares charcoal/magnetic iron ore composite material: weigh 5 g shell charcoals, 7.6 g Iron trichloride hexahydrates and
2.8 g, tetra- water frerrous chloride is placed in 250 mL beakers, is dissolved with 100 mL distilled water, is denoted as solution A, another to prepare 1 mol/L
NaOH solution is denoted as solution B；By solution A ultrasound 0.5h to after mixing, it is added in four-hole boiling flask, in temperature 60 C, 140
1.5 h of r/min revolving speed and the lower stirring of nitrogen atmosphere protection；Solution B is added dropwise into four-hole boiling flask suspension, adjusts pH to 10
Left and right, stirs 1.5 h under 90 DEG C of environment.
Step 3: it prepares charcoal/ferrihydrite composite material: weighing 5 g shell charcoals, 10 g, nine water ferric nitrate is placed in
In 250 mL beakers, 50 mL distilled water, 0.5 h of high speed magnetic stirring is added；1 mol/ is added dropwise into above-mentioned mixed solution
L KOH adjusts pH about to after 7, continuing to stir 0.5h.
Step 4 after the reaction was completed washs mixed solution to neutrality, after sediment distinguishes freeze-dried/vacuum drying
Obtain charcoal/silicon/iron oxide composite material.
Preferably, charcoal/silicon/iron oxide composite material is for adsorbing phosphate；Adsorption process is chemisorption.
Preferably, the phosphatic adsorption method are as follows: take the phosphate solution of 20 mL in 50 mL centrifuge tubes, be added
Charcoal/silicon/iron oxide composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphatic concentration,
According to the residual concentration of the phosphate solution of solution after the initial concentration and absorption that phosphate solution is added, phosphatic go is calculated
Except rate.
Preferably, the difference of phosphate concn described in charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material
For 4-60 mg/L and 2-100 mg/L.
Preferably, removal rate highest when phosphate solution concentration is 8 mg/L.
Preferably, charcoal/magnetic iron ore and charcoal/ferrihydrite composite material recycling number are more than or equal to 5.
Preferably, when adsorbing phosphate, charcoal/magnetic iron ore and charcoal/ferrihydrite composite material dosage are respectively
0.06 g and 0.05 g.
Preferably, when adsorbing phosphate, charcoal/magnetic iron ore and charcoal/ferrihydrite composite material, it is characterised in that inhale
Attached equilibration time is 120 min and 180 min respectively.
Preferably, charcoal/magnetic iron ore and charcoal/ferrihydrite composite material are in simulation water adsorption experiment to phosphate
Removal effect it is good.
Beneficial effect
(1) charcoal and ferriferous oxide there is collaboration to make removal phosphatic in water in charcoal/silicon/iron oxide composite material
With.
(2) phosphate concn described in charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material is respectively 4-
When 60 mg/L and 2-100 mg/L, removal rate is higher；When phosphate concn is 8 mg/L, adsorption effect is best.
(3) charcoal/silicon/iron oxide composite material meets quasi- second-order kinetic equation, shows to phosphatic being adsorbed as
Learn absorption.Charcoal/silicon/iron oxide composite material XPS analysis after absorption phosphate shows that suction-operated includes phosphate and answers
The electrostatic attraction of condensation material surface functional group and ligand exchange effect, further explanation are adsorbed as chemisorption to phosphatic.
(4) charcoal/iron oxide material absorption phosphate is a complicated process.First stage is quick
Grain adsorption；Second stage is absorption in particle.First stage is faster than second stage, mainly since particle interior suction is accompanied by and
With the progress of absorption, phosphate concn is reduced in aqueous solution, so that the rate of adsorption reduces.
(5) charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material dosage are respectively 0.06g and 0.05
Using effect is preferable when g.
(6) when adsorbing phosphate, charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material, feature exist
In time of equilibrium adsorption be 120 min and 180 min respectively.
(7) charcoal/silicon/iron oxide composite material reuse effect is preferable.
(8) charcoal/silicon/iron oxide composite material is preferable to phosphate effect in simulation water adsorption experiment.
Detailed description of the invention
Fig. 1 is charcoal/silicon/iron oxide composite material preparation flow and mechanism of action schematic diagram.
Fig. 2 is the charcoal/magnetic iron ore composite material (caption: BC-M) and charcoal/water that embodiment 2 and 6 is prepared
Iron ore composite material (caption: BC-F) characterization result.Wherein, (A) is charcoal/silicon/iron oxide composite material XRD diagram；(B)
It is charcoal/silicon/iron oxide composite material XPS figure.
Fig. 3 is the charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material that embodiment 2 and 6 is prepared
Adsorb the XPS map of O 1s, the C 1s and Fe 2p before and after phosphate.
Fig. 4 is the charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material that embodiment 2 and 6 is prepared
TEM, HRTEM, SEM and EDS phenogram.
Fig. 5 is the charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material that embodiment 2 and 6 is prepared
BET figure.
Fig. 6 is the charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material that embodiment 2 and 6 is prepared
Adsorption property research.It (A) is that charcoal/silicon/iron oxide composite material of different amounts and charcoal adsorb phosphatic removal
Rate curve；It (B) is charcoal under condition of different pH/silicon/iron oxide composite material adsorption rate curve；It (C) is charcoal/iron oxidation
Removal rate curve of the object composite material in different adsorption times.
