CN108745302A - A kind of magnetic modified oyster removes the preparation method of lead absorbent - Google Patents
A kind of magnetic modified oyster removes the preparation method of lead absorbent Download PDFInfo
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- CN108745302A CN108745302A CN201810522379.0A CN201810522379A CN108745302A CN 108745302 A CN108745302 A CN 108745302A CN 201810522379 A CN201810522379 A CN 201810522379A CN 108745302 A CN108745302 A CN 108745302A
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
-
- 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
A kind of magnetic modified oyster removes the preparation method of lead absorbent, belongs to technical field of absorbent.Specific preparation process is as follows：It takes oyster shell to clean, drying, is then ground to powder；By the ultrasonic disperse into the water of the fine powder after grinding, FeCl is then added3Solution and FeCl2Lye and hydrazine hydrate are added after mixing for solution, and then heating water bath, is filtered after being cooled to room temperature；Filtrate is cleaned, is then dried；Dried product exhibited is put into flyash and sludge, stands, then dries at room temperature；Mixture crushes after will be dry, is put into Muffle furnace and is pyrolyzed, then crushes thermal decomposition product, and the magnetic modified oyster is finally made and removes lead absorbent.The raw material that the method for the invention is used is simple and easy to get, environmentally safe, and the magnetic modified oyster of preparation is excellent except lead absorbent properties.It is 20 mg/L in waste liquid initial concentration, under the conditions of adsorption time is 1h, 1g samples are 96.9 ~ 99.4% except lead rate.
Description
Technical field
The invention belongs to technical field of absorbent, and in particular to a kind of magnetic modified oyster removes the preparation side of lead absorbent
Method.
Background technology
Application of the lead in modern industrial and agricultural production is very extensive, and at the same time, lead causes to provide air, soil and water again
The pollution in source.Lead and soluble lead salt are all toxic, and lead waste water has seriously environment, health and crop growth
Harm.With the development of society, the pollution of the heavy metals such as Pb In Exhausted Water is in the trend persistently aggravated.
Common waste water deleading technology mainly has following a few major class：First, the precipitation method, it is removed by the way that chemical reaction occurs
Go heavy metal ions in wastewater, including neutralization precipitation method, sulphide precipitation, ferrite coprecipitation, chemical reduction method, electrification
Learn reduction method and high molecular heavy metals trapping agent method etc.；Second is that making the heavy metal in waste water in the condition for not changing its chemical form
The lower method being adsorbed, concentrated, detached, including absorption, solvent extraction, evaporation and freezing method, ion exchange and UF membrane etc.；
Third, by the method that the effects that flocculation of microorganism or plant, absorption, accumulation, enrichment removes heavy metal in waste water, including life
Object flocculation, biochemical process and plant ecological reparation etc..Wherein absorption method has processing as a kind of traditional water technology
Capacity is big, can remove each metal ion species and acid ion, it is simple for process, easy to operate, treatment effeciency is high the advantages that, at present still
It is one of the main method for administering lead waste water.
Oyster shell has special physique, contains a large amount of 2~10 μm of micropores, makes it have stronger adsorption capacity, friendship
The effects that transducing power and catalytic decomposition, is the inorganic adsorbent for preparing of primary raw material with nontoxic using oyster shell, does not generate secondary
The advantages that pollution, adsorption capacity is strong, at low cost, adsorption effect is good, service life is long, the waste water of new generation for becoming great potential are inhaled
Attached dose.But simple oyster shell lead adsorption capacity is slow, adsorption efficiency is low and adsorption energy force difference, needs to be modified.
Invention content
The technical issues of solution：In view of the above technical problems, a kind of magnetic modified oyster of present invention offer removes lead absorbent
Preparation method, have the advantages that raw material is simple and easy to get, environmentally safe, the adsorbent adsorption time of preparation is short, adsorbance
Greatly, secondary pollution will not be caused.
