CN107376871B - A kind of high-efficiency adsorbent and the preparation method and application thereof of heavy metal lead ion - Google Patents
A kind of high-efficiency adsorbent and the preparation method and application thereof of heavy metal lead ion Download PDFInfo
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- CN107376871B CN107376871B CN201710640372.4A CN201710640372A CN107376871B CN 107376871 B CN107376871 B CN 107376871B CN 201710640372 A CN201710640372 A CN 201710640372A CN 107376871 B CN107376871 B CN 107376871B
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
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- 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
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a kind of high-efficiency adsorbent and preparation method thereof of heavy metal lead ion, which is composite magnetic nano material Fe3O4/PEG/TiP.The present invention filters out the best preparation method of heavy metal lead ion adsorbent by many experiments, a large number of experiments verifying shows, heavy metal lead ion adsorbent economy provided by the invention, environmental protection, have the function of to adsorb and remove well to lead ion, removal rate is up to 90% or more, and it can desorb and regenerate, it can be widely applied to the adsorption treatment of lead ion in high-concentration waste water, it can overcome at high cost in the prior art, many deficiencies such as Adsorption low efficiency have important social effect and economic benefit.
Description
Technical field
The present invention relates to a kind of heavy metal treatment agents, and in particular to a kind of high-efficiency adsorbent and its system of heavy metal lead ion
Preparation Method belongs to environmental friendly material field.
Background technique
Water occupies very important status in we live as resource indispensable in human development and existence.
However as the growth of population base, the quickening of social urbanization and process of industrialization, water resources ownership per capita is sharply reduced,
Water pollution problems aggravation, seriously affects the sustainable development in China.The reason of causing water pollution includes many aspects, thoughts
Official's contact scar, organic contamination, inorganic pollution (including heavy metal pollution), biologic contamination.Wherein heavy metal pollution is the tightest
One of the problem of weight, because heavy metal is a kind of typical accumulation type pollutant, with the big spy of accumulation, non-degradable, toxicity
Property, finally slow poisoning etc. can be caused to endanger in human body accumulation along food chain by bio-absorbable, enrichment.Most typical example is just
It is canceration caused by minamata disease caused by Itai-itai diseases, Hg caused by Cd pollution and Hg, Cd, As, Pb pollution.Due to heavy metal pollution
Serious harm is caused to ecological environment and human health, many domestic and foreign scholars have developed many improvement heavy metals in succession
Technology.Such as physical method (electric recovery technique, electrode method), chemical method (precipitating, electrolysis, electrochemistry), physical-chemical process (ion
Exchange process, membrane separation process, absorption method), bioanalysis (bio-flocculation process, phytoremediation, animal reparation method) etc..But at existing
Manage low efficiency, it is at high cost the disadvantages of.
Therefore, it is necessary on the basis of existing technology, research and develop a kind of economic, efficiently, environmentally friendly heavy metal lead
The high-efficiency adsorbent of ion.
Summary of the invention
Goal of the invention: It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of raw materials to be easy to get, can be again
It is raw, it is at low cost, it easily promotes and applies, the high-efficiency adsorbent of efficient, economic, environmental protection heavy metal lead ion, another mesh of the invention
The preparation method and applications for being to provide heavy metal lead ion adsorbent.
Technical solution: in order to achieve the object of the present invention, the technical solution adopted by the present invention are as follows:
A kind of high-efficiency adsorbent of heavy metal lead ion, adsorbent are composite magnetic nano material Fe3O4/ PEG/TiP is
Polyethylene glycol-ferroso-ferric oxide (PEG-Fe3O4) load phosphoric acid hydrogen titanium (TiP) adsorbent.