Fig. 7 is the charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material that embodiment 2 and 6 is prepared
Adsorb phosphatic adsorption dynamics adsorption kinetics and thermoisopleth research.It (A) is quasi- second-order kinetics research；It (B) is intra-particle diffusion model
Research；It (C) is adsorption isotherm research.
Fig. 8 is the charcoal/silicon/iron oxide composite material FTIR(A adsorbed after phosphate), XRD(B), XPS(C) and
HR-XPS (P2p) (D) analysis.
Fig. 9 is charcoal/silicon/iron oxide composite material adsorption-desorption cycle, and (A) is the absorption time of 2 material circulation of embodiment
Number figure；(B) number figure is adsorbed for 6 material circulation of embodiment.
Figure 10 is that charcoal/silicon/iron oxide composite material simulation water adsorption experiment (A) is adsorbed for 2 material simulation water of embodiment
Experiment；It (B) is 6 material simulation water adsorption experiment of embodiment.
Specific embodiment
One, charcoal/silicon/iron oxide composite material preparation
Embodiment 1:
(1) the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.
(2) 5 g shell charcoals, 2.7 g Iron trichloride hexahydrates and 1.0 g, tetra- water frerrous chloride are weighed and is placed in 250 mL beakers
In, it is dissolved with 100 mL distilled water, is denoted as solution A；It is another to prepare 1 mol/L NaOH solution, it is denoted as solution B.
(3) solution A 0.5 h of ultrasound is added in four-hole boiling flask, to after mixing in 60 DEG C of environment temperatures, 140 r/
1.5 h of min revolving speed and the lower stirring of nitrogen atmosphere protection.Solution B is added dropwise into four-hole boiling flask suspension, it is left to adjust pH to 10
1.5 h are stirred on the right side under 90 DEG C of environment.
(4) mixed solution is washed to neutrality after the reaction was completed, it is freeze-dried rear spare obtains sediment.
At room temperature, 0.06 g charcoal/magnetic iron ore composite material is added in the phosphate solution of 20 mL, 8 mg/L,
4 h are vibrated, adsorption rate reaches 65.1%.
Embodiment 2:
(1) the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.
(2) 5 g shell charcoals, 7.6 g Iron trichloride hexahydrates and 2.8 g, tetra- water frerrous chloride are weighed and is placed in 250 mL beakers
In, it is dissolved with 100 mL distilled water, is denoted as solution A；It is another to prepare 1 mol/L NaOH solution, it is denoted as solution B.
(3) solution A ultrasound 0.5h is added in four-hole boiling flask, to after mixing in 60 DEG C of environment temperatures, 140 r/
1.5 h of min revolving speed and the lower stirring of nitrogen atmosphere protection.Solution B is added dropwise into four-hole boiling flask suspension, it is left to adjust pH to 10
1.5 h are stirred on the right side under 90 DEG C of environment.
(4) mixed solution is washed to neutrality after the reaction was completed, it is freeze-dried rear spare obtains sediment.
At room temperature, 0.06 g charcoal/magnetic iron ore composite material is added in the phosphate solution of 20 mL, 8 mg/L,
4 h are vibrated, adsorption rate reaches 87.8%.
Embodiment 3:
(1) the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.
(2) 5 g shell charcoals are weighed, 2.5 g, nine water ferric nitrate is placed in 250 mL beakers, be added 50 mL distilled water,
0.5 h of high speed magnetic stirring.It is added dropwise 1 mol/L KOH into above-mentioned mixed solution, adjusts pH about to after 7, continue to stir
0.5h。
(3) mixed solution is washed to neutrality after the reaction was completed, it is spare after 60 DEG C of vacuum drying obtains sediment.
At room temperature, 0.05 g charcoal/ferrihydrite composite material is added in the phosphate solution of 20 mL, 8 mg/L,
4 h are vibrated, adsorption rate reaches 15.5%.
Embodiment 4:
(1) the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.
(2) 5 g shell charcoals are weighed, 5.0 g, nine water ferric nitrate is placed in 250 mL beakers, be added 50 mL distilled water,
0.5 h of high speed magnetic stirring.It is added dropwise 1 mol/L KOH into above-mentioned mixed solution, adjusts pH about to after 7, continue to stir
0.5h。
(3) mixed solution is washed to neutrality after the reaction was completed, it is spare after 60 DEG C of vacuum drying obtains sediment.
At room temperature, 0.05 g charcoal/ferrihydrite composite material is added in the phosphate solution of 20 mL, 8 mg/L,
4 h are vibrated, adsorption rate reaches 67.8%.
Embodiment 5:
(1) the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.
(2) 5 g shell charcoals are weighed, 6.0 g, nine water ferric nitrate is placed in 250 mL beakers, be added 50 mL distilled water,
0.5 h of high speed magnetic stirring.It is added dropwise 1 mol/L KOH into above-mentioned mixed solution, adjusts pH about to after 7, continue to stir
0.5h。
(3) mixed solution is washed to neutrality after the reaction was completed, it is spare after 60 DEG C of vacuum drying obtains sediment.
At room temperature, 0.05 g charcoal/ferrihydrite composite material is added in the phosphate solution of 20 mL, 8 mg/L,
4 h are vibrated, adsorption rate reaches 74.8%.
Embodiment 6:
(1) the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.