Technical solution：A kind of magnetic modified oyster removes the preparation method of lead absorbent, and the preparation method includes following step
Suddenly：
Step 1 weighs the cleaning of 20~25 mass parts oyster shells, drying, and it is 100~200 μm thin to be then ground to granularity
Powder；
Fine powder after grinding is put into 30~40 mass parts water by step 2, then 30~50min of ultrasonic disperse is added
10~15 mass parts 2mol/LFeCl3Solution and 5~12 mass parts 2mol/LFeCl2Solution is uniformly mixed under the protection of nitrogen,
Then pH value of solution is adjusted to 10~12, and 0.2~0.4 mass parts hydrazine hydrate is added, mixed liquor is heated 4 in 80~90 DEG C of water-baths
~6h is filtered after being cooled to room temperature；
Step 3 cleaned filtered product with deionized water, then 60~80 DEG C of dry 4~6h under nitrogen atmosphere；
2~4 mass parts flyash and 10~20 mass parts sludge are added into dried product exhibited by step 4, stir evenly,
It is put into blast drier after standing 12~15h at room temperature, dry 10~11h at a temperature of 100~120 DEG C；
It is 10~20 mesh that mixture after drying is crushed to grain size by step 5, is then placed in Muffle furnace 300~450
It is pyrolyzed 30~45min at a temperature of DEG C, thermal decomposition product is crushed to 40~60 mesh, the magnetic modified oyster is finally made except lead is inhaled
Receive agent.
Preferably, weighing the cleaning of 25 mass parts oyster shells, drying in the step 1, it is 150 μ to be then ground to granularity
The fine powder of m.
Preferably, the fine powder after grinding is put into 35 mass parts water in the step 2, ultrasonic disperse 40min, so
After 13 mass parts 2mol/L FeCl are added3Solution and 7 mass parts 2mol/L FeCl2Solution is uniformly mixed under the protection of nitrogen,
Then pH value of solution is adjusted to 10, and 0.3 mass parts hydrazine hydrate is added, mixed liquor is heated into 5h in 85 DEG C of water-baths, is cooled to room temperature
After filter.
Preferably, cleaned filtered product with deionized water in the step 3, then under nitrogen atmosphere 70 DEG C it is dry
Dry 5h.
Preferably, sludge includes water, ash content, volatile matter and fixed carbon, wherein water content in the step 4
10.49wt.%, content of ashes 27.31wt.%, volatile matter 51.65wt.%, fixed carbon 10.55wt.%.
Preferably, 3 mass parts flyash and 15 mass parts sludge are added in the step 4 into dried product exhibited, stir
It mixes uniformly, is put into blast drier after standing 13h at room temperature, dry 10.5h at a temperature of 110 DEG C.
Preferably, it is 15 mesh that mixture after drying, which is crushed to grain size, in the step 5, it is then placed in Muffle furnace
It is pyrolyzed 40min at a temperature of 400 DEG C, thermal decomposition product is crushed to 50 mesh, the magnetic modified oyster is finally made except lead absorbs
Agent.
Advantageous effect：The method of the invention is auxiliary material by major ingredient, flyash and sludge of magnetic modified oyster, is used
Raw material is simple and easy to get, environmentally safe, and the magnetic modified oyster of preparation is excellent except lead absorbent properties.In waste liquid initial concentration
For 20mg/L, under the conditions of adsorption time is 1h, 1g samples are 96.9~99.4% except lead rate.The adsorbent adsorption time of preparation
Short, large amount of adsorption will not cause secondary pollution.
Specific implementation mode
Embodiment 1
A kind of magnetic modified oyster removes the preparation method of lead absorbent, and the preparation method comprises the following steps：
Step 1 weighs the cleaning of 20 mass parts oyster shells, drying, is then ground to the fine powder that granularity is 100 μm.
Fine powder after grinding is put into 30 mass parts water by step 2, then 10 mass parts are added in ultrasonic disperse 30min
2mol/LFeCl3Solution and 5 mass parts 2mol/LFeCl2Solution under the protection of nitrogen be uniformly mixed, then adjust pH value of solution to
10,0.2 mass parts hydrazine hydrate is added, mixed liquor is heated into 4h in 80 DEG C of water-baths, is filtered after being cooled to room temperature.
Step 3 cleaned filtered product with deionized water, then 60 DEG C of dry 4h under nitrogen atmosphere.