The preparation method of the high-efficiency adsorbent of heavy metal lead ion of the present invention, comprising the following steps:
(1)Fe3O4The preparation of/PEG
Weigh FeSO4·7H2O、Na2S2O3·5H2O is poured into reaction kettle, adds after grinding uniformly in agate mortar
Enter PEG aqueous solution, NaOH solid is then added, is stirred evenly with glass rod, reaction kettle is put into baking oven and is reacted;Reaction terminates
Afterwards, it is dry to be then placed in vacuum with distilled water and dehydrated alcohol centrifuge washing product to pH value of solution close to 7 for cooled to room temperature
Dry case is dried, and ground 160 the polished standard screen is stored in spare in sack;
(2)Fe3O4The preparation of/PEG/TiP
Phosphoric acid solution is pipetted, the Fe that step (1) is prepared is added3O4/ PEG, stirs evenly, under mechanical agitation,
TiCl is added dropwise4Solution reaction is centrifugated after the reaction was completed, with dehydrated alcohol and distillation water washing to pH close to 7, then
Dry in baking oven, composite magnetic nano material Fe is prepared in ground 160 the polished standard screen3O4/PEG/TiP。
Preferably, the preparation method of the high-efficiency adsorbent of above-described heavy metal lead ion, in step (1),
Weigh 2.224g FeSO4·7H2O、0.9926g Na2S2O3·5H2O is poured into 100mL after grinding uniformly in agate mortar
Ptfe autoclave in, addition mass concentration be 0.33g/mLPEG aqueous solution, then be added 4g NaOH solid, use glass
Stick stirs evenly, and reaction kettle is put into 100 DEG C of baking oven and is reacted for 24 hours, after reaction, cooled to room temperature, with distillation
Water and dehydrated alcohol centrifuge washing product are then placed in 100 DEG C of vacuum oven and are dried to pH value of solution close to 7, grind
Cross 160 the polished standard screens.
Preferably, the preparation method of the high-efficiency adsorbent of above-described heavy metal lead ion, in step (2),
The phosphoric acid solution of 250mL 0.6mol/L is pipetted, the Fe that 10g step (1) is prepared is added3O4/ PEG, stirs evenly, in machinery
Under stirring condition, the TiCl of 125mL 0.3mol/L is added dropwise4Solution carries out reaction 8h at 60 DEG C;After the reaction was completed from
Heart separation is dried to pH close in 7,100 DEG C of baking oven, ground 160 the polished standard screen with dehydrated alcohol and distillation water washing.
Preferably, the preparation method of the high-efficiency adsorbent of above-described heavy metal lead ion, PEG molecular weight are
2000 or 4000.
One, craft screening is tested:
(1)Fe3O4The preparation of/PEG
Weigh 2.224g (8mmol) FeSO4·7H2O、0.9926g Na2S2O3·5H2O is ground uniform in agate mortar
It after (about 15min), is poured into the ptfe autoclave of 100mL, it is water-soluble to sequentially add the PEG that 20mL is prepared according to table 1
Liquid (PEG molecular weight is 2000 and 4000), is then added 4g NaOH solid, is stirred evenly with glass rod.Reaction kettle is put into 100
DEG C baking oven in react for 24 hours.After reaction, cooled to room temperature.Extremely with distilled water and dehydrated alcohol centrifuge washing product
PH value of solution is then placed in 100 DEG C of vacuum oven and is dried close to 7.Ground 160 the polished standard screen, is stored in sack
It is interior spare.
The preparation of 1 PEG solution of table
Serial number | PEG mass (g) | Distilled water volume (mL) |
1 | 0 | 20 |
2 | 5 | 15 |
3 | 6.67 | 13.33 |
4 | 10 | 10 |
5 | 15 | 5 |
6 | 20 | 0 |
(2)Fe3O4The preparation of/PEG/TiP
The hydrochloric acid of 2mol/L is prepared: being pipetted the dense HCl of 30.70mL, is diluted with water, is transferred to the volumetric flask of 500mL, constant volume.
The phosphoric acid solution of 0.6mol/L is prepared: 9.00mL concentrated phosphoric acid pipetted, is diluted with water, the volumetric flask of 250mL is transferred to,
Constant volume.
The TiCl of 0.3mol/L4Solution is prepared: being taken the hydrochloric acid solution of appropriate 2mol/L in 100mL beaker, is added
8.30mL titanium tetrachloride, is transferred in the volumetric flask of 250mL, with the hydrochloric acid solution constant volume of 2mol/L.