(2) 5 g shell charcoals are weighed, 10.0 g, nine water ferric nitrate is placed in 250 mL beakers, addition 50 mL distillation
Water, 0.5 h of high speed magnetic stirring.It is added dropwise 1 mol/L KOH into above-mentioned mixed solution, adjusts pH about to after 7, continue to stir
Mix 0.5h.
(3) mixed solution is washed to neutrality after the reaction was completed, it is spare after 60 DEG C of vacuum drying obtains sediment.
At room temperature, 0.05 g charcoal/ferrihydrite composite material is added in the phosphate solution of 20 mL, 8 mg/L,
4 h are vibrated, adsorption rate reaches 81.0%.
Embodiment 7:
(1) the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.
(2) 5 g shell charcoals are weighed, 15.0 g, nine water ferric nitrate is placed in 250 mL beakers, addition 50 mL distillation
Water, 0.5 h of high speed magnetic stirring.It is added dropwise 1 mol/L KOH into above-mentioned mixed solution, adjusts pH about to after 7, continue to stir
Mix 0.5h.
(3) mixed solution is washed to neutrality after the reaction was completed, it is spare after 60 DEG C of vacuum drying obtains sediment.
At room temperature, 0.05 g charcoal/ferrihydrite composite material is added in the phosphate solution of 20 mL, 8 mg/L,
4 h are vibrated, adsorption rate reaches 86.1%.
Table 1: the adsorption effect comparison that charcoal/magnetic iron ore composite material embodiment is prepared
Table 2: the adsorption effect comparison that charcoal/ferrihydrite composite material embodiment is prepared
Through analyzing, selection example 2 is charcoal/magnetic iron ore composite material to phosphatic optimal adsorption, and embodiment 6 is biology
Charcoal/ferrihydrite composite material is to phosphatic optimal adsorption.
Two, advantage of the charcoal/silicon/iron oxide composite material compared to charcoal, ferriferous oxide
The material preparation method of following example 8-12 are as follows:
The preparation of magnetic iron ore: weighing 7.6 g Iron trichloride hexahydrates and 2.8 g, tetra- water frerrous chloride is placed in 250 mL beakers, with 100
The dissolution of mL distilled water, is denoted as solution A；It is another to prepare 1 mol/L NaOH solution, it is denoted as solution B.By solution A 0.5 h of ultrasound to mixed
It after closing uniformly, is added in four-hole boiling flask, stirs 1.5 under the protection of 60 DEG C of environment temperatures, 140 r/min revolving speeds and nitrogen atmosphere
h.Solution B is added dropwise into four-hole boiling flask suspension, adjusts pH to 10 or so, 1.5 h is stirred under 90 DEG C of environment.It has reacted
Mixed solution is washed to neutrality after, it is freeze-dried rear spare to obtain sediment.
The preparation of ferrihydrite: weighing 10.0 g, nine water ferric nitrate and be placed in 250 mL beakers, and 50 mL distilled water are added, high
Fast 0.5 h of magnetic agitation.It is added dropwise 1 mol/L KOH into above-mentioned mixed solution, adjusts pH about to after 7, continue stirring 0.5
h.Mixed solution is washed to neutrality after the reaction was completed, it is spare after 60 DEG C of vacuum drying to obtain sediment.
The preparation of charcoal/magnetic iron ore composite material: the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.Claim
It takes 5 g shell charcoals, 7.6 g Iron trichloride hexahydrates and 2.8 g, tetra- water frerrous chloride to be placed in 250 mL beakers, is steamed with 100 mL
Distilled water dissolution, is denoted as solution A；It is another to prepare 1 mol/L NaOH solution, it is denoted as solution B.0.5 h of solution A ultrasound is equal to mixing
It after even, is added in four-hole boiling flask, stirs 1.5 h under the protection of 60 DEG C of environment temperatures, 140 r/min revolving speeds and nitrogen atmosphere.To
Solution B is added dropwise in four-hole boiling flask suspension, adjusts pH to 10 or so, 1.5 h is stirred under 90 DEG C of environment.After the reaction was completed
Mixed solution is washed to neutrality, it is freeze-dried rear spare to obtain sediment.
The preparation of charcoal/ferrihydrite composite material: the shell charcoal after being pyrolyzed at 900 DEG C is crossed into 200 meshes.Claim
It takes 5 g shell charcoals, 10.0 g, nine water ferric nitrate to be placed in 250 mL beakers, 50 mL distilled water, high speed magnetic stirring is added
0.5 h.It is added dropwise 1 mol/L KOH into above-mentioned mixed solution, adjusts pH about to after 7, continue to stir 0.5 h.It has reacted
Mixed solution is washed to neutrality after, it is spare after 60 DEG C of vacuum drying to obtain sediment.
Embodiment 8: shell charcoal is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, the shell charcoal of 0.05 g, room is added
Temperature is lower to vibrate 4 h, is then centrifuged, supernatant is taken to detect phosphate concn, according to the initial concentration that phosphate solution is added
With the phosphate residual concentration of solution after absorption, calculating phosphatic removal rate is 0.4%.
Embodiment 9: magnetic iron ore is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, the fruit magnetic iron ore of 0.05 g, room temperature is added
4 h of lower oscillation, are then centrifuged, take supernatant detect phosphate concn, according to be added phosphate solution initial concentration and
The phosphate residual concentration of solution after absorption, calculating phosphatic removal rate is 70.2%.