2 mass parts flyash and 10 mass parts sludge are added into dried product exhibited by step 4, stir evenly, in room temperature
Be put into blast drier after lower standing 12h, dry 10h at a temperature of 100 DEG C, the sludge include water, ash content, volatile matter and
Fixed carbon, wherein water content 10.49wt.%, content of ashes 27.31wt.%, volatile matter 51.65wt.%, fixed carbon
10.55wt.%.
It is 10 mesh that mixture after drying is crushed to grain size by step 5, is then placed in Muffle furnace hot at a temperature of 300 DEG C
30min is solved, thermal decomposition product is crushed to 40 mesh, the magnetic modified oyster is finally made and removes lead absorbent.
Embodiment 2
A kind of magnetic modified oyster removes the preparation method of lead absorbent, and the preparation method comprises the following steps：
Step 1 weighs the cleaning of 25 mass parts oyster shells, drying, is then ground to the fine powder that granularity is 200 μm.
Fine powder after grinding is put into 40 mass parts water by step 2, then 15 mass parts are added in ultrasonic disperse 50min
2mol/LFeCl3Solution and 12 mass parts 2mol/LFeCl2Solution is uniformly mixed under the protection of nitrogen, then adjusts pH value of solution
To 12,0.4 mass parts hydrazine hydrate is added, mixed liquor is heated into 6h in 90 DEG C of water-baths, is filtered after being cooled to room temperature.
Step 3 cleaned filtered product with deionized water, then 80 DEG C of dry 6h under nitrogen atmosphere.
4 mass parts flyash and 20 mass parts sludge are added into dried product exhibited by step 4, stir evenly, in room temperature
Be put into blast drier after lower standing 15h, dry 11h at a temperature of 120 DEG C, the sludge include water, ash content, volatile matter and
Fixed carbon, wherein water content 10.49wt.%, content of ashes 27.31wt.%, volatile matter 51.65wt.%, fixed carbon
10.55wt.%.
It is 20 mesh that mixture after drying is crushed to grain size by step 5, is then placed in Muffle furnace hot at a temperature of 450 DEG C
45min is solved, thermal decomposition product is crushed to 60 mesh, the magnetic modified oyster is finally made and removes lead absorbent.
Embodiment 3
A kind of magnetic modified oyster removes the preparation method of lead absorbent, and the preparation method comprises the following steps：
Step 1 weighs the cleaning of 25 mass parts oyster shells, drying, is then ground to the fine powder that granularity is 150 μm.
Fine powder after grinding is put into 35 mass parts water by step 2, then 13 mass parts are added in ultrasonic disperse 40min
2mol/LFeCl3Solution and 7 mass parts 2mol/LFeCl2Solution under the protection of nitrogen be uniformly mixed, then adjust pH value of solution to
10,0.3 mass parts hydrazine hydrate is added, mixed liquor is heated into 5h in 85 DEG C of water-baths, is filtered after being cooled to room temperature.
Step 3 cleaned filtered product with deionized water, then 70 DEG C of dry 5h under nitrogen atmosphere.
3 mass parts flyash and 15 mass parts sludge are added into dried product exhibited by step 4, stir evenly, in room temperature
It is put into blast drier after lower standing 13h, dry 10.5h at a temperature of 110 DEG C, the sludge includes water, ash content, volatile matter
And fixed carbon, wherein water content 10.49wt.%, content of ashes 27.31wt.%, volatile matter 51.65wt.%, fixed carbon
10.55wt.%.
It is 15 mesh that mixture after drying is crushed to grain size by step 5, is then placed in Muffle furnace hot at a temperature of 400 DEG C
40min is solved, thermal decomposition product is crushed to 50 mesh, the magnetic modified oyster is finally made and removes lead absorbent.
Comparative example 1
With embodiment 3, difference lies in flyash is not added, specific preparation process is as follows：
Step 1 weighs the cleaning of 25 mass parts oyster shells, drying, is then ground to the fine powder that granularity is 150 μm.