The phosphoric acid solution of 250mL 0.6mol/L is pipetted, 10g Fe is added3O4/ PEG (screening in advance), stirs evenly, in machine
Under tool stirring condition, the TiCl of 125mL 0.3mol/L is added dropwise4Solution carries out reaction 8h at 60 DEG C.After the reaction was completed
Centrifuge separation is dried to pH close in 7,100 DEG C of baking oven, the standard of ground 160 mesh with dehydrated alcohol and distillation water washing
Sieve, it is spare to be put into sack.
(3) characterization of material --- hysteresis loop test
The Fe that will be prepared according to table 13O4/ PEG carries out hysteresis loop test on vibrating specimen magnetometer, the results are shown in Table 2.
2 Fe of table3O4The saturation magnetization of/PEG-4000
As seen from Table 2, generally, with the increase of PEG dosage/ratio, Fe3O4The saturation magnetization of/PEG is successively decreased.Together
When, all Fe containing PEG3O4/ PEG sample is insoluble in the HCl solution of 0.1mol/L, so using in subsequent experimental
PEG:H2The Fe that O mass ratio synthesizes under conditions of being 1:33O4/ PEG carries out TiP load test.And the experimental results showed that Fe3O4/
The specific saturation magnetization of 1:3 ratio is 40.08emu/g in PEG2000, is lower than Fe3O4/PEG4000。
(4) the influence experiment of pH factor
The concentrated nitric acid solution for pipetting 50mL distilled water and 3mL pours into the beaker of 100mL, accurate that 1.5984g nitric acid is added
Lead, stirring and dissolving are transferred in the volumetric flask of 1000mL, are cleaned three times with the beaker of distilled water rinse 100mL, constant volume obtains
Pb2+Concentration is the solution of 1000mg/L.25mL is taken to prepare the lead standard liquid of 50mg/L in the volumetric flask of 500mL after shaking up.
The lead titer of seven groups of 50mL 50mg/L is pipetted into 250mL conical flask, be respectively adjusted to 3.0 with pH instrument, 3.5,
4.0,4.5,5.0,5.5,6.0, it is separately added into 0.1000g Fe3O4It is put into after/PEG/TiP sample in complete warm oscillator at 25 DEG C
The lower oscillation for carrying out 2h.Solution after filtering oscillation, takes filtrate with flame atomic absorption spectrometry plumbum ion concentration.PH is research
Important object of the material to the heavy metal adsorption influential effect factor.Fig. 1 show different pH value (3.0,3.5,4.0,4.5,
5.0, Fe when 5.5,6.0)3O4/ PEG/TiP composite material is to Pb2+Adsorption effect.It can be seen from the figure that composite material pair
Pb2+Adsorbance increase sharply when pH is in 2.8-3.5, tend to be steady in 3.5-5.5, particularly preferred pH value be 5.
When solution ph is lower, H in solution+Concentration it is higher can with other ions generate competition, keep lead ion separate
The adsorption effect of adsorbent, adsorbent reduces.With the increase of pH, H in solution+Concentration gradually decreases, lead ion and compound suction
The repulsion on attached dose of surface accordingly reduces, therefore the adsorption capacity of adsorbent increases, although pH increases the absorption that can improve adsorbent
Ability, but it is once excessively high lead ion can be made to precipitate, such case will affect the subsequent recycling to adsorbent.Therefore it selects
PH=5 is Optimal pH, at this moment both generates removal rate or very high simultaneously without sediment.
(5) influence of ionic strength
Prepare 2mol/L NaCl solution (taking 11.7g NaCl in constant volume in the volumetric flask of 100mL), take respectively 0mL,
The 2mol/LNaCl solution of 1.25mL, 3.75mL, 7.5mL, 15mL, 20mL and the lead standard liquid of 25mL 100mg/L are in 50mL capacity
In bottle, with deionized water constant volume, preparation obtain NaCl concentration be 0mol/L, 0.05mol/L, 0.15mol/L, 0.3mol/L,
0.6mol/L、0.8mol/L、Pb2+Concentration is the mixed solution of 50mg/L.PH value is adjusted to 5,0.1000g Fe is added3O4/
PEG/TiP sample reacts 2h at 25 DEG C.The concentration of filtrate is surveyed with atomic absorption spectrophotometer, calculates adsorbance.