Embodiment 10: ferrihydrite is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, the shell charcoal of 0.05 g, room is added
Temperature is lower to vibrate 4 h, is then centrifuged, supernatant is taken to detect phosphate concn, according to the initial concentration that phosphate solution is added
With the phosphate residual concentration of solution after absorption, calculating phosphatic removal rate is 75.4%.
Embodiment 11: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 78.0%.
Embodiment 12: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 81.0%.
Table 3: each embodiment adsorption effect comparison
Relative magnet mine (ferrihydrite) and the final synthetic quantity of charcoal/silicon/iron oxide composite material are found in charcoal/iron oxygen
Charcoal and magnetic iron ore (ferrihydrite) mass component ratio about 5:2 in compound composite material.The charcoal of every 7 g in the present invention/
It include 5 g shell charcoals and 2 g magnetic iron ores (ferrihydrite) in silicon/iron oxide composite material.
For in verifying charcoal/silicon/iron oxide composite material, charcoal and ferriferous oxide whether there is synergistic effect, comparison
To phosphatic adsorption capacity, discovery is multiple for independent charcoal, independent ferriferous oxide and object charcoal/silicon/iron oxide composite material in table 3
Condensation material adsorption capacity has more advantage, so existing between charcoal and ferriferous oxide in charcoal/silicon/iron oxide composite material
Synergistic effect, adsorption capacity are effectively increased.
Three, charcoal/silicon/iron oxide composite material is to the phosphatic absorption of various concentration
Embodiment 13: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 4 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 87.9%.
Embodiment 14: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 5 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 86.2%.
Embodiment 15: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 6 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 89.4%.
Embodiment 16: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 87.5%.
Embodiment 17: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 10 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 81.2%.
Embodiment 18: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 15 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 77.4%.
Embodiment 19: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 20 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 71.0%.
Embodiment 20: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 25 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 61.2%
Embodiment 21: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 40 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 49.8%
Embodiment 22: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 50 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 48.0%
Embodiment 23: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 60 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 45.6%
Table 4: charcoal/magnetic iron ore composite material is to the phosphatic absorption of various concentration
For comparative example 13-23 it is found that when phosphate concn is 4-60 mg/L, removal rate is higher；Comprehensive each factor, choosing
Selecting phosphate concn is 8 mg/L, and absorption property is best.
Embodiment 24: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 2 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 93.5%.
Embodiment 25: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 4 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 93.0%.
Embodiment 26: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 5 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 92.0%.
Embodiment 27: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 6 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 95.8%.
Embodiment 28: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 95.0%.
Embodiment 29: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 10 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 93.2%.
Embodiment 30: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 15 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 94.8%.
Embodiment 31: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 20 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 92.8%.
Embodiment 32: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 25 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 86.6%.
Embodiment 33: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 40 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 72.7%.
Embodiment 34: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 50 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 68.9%.
Embodiment 35: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 60 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 67.0%.
Embodiment 36: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 80 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition phosphate solution
Initial concentration and absorption after solution phosphate residual concentration, calculate phosphatic removal rate be 54.2%.
Embodiment 37: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 100 mg/L in 50 mL centrifuge tubes, charcoal/water iron of 0.05 g is added
Mine composite material vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, and according to being added, phosphate is molten
The phosphate residual concentration of solution after the initial concentration of liquid and absorption, calculating phosphatic removal rate is 44.3%.
For comparative example 24-37 it is found that when phosphate concn is 2-100 mg/L, removal rate is higher；It is comprehensive it is each because
Element, selects phosphate concn for 8 mg/L, and absorption property is best.
Table 5: charcoal/ferrihydrite composite material is to the phosphatic absorption of various concentration
Adsorption isotherm research
In adsorption equilibrium research, the most commonly used is Freundlich adsorption isotherms and Langmuir to inhale for description adsorption isotherm
Attached isotherm formula, abbreviation F, L-type.Hereinafter, using progress adsorption isotherm research to embodiment 16- embodiment 43.
Freundlich model meets equation:；Langmuir model meets equation:。
Wherein,q e(mg/g) andq m(mg/g) equilibrium adsorption capacity and maximal absorptive capacity are respectively indicated；c eIt (mg/L) is equilibrium concentration；K L
It (L/mg) is Langmuir constant；K F((mg/g)/(mg/L)n) it is Freundlich constant；nIt is constant.
Fig. 7 (C) is phosphatic adsorption isotherm, and table 6 is adsorption isotherm fitting result.The results show that charcoal/magnetic
Iron ore composite material better conforms to Freundlich model and Langmuir model, charcoal/water iron to Phosphate Adsorption
Mine composite material more meets Langmuir model.
Table 6: adsorption isotherm research
Four, charcoal/silicon/iron oxide composite material studies phosphatic adsorption time
Embodiment 38: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, charcoal/magnetic iron ore of 0.06 g is added
Composite material vibrates certain time (table 7) at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition
The phosphate residual concentration of solution, calculates phosphatic removal rate after the initial concentration of phosphate solution and absorption.
Table 7: charcoal/magnetic iron ore composite material studies phosphatic adsorption time
Embodiment 39: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, charcoal/ferrihydrite of 0.05 g is added
Composite material vibrates certain time (table 8) at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition
The phosphate residual concentration of solution, calculates phosphatic removal rate after the initial concentration of phosphate solution and absorption.
