CN104923160B - Preparation method for adsorbing the composite of heavy metal ion in stain disease - Google Patents
Preparation method for adsorbing the composite of heavy metal ion in stain disease Download PDFInfo
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Abstract
The present invention is used for the preparation method of the composite for adsorbing heavy metal ion in stain disease, is related to porosu solid adsorbent composite, and the composite is the composite of mineral nano fiber powder and foamy carbon, and step is：Prepare the mineral nano fiber powder with inner porosity；Template prepares light weight and porous foamy carbon；Mineral nano fiber powder is combined with foamy carbon, is obtained for adsorbing the mineral nano fiber powder of heavy metal ion in stain disease and the composite of foamy carbon.The present invention overcomes the complicated condition, big power consumption, high cost that the adsorbent adsorption efficiency that is currently used for heavy metal-containing wastewater treatment is high, preparation technology needs and it is not easy to the defect for reclaiming.
Description
Technical field
Technical scheme is related to porosu solid adsorbent composite, is particularly used for weight in absorption stain disease
The preparation method of the composite of metal ion.
Background technology
With the quickening of the fast-developing and modernization of industrial or agricultural, the blowdown flow rate of industrial wastewater is also growing day by day.Work
The discharge of industry waste water highly impacts the quality of people's daily life drinking-water, the discharge and pollution of particularly heavy metal-polluted waste water
The environmental problem that people extremely pay close attention to is turned into.Heavy metal-polluted waste water is essentially from two aspects：One is the various productions work of the mankind
It is dynamic to have discharged substantial amounts of heavy metal substance and be flowed into lake, river, the inferior area in ocean and ground, water pollution is caused, cause
Biocoene in the physicochemical properties and water body of water body changes, and reduces water body value；Two is in China one
A little areas based on extensive economy mode, indivedual enterprises neglect ecological environments only demand profit maximization, in addition to containing weight
The utilization ratio of the raw material of metal is low, causes unit output value to discharge excessive containing heavy metal-polluted waste water.Heavy metal-polluted wastewater toxicity
By force, but also with persistence and the features such as non-degradable, excessively enrichment can be caused greatly to environment and human body in nature
Harm, therefore, develop efficiently and be easy to reclaim the adsorbent for the Adsorption of Heavy Metals ion from stain disease very weigh
Will.
Natural minerals nano-fiber material adsorbent has unique structure, thus with good absorption and ion exchange
Performance, and cheap, rich reserves, make it have preferable application prospect in stain disease treatment.Foamy carbon is a kind of
With carbon atom as skeleton, the lightweight solid carbon materials of the porous network structure mutually piled up between carbon atom and formed.Carbon foam
With chemical stability higher, larger specific surface area, the characteristic such as relatively low thermal coefficient of expansion and hole higher, using model
Enclose widely.However, because powdered natural minerals nano-fiber material has extremely strong water imbibition, viscosity is big after water suction,
Separation and recovery poor performance, although shaping natural minerals nano-fiber material solves separation problem, but absorption property again not as good as powder
Last shape mineral nano fibrous material is excellent.CN102600803A discloses the preparation of the adsorbent for heavy metal-containing wastewater treatment
Method, it is raw material to choose city domestic sewage treatment plant dewatered sludge, by alkali lye extraction, ethanol precipitation, centrifugation and low
The step that temperature is dried prepares a kind of adsorbent for heavy metal-containing wastewater treatment.Its defect is：1. dewatered sludge is used,
By after dehydration, determined depending on the efficiency of the property and dehydration equipment of sludge and sediment its moisture percentage in sewage sludge can be reduced to 55%~
80%, the condition that preparation technology needs is complex, and power consumption is big, and high cost is unfavorable for industrialized production；2. the absorption of product is imitated
Rate is not high.
The content of the invention
The technical problems to be solved by the invention are：Composite for adsorbing heavy metal ion in stain disease is provided
Preparation method, the composite is the composite of mineral nano fiber and foamy carbon, chooses raw material for inexpensively and with good
The mineral fibres powder of good suction-operated, and deep processing treatment is carried out to it, prepare the mineral with inner porosity and receive
Rice fiber powder, then the light porous foamy carbon prepared with template is combined, and is fired into block, is overcome well existing
The complicated condition that adsorbent adsorption efficiency is high, preparation technology needs, power consumption for heavy metal-containing wastewater treatment are big, high cost
With the defect for being not easy to reclaim.