By Fig. 2 it is known that with NaCl concentration raising, magnetic composite Fe3O4/ PEG/TiP is to Pb2+Absorption
Ability gradually decreases, this may be due to the Na in solution+With Pb2+Competitive Adsorption is generated, when the concentration of NaCl solution is
When 0.6mol/L, adsorbent has reached 5.704mg/g to the adsorbance of lead ion, and 23.4% when for no ion interference lowers
It is very much, therefore Na present in solution+It is unfavorable for magnetic composite Fe3O4/ PEG/TiP is to Pb2+Absorption, but still better than
Many adsorbents.
(6) screening of adsorption time
The lead titer of eight groups of 50mL 50mg/L is pipetted into 250mL conical flask, pH is respectively adjusted to pH meter and adds for 5
The composite material for entering 0.1000g, be respectively put into oscillator vibrated at 15 DEG C, 25 DEG C, 35 DEG C 10min, 30min, 45min,
It is filtered after 60min, 90min, 120min, 150min, 180min.Take filtrate dense with flame atomic absorption spectrometry lead ion
Degree, and calculated equilibrium adsorbance.
As shown in figure 3, at the same temperature, composite material is divided into two stages, first stage to the absorption of lead ion
For the quick adsorption stage, adsorbance is quicklyd increase with being incremented by for time, and especially in 40min, second stage is balance
Stage, adsorbance tend to balance with being incremented by for time.And at a temperature of different within the same time, adsorbance is with temperature
Raising and increase, illustrating that temperature increases will increase the adsorption effect of adsorbent, be conducive to absorption of the adsorbent to lead ion.?
In the past, saturation has not been reached yet in the time of contact of adsorbent and lead ion to 45min, and the absorption point bit comparison of adsorbent surface is more,
Adsorption capacity is stronger, and adsorbance rapidly increases;The time of contact of adsorbent and lead ion, which increases, after 45min makes surface
Point is reduced, and point is adsorbed after 120min and is largely reduced, adsorbance tends to balance.It is thus determined that the Best Times of adsorbent
For 120min.
(6) desorption experiment
Adsorption experiment: taking the lead solution 50mL of eight groups of 60mg/L to pour into the conical flask of 250mL, adjust pH to 5, respectively plus
Enter 0.1000g sample, 2h is reacted at 25 DEG C, filters, Pb in filtrates tested2+Solid is placed in 100 DEG C of baking oven and does by content
It is dry.
Desorption experiment: crossing 160 mesh standard sieves for the sample after drying, and the dilute HCl solution of 50mL 0.5mol/L is taken (to take
21.5mL concentrated hydrochloric acid dissolves in constant volume to the volumetric flask of 500mL), it pours into the conical flask of seven groups of 250mL, every group of above-mentioned baking of addition
Dry sample 0.1000g, which is put into oscillator, vibrates 2h, and filtering measures Pb in filtrate2+Solid is placed on 100 DEG C of baking by content
It is dry in case.It repeats above-mentioned absorption-desorption process 3 times.Adsorbent reuse 3 adsorbances be respectively 54.29mg/g,
52.48mg/g, 51.49mg/g, fall is smaller, and desorption effect is good (desorption efficiency 90% or so), illustrates magnetic coupling material
Material can reuse.
The utility model has the advantages that the high-efficiency adsorbent of heavy metal lead ion provided by the invention compared to the prior art have it is following excellent
Point:
1, the present invention filters out Fe by a large number of experiments3O4/ PEG/TiP adsorbent, experiment show have absorption well high
The effect of lead ion in concentration waste water has good governance role to pollution of waterhead.
2, Fe provided by the invention3O4The preparation process of/PEG/TiP adsorbent filters out optimal work by a large number of experiments
The Fe with fine adsorpting lead ion performance can be efficiently prepared in skill parameter3O4/ PEG/TiP adsorbent.