Table 8: charcoal/ferrihydrite composite material studies phosphatic adsorption time
The adsorption kinetic data data can with many kinetics equations for example primary adsorption rate equation, modified intra-particle diffusion model,
The models such as secondary absorption rate equation are fitted, this research using primary adsorption Rate Models, secondary absorption Rate Models and
Intra-particle diffusion model is fitted experimental data.
First _ order kinetics equation are as follows:；Second-order kinetic equation are as follows:。
Wherein,q e(mg/g) andq t(mg/g) adsorbance when equilibrium adsorption capacity and time t is respectively indicated；k 1(1/min) andk 2
(g/mg min) is respectively the rate constant of first _ order kinetics equation and second-order kinetic equation.
In order to further explore rate of adsorption rate-determining steps, usually studied using diffusion model in particle.Model
Formula are as follows:.Whereink di(mg/(g min1/2)) it is intra-particle diffusion rate constant.C iIt is one and boundary
The proportional intra-particle diffusion constant of thickness degree.
Table 9 be kinetics model of biosorption research, charcoal/silicon/iron oxide composite material meet quasi- second-order kinetic equation and
Intra-particle diffusion model shows to be adsorbed as chemisorption to phosphatic.
Fig. 7 (B) is that charcoal/silicon/iron oxide composite material adsorbs phosphatic modified intra-particle diffusion model fitting, as a result table
Bright charcoal/silicon/iron oxide composite material absorption phosphate is a complicated process.First stage is quick particle surface
Absorption；Second stage is absorption in particle.First stage is faster than second stage mainly since particle interior suction is accompanied by and with suction
Attached progress, phosphate ion concentration reduce, so that the rate of adsorption reduces.
Table 9: adsorption dynamics adsorption kinetics research
Five, influence of the dosage of adsorbent to removal rate
Embodiment 40: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, the charcoal or biology of different quality is added
Charcoal/magnetic iron ore composite material (table 10), vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, phosphatic removal rate is calculated.
Table 10: different amounts charcoal or charcoal/magnetic iron ore composite material are to phosphatic removal
Embodiment 41: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, the charcoal or biology of different quality is added
Charcoal/ferrihydrite composite material (table 11), vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, phosphatic removal rate is calculated.
Table 11: different amounts charcoal or charcoal/ferrihydrite composite material are to phosphatic removal
In conjunction with Fig. 7 (A) and table 10, table 11 it is found that charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material can
Select 0.06g and 0.05 g as usage amount respectively, and adsorption effect is substantially better than charcoal.
Six, influence of the difference pH to absorption
Embodiment 42: charcoal/magnetic iron ore composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, it is multiple that 0.06 g charcoal/magnetic iron ore is added
Condensation material adjusts different pH value (table 12), vibrates 4 h at room temperature, be then centrifuged, and supernatant is taken to detect phosphate concn,
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, phosphatic removal rate is calculated.
Embodiment 43: charcoal/ferrihydrite composite material is to phosphatic removal
It takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, it is multiple that 0.05 g charcoal/ferrihydrite is added
Condensation material adjusts different pH value (table 12), vibrates 4 h at room temperature, be then centrifuged, and supernatant is taken to detect phosphate concn,
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, phosphatic removal rate is calculated.
Table 12: different pH are to phosphatic removal
In conjunction with table 12 and Fig. 6 (B) it is found that charcoal/magnetic iron ore composite material removal rate when pH is 2 reaches 90% or more；It is raw
For object charcoal/ferrihydrite composite material when pH is 2-4 or so, removal rate is higher than 85%；As a result illustrate two kinds of materials to phosphatic suction
Attached process is influenced by pH value.
Seven, detachment assays
Embodiment 44:
(1) it step 1: takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, the biology of 0.06 g is added
Charcoal/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition
The phosphate residual concentration of solution after the initial concentration of phosphate solution and absorption calculates adsorbance and removal rate.
Step 2: charcoal/magnetic iron ore composite material after separation adds 20 mL with a certain amount of distillation water washing 3 times
0.5 mol/L sodium hydroxide solution parsing, oscillation after a certain period of time, centrifuge separation, by after centrifuge separation adsorbent dry
Repeat the above steps an adsorption process again afterwards, calculates adsorbance and removal rate.
Shown in experimental result such as Fig. 9 (A).
(2) it step 1: takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, is added 0.06 g's
Charcoal/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, foundation
The phosphate residual concentration of solution, calculates adsorbance and removal rate after the initial concentration of addition phosphate solution and absorption.
Step 2: charcoal/magnetic iron ore composite material after separation adds 20 mL with a certain amount of distillation water washing 3 times
1 mol/L sodium hydroxide solution parsing, oscillation after a certain period of time, centrifuge separation, by after centrifuge separation adsorbent drying after
Repeat the above steps an adsorption process again, calculates adsorbance and removal rate.
Shown in experimental result such as Fig. 9 (A).
It is preferable that effect is reused under two kinds of parsing agent by charcoal/magnetic iron ore composite material it can be seen from Fig. 9 (A),
Number is reused to be more than or equal to 5 times.
Embodiment 45:
(1) it step 1: takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, the biology of 0.05 g is added
Charcoal/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to addition
The phosphate residual concentration of solution after the initial concentration of phosphate solution and absorption calculates adsorbance and removal rate.
Step 2: charcoal/ferrihydrite composite material after separation adds 20 mL with a certain amount of distillation water washing 3 times
0.5 mol/L sodium hydroxide solution parsing, oscillation after a certain period of time, centrifuge separation, by after centrifuge separation adsorbent dry
Repeat the above steps an adsorption process again afterwards, calculates adsorbance and removal rate.