Fine powder after grinding is put into 35 mass parts water by step 2, then 13 mass parts are added in ultrasonic disperse 40min
2mol/LFeCl3Solution and 7 mass parts 2mol/LFeCl2Solution under the protection of nitrogen be uniformly mixed, then adjust pH value of solution to
10,0.3 mass parts hydrazine hydrate is added, mixed liquor is heated into 5h in 85 DEG C of water-baths, is filtered after being cooled to room temperature.
Step 3 cleaned filtered product with deionized water, then 70 DEG C of dry 5h under nitrogen atmosphere.
15 mass parts sludge are added into dried product exhibited by step 4, stir evenly, and are put into after standing 13h at room temperature
In blast drier, dry 10.5h at a temperature of 110 DEG C, the sludge includes water, ash content, volatile matter and fixed carbon, wherein water
Content 10.49wt.%, content of ashes 27.31wt.%, volatile matter 51.65wt.%, fixed carbon 10.55wt.%.
It is 15 mesh that mixture after drying is crushed to grain size by step 5, is then placed in Muffle furnace hot at a temperature of 400 DEG C
40min is solved, thermal decomposition product is crushed to 50 mesh, the magnetic modified oyster is finally made and removes lead absorbent.
The waste water that leaded initial concentration is 20mg/L is configured at room temperature, is then divided into four groups, every group and 50mL is taken to configure
Lead waste water, be separately added into magnetic modified oyster prepared by 1g Examples 1 to 3 and comparative example 1 and remove lead adsorbent, concussion absorption
After 1h, with TAS-986 type atomic adsorption spectrophotometric determination plumbum ion concentrations, adsorbance Qe(mg/g) it indicates, calculates public
Formula is as follows：
V is the volume (mL) of solution in formula；c0For Pb in waste water before processing2+Concentration (mg/L)；ceFor processed waste water
Middle Pb2+Concentration (mg/L)；M is the quality (g) of adsorbent.
Except lead rate η (%) calculation formula is as follows：
Except lead rate result of calculation is as follows：
| Except lead rate/% | |
| Embodiment 1 | 96.9 |
| Embodiment 2 | 97.8 |
| Embodiment 3 | 99.4 |
| Comparative example 1 | 89.3 |
Claims (7)
1. a kind of magnetic modified oyster removes the preparation method of lead absorbent, which is characterized in that the preparation method includes following step
Suddenly：
Step 1 weighs the cleaning of 20 ~ 25 mass parts oyster shells, drying, is then ground to the fine powder that granularity is 100 ~ 200 μm；
Fine powder after grinding is put into 30 ~ 40 mass parts water by step 2,30 ~ 50 min of ultrasonic disperse, is then added 10 ~ 15
2 mol/L FeCl of mass parts32 mol/L FeCl of solution and 5 ~ 12 mass parts2Solution is uniformly mixed under the protection of nitrogen, so
PH value of solution is adjusted afterwards to 10 ~ 12, and 0.2 ~ 0.4 mass parts hydrazine hydrate is added, mixed liquor is heated into 4 ~ 6 h in 80 ~ 90 DEG C of water-baths,
It is filtered after being cooled to room temperature；
Step 3 cleaned filtered product with deionized water, then 60 ~ 80 DEG C of 4 ~ 6 h of drying under nitrogen atmosphere；
2 ~ 4 mass parts flyash and 10 ~ 20 mass parts sludge are added into dried product exhibited by step 4, stir evenly, in room temperature
It is put into blast drier after 12 ~ 15 h of lower standing, dry 10 ~ 11 h at a temperature of 100 ~ 120 DEG C；
It is 10 ~ 20 mesh that mixture after drying is crushed to grain size by step 5, is then placed in Muffle furnace in 300 ~ 450 DEG C of temperature
30 ~ 45 min of lower pyrolysis, 40 ~ 60 mesh are crushed to by thermal decomposition product, and the magnetic modified oyster is finally made and removes lead absorbent.
2. a kind of magnetic modified oyster according to claim 1 removes the preparation method of lead absorbent, which is characterized in that described
The cleaning of 25 mass parts oyster shells, drying are weighed in step 1, are then ground to the fine powder that granularity is 150 μm.