3, the present invention screens different pH value by many experiments, different temperatures, adsorption time, the conditions such as adsorbent reactivation,
Filter out the optimum condition of adsorpting lead ion, verifying shows adsorbent economy provided by the invention, environmental protection, to high-concentration waste water
In lead ion removal rate up to 85% or more, can be widely applied to the processing of the industrial wastewater containing lead ion, can overcome existing
There is at high cost in technology, an Adsorption low efficiency, many deficiencies such as adsorbent cannot regenerate have important social effect.
Detailed description of the invention
Fig. 1 is the curve graph of influence situation of the different pH value to adsorption effect.
Fig. 2 is that ionic strength adsorbs Pb to sample2+Influence curve graph.
Fig. 3 is the curve graph that different time influences adsorption effect under different reaction temperatures.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention
The modification of form falls within the application range as defined in the appended claims.
Embodiment 1
A kind of preparation method of the high-efficiency adsorbent of heavy metal lead ion, comprising the following steps:
(1)Fe3O4The preparation of/PEG
Weigh 2.224g FeSO4·7H2O、0.9926g Na2S2O3·5H2O, after being ground uniformly in agate mortar,
Enter into the ptfe autoclave of 100mL, addition mass concentration is 0.33g/mL PEG4000 aqueous solution, and 4g is then added
NaOH solid, is stirred evenly with glass rod, reaction kettle is put into 100 DEG C of baking oven and is reacted for 24 hours, after reaction, natural cooling
100 DEG C of vacuum oven is then placed in room temperature with distilled water and dehydrated alcohol centrifuge washing product to pH value of solution close to 7
It is dried, ground 160 the polished standard screen.
(2)Fe3O4The preparation of/PEG/TiP
The phosphoric acid solution of 250mL 0.6mol/L is pipetted, the Fe that 10g step (1) is prepared is added3O4/ PEG, stirring are equal
It is even, under mechanical agitation, the TiCl of 125mL 0.3mol/L is added dropwise4Solution carries out reaction 8h at 60 DEG C;Reaction
It is centrifugated, is dried to pH close in 7,100 DEG C of baking oven with dehydrated alcohol and distillation water washing, ground 160 mesh after the completion
Standard screen, composite magnetic nano material Fe is prepared3O4/PEG/TiP。
The sample of synthesis is characterized using X ' the Pert Powder X-ray diffractometer of Dutch Panaco company, spoke
Penetrating source is AlKα, wavelength isTesting tube presses 40kV, tube current 40mA.
The sample of detection is the above-mentioned Fe being prepared3O4/ PEG and Fe3O4/ PEG/TiP, the results showed that 2 θ=30.10 °,
The diffraction maximums such as 35.45 °, 56.98 °, 62.57 ° are corresponding with (PDF#65-3107), are the Fe of cubic spinel structure3O4.When
Fe3O4After the unformed TiP of/PEG area load, Fe3O4Diffraction peak intensity declined, especially at 30.10 ° and 56.98 °
It is more obvious.Since TiP is unformed form, without strong diffraction maximum, so in Fe3O4Obviously do not become on/PEG/TiP curve
Change.
Fe3O4、Fe3O4/PEG、Fe3O4The infrared spectrogram of/PEG/TiP the result shows that, in 3432cm-1The width nearby occurred
Peak is the stretching vibration of O-H, 1616cm-1Place is the OH flexural vibrations peak of physical bond water, 581cm-1For the characteristic absorption of Fe-O
Peak.Fe3O4In the infrared figure of/PEG sample, 1238cm-1-1021cm-1The peak of range be PEG absorption peak, show PEG at
Function is wrapped in Fe3O4Surface.
Fe3O4In the infrared spectrogram of/PEG/TiP, PEG and Fe3O4Characteristic peak reduction, there is 1037cm-1The vibration at place
Dynamic peak, this is PO4 3-Tetrahedral asymmetric stretching vibration peak.