Shown in experimental result such as Figure 10 (B).
(2) it step 1: takes the phosphate solution that 20 mL concentration are 8 mg/L in 50 mL centrifuge tubes, is added 0.05 g's
Charcoal/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, foundation
The phosphate residual concentration of solution, calculates adsorbance and removal rate after the initial concentration of addition phosphate solution and absorption.
Step 2: charcoal/ferrihydrite composite material after separation adds 20 mL with a certain amount of distillation water washing 3 times
1 mol/L sodium hydroxide solution parsing, oscillation after a certain period of time, centrifuge separation, by after centrifuge separation adsorbent drying after
Repeat the above steps an adsorption process again, calculates adsorbance and removal rate.
Shown in experimental result such as Figure 10 (B).
Reused under two kinds of parsing agent by charcoal/ferrihydrite composite material it can be seen from Figure 10 (B) effect compared with
Good, recycling number is more than or equal to 5 times.
Eight, water adsorption experiment is simulated
Embodiment 46:
The life of 0.06 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the tap water that 20 mL concentration are 8 mg/L to prepare
Object charcoal/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, and foundation adds
Enter the initial concentration of phosphate solution and the phosphate residual concentration of solution after absorption, calculates adsorbance and removal rate.
Embodiment 47:
0.06 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the simulation surface water that 20 mL concentration are 8 mg/L to prepare
Charcoal/magnetic iron ore composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 48:
0.06 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the simulated groundwater that 20 mL concentration are 8 mg/L to prepare
Charcoal/magnetic iron ore composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 49:
0.06 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the practical surface water that 20 mL concentration are 8 mg/L to prepare
Charcoal/magnetic iron ore composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 50:
The phosphate solution for taking the practical seawater that 20 mL concentration are 8 mg/L to prepare is added 0.06 g's in 50 mL centrifuge tubes
Charcoal/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, foundation
The phosphate residual concentration of solution, calculates adsorbance and removal rate after the initial concentration of addition phosphate solution and absorption.
Shown in embodiment 46-50 experimental result such as Figure 10 (A).
Embodiment 51:
The life of 0.05 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the tap water that 20 mL concentration are 8 mg/L to prepare
Object charcoal/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, and foundation adds
Enter the initial concentration of phosphate solution and the phosphate residual concentration of solution after absorption, calculates adsorbance and removal rate.
Embodiment 52:
0.05 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the simulation surface water that 20 mL concentration are 8 mg/L to prepare
Charcoal/ferrihydrite composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 53:
0.05 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the simulated groundwater that 20 mL concentration are 8 mg/L to prepare
Charcoal/ferrihydrite composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 54:
0.05 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the practical surface water that 20 mL concentration are 8 mg/L to prepare
Charcoal/ferrihydrite composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 55:
The phosphate solution for taking the practical seawater that 20 mL concentration are 8 mg/L to prepare is added 0.05 g's in 50 mL centrifuge tubes
Charcoal/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, foundation
The phosphate residual concentration of solution, calculates adsorbance and removal rate after the initial concentration of addition phosphate solution and absorption.
Shown in embodiment 47-55 experimental result such as Figure 10 (B).
Embodiment 56:
The phosphate solution for taking the tap water that 20 mL concentration are 20 mg/L to prepare is added 0.06 g's in 50 mL centrifuge tubes
Charcoal/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, foundation
The phosphate residual concentration of solution, calculates adsorbance and removal rate after the initial concentration of addition phosphate solution and absorption.
Embodiment 57:
The phosphate solution for taking the simulation surface water that 20 mL concentration are 20 mg/L to prepare is added 0.06 in 50 mL centrifuge tubes
The charcoal of g/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 58:
The phosphate solution for taking the simulated groundwater that 20 mL concentration are 20 mg/L to prepare is added 0.06 in 50 mL centrifuge tubes
The charcoal of g/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 59:
The phosphate solution for taking the practical surface water that 20 mL concentration are 20 mg/L to prepare is added 0.06 in 50 mL centrifuge tubes
The charcoal of g/magnetic iron ore composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 60:
0.06 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the practical seawater that 20 mL concentration are 20 mg/L to prepare
Charcoal/magnetic iron ore composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Shown in embodiment 56-60 experimental result such as Figure 10 (B).
Embodiment 61:
The phosphate solution for taking the tap water that 20 mL concentration are 20 mg/L to prepare is added 0.05 g's in 50 mL centrifuge tubes
Charcoal/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, foundation
The phosphate residual concentration of solution, calculates adsorbance and removal rate after the initial concentration of addition phosphate solution and absorption.
Embodiment 62:
The phosphate solution for taking the simulation surface water that 20 mL concentration are 20 mg/L to prepare is added 0.05 in 50 mL centrifuge tubes
The charcoal of g/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 63:
The phosphate solution for taking the simulated groundwater that 20 mL concentration are 20 mg/L to prepare is added 0.05 in 50 mL centrifuge tubes
The charcoal of g/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 64:
The phosphate solution for taking the practical surface water that 20 mL concentration are 20 mg/L to prepare is added 0.05 in 50 mL centrifuge tubes
The charcoal of g/ferrihydrite composite material, vibrates 4 h at room temperature, is then centrifuged, and supernatant is taken to detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Embodiment 65:
0.05 g is added in 50 mL centrifuge tubes in the phosphate solution for taking the practical seawater that 20 mL concentration are 20 mg/L to prepare
Charcoal/ferrihydrite composite material, vibrate 4 h at room temperature, be then centrifuged, take supernatant detect phosphate concn, according to
According to the phosphate residual concentration of solution after the initial concentration and absorption that phosphate solution is added, adsorbance and removal rate are calculated.