3. a kind of magnetic modified oyster according to claim 1 removes the preparation method of lead absorbent, which is characterized in that described
The fine powder after grinding is put into 35 mass parts water in step 2, then 13 mass parts, 2 mol/L is added in 40 min of ultrasonic disperse
FeCl32 mol/L FeCl of solution and 7 mass parts2Solution is uniformly mixed under the protection of nitrogen, then adjusting pH value of solution to 10,
0.3 mass parts hydrazine hydrate is added, mixed liquor is heated into 5 h in 85 DEG C of water-baths, is filtered after being cooled to room temperature.
4. a kind of magnetic modified oyster according to claim 1 removes the preparation method of lead absorbent, which is characterized in that described
Filtered product was cleaned with deionized water in step 3, then 70 DEG C of 5 h of drying under nitrogen atmosphere.
5. a kind of magnetic modified oyster according to claim 1 removes the preparation method of lead absorbent, which is characterized in that described
Sludge includes water, ash content, volatile matter and fixed carbon, wherein 10.49 wt.% of water content, content of ashes 27.31 in step 4
Wt.%, 51.65 wt.% of volatile matter, 10.55 wt.% of fixed carbon.
6. a kind of magnetic modified oyster according to claim 1 removes the preparation method of lead absorbent, which is characterized in that described
3 mass parts flyash and 15 mass parts sludge are added in step 4 into dried product exhibited, stirs evenly, stands 13 at room temperature
It is put into blast drier after h, dry 10.5 h at a temperature of 110 DEG C.
7. a kind of magnetic modified oyster according to claim 1 removes the preparation method of lead absorbent, which is characterized in that described
It is 15 mesh that mixture after drying, which is crushed to grain size, in step 5, is then placed in Muffle furnace and is pyrolyzed 40 at a temperature of 400 DEG C
Thermal decomposition product is crushed to 50 mesh by min, and the magnetic modified oyster is finally made and removes lead absorbent.
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| CN201810522379.0A CN108745302A (en) | 2018-05-28 | 2018-05-28 | A kind of magnetic modified oyster removes the preparation method of lead absorbent |
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| CN201810522379.0A CN108745302A (en) | 2018-05-28 | 2018-05-28 | A kind of magnetic modified oyster removes the preparation method of lead absorbent |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005255737A (en) * | 2004-03-09 | 2005-09-22 | Sumitomo Osaka Cement Co Ltd | Method for producing heavy metal adsorbent from waste and heavy metal adsorbent obtained by the method |
| CN104174378A (en) * | 2013-05-26 | 2014-12-03 | 青岛国强环保科技有限公司 | Nanometer composite material efficiently adsorbing lead-containing wastewater |
| CN104549126A (en) * | 2015-01-28 | 2015-04-29 | 福建农林大学 | Nano iron/oyster shell composite material, and preparation method and application thereof |
| CN105709699A (en) * | 2016-04-18 | 2016-06-29 | 华中科技大学 | Soil heavy metal adsorbent and preparation method thereof |
| CN106582513A (en) * | 2016-12-22 | 2017-04-26 | 郑州丽福爱生物技术有限公司 | Composite adsorption material for treatment of heavy metal wastewater and preparation method thereof |
-
2018
- 2018-05-28 CN CN201810522379.0A patent/CN108745302A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005255737A (en) * | 2004-03-09 | 2005-09-22 | Sumitomo Osaka Cement Co Ltd | Method for producing heavy metal adsorbent from waste and heavy metal adsorbent obtained by the method |
| CN104174378A (en) * | 2013-05-26 | 2014-12-03 | 青岛国强环保科技有限公司 | Nanometer composite material efficiently adsorbing lead-containing wastewater |
| CN104549126A (en) * | 2015-01-28 | 2015-04-29 | 福建农林大学 | Nano iron/oyster shell composite material, and preparation method and application thereof |
| CN105709699A (en) * | 2016-04-18 | 2016-06-29 | 华中科技大学 | Soil heavy metal adsorbent and preparation method thereof |
| CN106582513A (en) * | 2016-12-22 | 2017-04-26 | 郑州丽福爱生物技术有限公司 | Composite adsorption material for treatment of heavy metal wastewater and preparation method thereof |
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Application publication date: 20181106 |