Each adsorbent absorption property of embodiment 2 compares
The present invention compares the absorption property of various adsorbents, and specific experiment the results are shown in Table shown in 3:
The maximal absorptive capacity of the different adsorbents of table 3 compares
Adsorbent | Adsorbance qm(mg/g) | Condition |
Shell-core structure Fe3O4/MnO2 | 142 | T=25 DEG C |
Fe3O4/ chitosan | 105.5 | PH=5 T=25 DEG C |
Fe3O4/PAA/ATP | 35.44 | PH=5 |
Wheat straw biologic charcoal | 17.38 | T=25 DEG C |
Nano ferriferrous oxide | 10.44 | T=10 DEG C |
TiP-NaCMC-Fe3O4 | 46.78 | PH=5 T=25 DEG C |
Fe3O4/PEG/TiP | 61.47 | PH=5 T=25 DEG C |
According to the fitting result of Langmuir model, Fe that the present invention is prepared3O4/PEG/TiP adsorbent absorption property
Better than Fe3O4/ PAA/ATP, wheat straw biologic charcoal, nano ferriferrous oxide and TiP-NaCMC-Fe3O4.But absorption property is weak
In shell-core structure Fe3O4/MnO2、Fe3O4/ chitosan.
3 lead ion of embodiment adsorbs clearance test
2 parts of industrial wastewater of the 10L containing lead ion is taken, puts into the Fe that the embodiment of the present invention 1 is prepared respectively3O4/PEG/
TiP 20g, adjustment reaction temperature are 35 DEG C, and adjustment wastewater pH is 5, and the reaction time is 120 minutes, calculate Pb In Exhausted Water ion
Removal rate is respectively 91.7% and 90.5%, shows the Fe that the present invention is prepared3O4/ PEG/TiP adsorbent has to be inhaled well
The effect of attached removal Pb In Exhausted Water ion.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of preparation method of the high-efficiency adsorbent of heavy metal lead ion, which is characterized in that adsorbent is composite magnetic nanometer
Material Fe3O4/PEG/TiP;
The preparation method of heavy metal lead ion high-efficiency adsorbent, comprising the following steps:
(1)Fe3O4The preparation of/PEG
Weigh 2.224g FeSO4·7H2O、0.9926g Na2S2O3·5H2O is poured into after grinding uniformly in agate mortar
In the ptfe autoclave of 100mL, addition mass concentration is 0.33g/mL PEG aqueous solution, and it is solid that 4g NaOH is then added
Body is stirred evenly with glass rod, reaction kettle is put into 100 DEG C of baking oven and is reacted for 24 hours, after reaction, cooled to room temperature,
With distilled water and dehydrated alcohol centrifuge washing product to pH value of solution close to 7, it is then placed in 100 DEG C of vacuum oven and is done
Dry, ground 160 the polished standard screen is stored in spare in sack;
(2)Fe3O4The preparation of/PEG/TiP
The phosphoric acid solution of 250mL 0.6mol/L is pipetted, the Fe that 10g step (1) is prepared is added3O4/ PEG, stirs evenly,
Under mechanical agitation, the TiCl of 125mL 0.3mol/L is added dropwise4Solution carries out reaction 8h at 60 DEG C;Reaction is completed
After be centrifugated, with dehydrated alcohol and distillation water washing to pH dry, the mark of ground 160 mesh close in 7,100 DEG C of baking oven
Quasi- sieve, is prepared composite magnetic nano material Fe3O4/PEG/TiP。
2. the preparation method of the high-efficiency adsorbent of heavy metal lead ion according to claim 1, which is characterized in that PEG points
Son amount is 2000 or 4000.
3. a kind of high-efficiency adsorbent adsorption treatment metal of the heavy metal lead ion obtained with preparation method described in claim 1
Lead ion method, which is characterized in that the condition of processing are as follows: the reaction time is 40~120 minutes, and reaction temperature is 15~35 DEG C,
PH is 5, and adsorbent dosage is 1g/mL to 2g/mL.
4. the high-efficiency adsorbent for the heavy metal lead ion that preparation method described in claim 1 obtains processing containing heavy metal lead from
Application in sub- waste water.
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