Shown in embodiment 61-65 experimental result such as Figure 10 (B).
Claims (8)
1. charcoal/silicon/iron oxide composite material preparation method and application, which is characterized in that the charcoal/ferriferous oxide
Composite material preparation is as follows:
Step 1 prepares charcoal: the shell charcoal after being pyrolyzed at 900 DEG C is crossed 200 meshes；
Step 2 prepares charcoal/magnetic iron ore composite material: weighing 5 g shell charcoals, 7.6 g Iron trichloride hexahydrates and 2.8 g
Four water frerrous chlorides are placed in 250 mL beakers, are dissolved with 100 mL distilled water, are denoted as solution A, another to prepare 1 mol/L NaOH
Solution is denoted as solution B；By solution A ultrasound 0.5h to after mixing, it is added in four-hole boiling flask, in temperature 60 C, 140 r/
1.5 h of min revolving speed and the lower stirring of nitrogen atmosphere protection；Solution B is added dropwise into four-hole boiling flask suspension, it is left to adjust pH to 10
1.5 h are stirred on the right side under 90 DEG C of environment；
Step 3: it prepares charcoal/ferrihydrite composite material: weighing 5 g shell charcoals, 10 g, nine water ferric nitrate is placed in 250
In mL beaker, 50 mL distilled water, 0.5 h of high speed magnetic stirring is added；1 mol/L is added dropwise into above-mentioned mixed solution
KOH adjusts pH about to after 7, continuing to stir 0.5h；
Step 4 after the reaction was completed washs mixed solution to neutrality, and sediment obtains after distinguishing freeze-dried/vacuum drying
Charcoal/silicon/iron oxide composite material；
At room temperature, 0.06 g charcoal/magnetic iron ore composite material is added in the phosphate solution of 20 mL, 8 mg/L, is vibrated
4 h, adsorption rate reach 87.8%；
At room temperature, 0.05 g charcoal/ferrihydrite composite material is added in the phosphate solution of 20 mL, 8 mg/L, is vibrated
4 h, adsorption rate reach 81.0%.
2. the preparation method and application of charcoal/silicon/iron oxide composite material as described in claim 1, feature exist, biology
For charcoal/silicon/iron oxide composite material for phosphate in adsorption aqueous solution, mechanism of action is chemisorption.
3. the preparation method and application of charcoal/silicon/iron oxide composite material as claimed in claim 2, feature exists, described
The adsorption method of phosphate anion are as follows: take 20 mL phosphate solutions in 50 mL centrifuge tubes, it is multiple that charcoal/ferriferous oxide is added
Condensation material vibrates 4 h at room temperature, is then centrifuged, and takes the concentration of supernatant detection phosphate anion, according to addition phosphate radical
The residual concentration of the phosphate anion solution of solution, calculates phosphatic removal rate after the initial concentration of solion and absorption.
4. charcoal/magnetic iron ore the composite material and charcoal/ferrihydrite composite material preparation side as claimed in claim 3
Method and application, which is characterized in that the phosphate concn is respectively 4-60 mg/L and 2-100 mg/L.
5. charcoal/silicon/iron oxide composite material preparation method and application as claimed in claim 4, which is characterized in that
Removal rate highest when phosphate concn is 8 mg/L.
6. the preparation method and application of charcoal/silicon/iron oxide composite material as claimed in claims 1-5, which is characterized in that
Charcoal/silicon/iron oxide composite material adsorbent recycling number is more than or equal to 5.
7. charcoal/silicon/iron oxide composite material preparation method and application as described in claim 1-6, which is characterized in that
When adsorbing phosphate, charcoal/magnetic iron ore composite material and charcoal/ferrihydrite composite material dosage be respectively 0.06g and
0.05 g。
8. charcoal/magnetic iron ore as described in claim 1 and charcoal/ferrihydrite composite material, it is characterised in that Phosphate Sorption
Time of equilibrium adsorption is 120 min and 180 min respectively when hydrochlorate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910745086.3A CN110449125A (en) | 2019-08-13 | 2019-08-13 | Charcoal/silicon/iron oxide composite material preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910745086.3A CN110449125A (en) | 2019-08-13 | 2019-08-13 | Charcoal/silicon/iron oxide composite material preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110449125A true CN110449125A (en) | 2019-11-15 |
Family
ID=68486274
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910745086.3A Pending CN110449125A (en) | 2019-08-13 | 2019-08-13 | Charcoal/silicon/iron oxide composite material preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110449125A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111001387A (en) * | 2019-12-17 | 2020-04-14 | 桂林理工大学 | Preparation method and application of gingko shell morph-genetic Fe/C composite material |
| CN111203180A (en) * | 2020-01-15 | 2020-05-29 | 浙江大学 | Magnetic biochar composite adsorbent and preparation method and application thereof |
| CN113351162A (en) * | 2021-06-07 | 2021-09-07 | 东北农业大学 | Preparation method and application of carbon-based phosphorus-doped ferrihydrite |
| CN113750959A (en) * | 2021-08-10 | 2021-12-07 | 同济大学 | Ferrihydrite @ bone charcoal material capable of synchronously fixing negative and positive heavy metal ions |
| CN113926422A (en) * | 2020-07-13 | 2022-01-14 | 广西大学 | Preparation and application of magnetic bagasse carbon-loaded ferrihydrite composite adsorbent |
| CN113952926A (en) * | 2021-10-08 | 2022-01-21 | 农业农村部环境保护科研监测所 | Method for synchronously removing arsenic and organic pollutants by using loaded ferrihydrite nanoparticle biochar prepared by combining biological/chemical means |
-
2019
- 2019-08-13 CN CN201910745086.3A patent/CN110449125A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111001387A (en) * | 2019-12-17 | 2020-04-14 | 桂林理工大学 | Preparation method and application of gingko shell morph-genetic Fe/C composite material |
| CN111203180A (en) * | 2020-01-15 | 2020-05-29 | 浙江大学 | Magnetic biochar composite adsorbent and preparation method and application thereof |
| CN113926422A (en) * | 2020-07-13 | 2022-01-14 | 广西大学 | Preparation and application of magnetic bagasse carbon-loaded ferrihydrite composite adsorbent |
| CN113351162A (en) * | 2021-06-07 | 2021-09-07 | 东北农业大学 | Preparation method and application of carbon-based phosphorus-doped ferrihydrite |
| CN113351162B (en) * | 2021-06-07 | 2023-03-17 | 东北农业大学 | Preparation method and application of carbon-based phosphorus-doped ferrihydrite |
| CN113750959A (en) * | 2021-08-10 | 2021-12-07 | 同济大学 | Ferrihydrite @ bone charcoal material capable of synchronously fixing negative and positive heavy metal ions |
| CN113952926A (en) * | 2021-10-08 | 2022-01-21 | 农业农村部环境保护科研监测所 | Method for synchronously removing arsenic and organic pollutants by using loaded ferrihydrite nanoparticle biochar prepared by combining biological/chemical means |
| CN113952926B (en) * | 2021-10-08 | 2024-01-23 | 农业农村部环境保护科研监测所 | Method for synchronously removing arsenic and organic pollutants by using ferrihydrite nanoparticle-loaded biochar prepared by combining biological/chemical means |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110449125A (en) | Charcoal/silicon/iron oxide composite material preparation method and application | |
| Li et al. | High efficient separation of U (VI) and Th (IV) from rare earth elements in strong acidic solution by selective sorption on phenanthroline diamide functionalized graphene oxide | |
| Yu et al. | Enhancing phosphate adsorption capacity of SDS-based magnetite by surface modification of citric acid | |
| Kumar et al. | Fabrication of metal ions cross-linked alginate assisted biocomposite beads for selective phosphate removal | |
| Jellali et al. | Adsorption characteristics of phosphorus from aqueous solutions onto phosphate mine wastes | |
| CN110280209B (en) | Water body phosphorus adsorption material and preparation and application methods thereof | |
| JP5674952B2 (en) | Magnetite-bernite mixture, synthesis method thereof and water treatment method | |
| Kajjumba et al. | A review of the application of cerium and lanthanum in phosphorus removal during wastewater treatment: Characteristics, mechanism, and recovery | |
| CN113441108A (en) | Preparation method of modified attapulgite loaded nano zero-valent iron heavy metal adsorbent, product and application thereof | |
| Plohl et al. | Magnetic nanostructures functionalized with a derived lysine coating applied to simultaneously remove heavy metal pollutants from environmental systems | |
| Du et al. | Purification of starch and phosphorus wastewater using core-shell magnetic seeds prepared by sulfated roasting | |
| Li et al. | High-efficient phosphate removal from wastewater by weak magnetic La (OH) 3 modified platanus biochar | |
| Yang et al. | Optimization of the adsorption and removal of Sb (iii) by MIL-53 (Fe)/GO using response surface methodology | |
| Abdelmigeed et al. | Novel easily separable core–shell Fe 3 O 4/PVP/ZIF-8 nanostructure adsorbent: optimization of phosphorus removal from Fosfomycin pharmaceutical wastewater | |
| Kuang et al. | Adsorption kinetics and adsorption isotherm studies of chromium from aqueous solutions by HPAM-chitosan gel beads | |
| US20170349459A1 (en) | Contaminate Removal Using Aluminum-Doped Magnetic Nanoparticles | |
| US20100140179A1 (en) | Porous iron oxide and method for producing the same and method for treating solutions | |
| CN110354798A (en) | A kind of cerium zirconium zinc metal composite adsorbent and the preparation method and application thereof | |
| CN107694542A (en) | A kind of adsorbent for zwitterion absorption and preparation method thereof | |
| CN106914224A (en) | A kind of biological source ferriferous oxide adsorbent and preparation method and application | |
| Cheng et al. | Optimized Ca-Al-La modified biochar with rapid and efficient phosphate removal performance and excellent pH stability | |
| Bai et al. | Magnetized vermiculite loaded with waste polishing powder to recover phosphorus in waste water | |
| AU654449B2 (en) | Process for the removal of phosphorous | |
| Hu et al. | Adsorption of divalent manganese ion on manganese-coated sand | |
| CN113368823A (en) | Magnetically-modified lignite adsorption material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20191115 |
|
| WD01 | Invention patent application deemed withdrawn after publication |