The present invention solves the technical scheme that is used of the technical problem：For adsorbing answering for heavy metal ion in stain disease
The preparation method of condensation material, the composite is the composite of mineral nano fiber powder and foamy carbon, and specific steps are such as
Under：
The first step, prepares the mineral nano fiber powder with inner porosity：
Take 300~500g and crossed the mineral fibres powder of 20~30 mesh sieves and be placed in the beaker of 5000mL, add 2500~
The deionized water of 3500mL and the hydrochloric acid solution that 250~350mL mass percent concentrations are 36%, with 1200~1700r/min
Rotating speed 0.5~1.5h of dispersion into slurries, by slurries filtering and washing repeatedly, until pH value is neutrality, obtains filter cake at a high speed；Will
The filter cake is placed in baking oven and 24h to drying is dried at a temperature of 60~80 DEG C, then ground 20~30 mesh sieve, then is entered with airflow milling
The treatment of row supersonic airstream depth solution beam, is obtained the mineral nano fiber powder with inner porosity, and its granularity is
10nm~50nm, aperture is 2nm~50nm, stand-by；
Second step, template prepares light weight and porous foamy carbon：
(2.1) polyamic acid solution is prepared：In 500mL beakers, the analytically pure DMA 40 of addition~
96mL, then by concentration for the 20~30mL of polyamic acid solution of 24wt% pours into this beaker, after stirring, it is 5 to obtain concentration
The polyamic acid solution of~15wt%,
(2.2) dipping of polyurethane foam：By the polyurethane foam of 0.1~0.3g in the polyamic acid obtained by (2.1) step
0.5~1.5h is impregnated in solution, the compound foams of polyurethane foam and liquid carbon source are obtained,
(2.3) extruding of compound foams：The polyurethane foam that polyamic acid solution is obtained is impregnated in taking-up (2.2) step
With the compound foams of liquid carbon source, extruded under 10~15MPa with mould,
(2.4) drying of compound foams：Compound foams after (2.3) step is extruded are put into vacuum drying chamber,
8~12h is dried at 60~80 DEG C, vacuum is 100Pa,
(2.5) charing of compound foams：Compound foams after solidification are placed in quartz boat, in tubular electric resistance
Heated up with the speed of 10~20 DEG C/min in stove, charing process carried out in the nitrogen atmosphere that gas flow rate is 30~40mL/min,
Condition is, charing final temperature is 800~1000 DEG C, and constant temperature time is 1~2h, then naturally cools to and be obtained after room temperature light weight and many
The foamy carbon in hole；
3rd step, mineral nano fiber powder is combined with foamy carbon：
Mineral nano fiber powder obtained in the first step is placed in 500mL beakers, plus deionized water is made into mixed liquor, Gu
Liquid mass ratio is 1:10, light weight obtained in second step and porous foamy carbon are put into after impregnating 0.5-1.5h in above-mentioned mixed liquor
Take out, mineral nano fiber powder is 1 with the mass ratio of foamy carbon:1~2, being put into batch-type furnace carries out 400~600 DEG C of sintering,
2~3h of insulation, is obtained the composite for adsorbing heavy metal ion in stain disease, and the composite is mineral nano fiber
The composite of powder and foamy carbon.
The above-mentioned preparation method for adsorbing the composite of heavy metal ion in stain disease, the mineral fibres powder is
Sepiolite fibre powder or palygorskite fiber powder.
The beneficial effects of the invention are as follows：Compared with prior art, the substantive distinguishing features of protrusion of the invention and marked improvement
It is as follows：
(1) because mineral fibres powder to be made the inventive method the mineral nano fiber powder with inner porosity
Body, the powder plays the synergy of Adsorption of Heavy Metals ion with the porous foamy carbon bar matrix of light weight, is removing removing heavy metals
The efficiency of ion no matter from adsorptivity in theory, or be significantly improved in practical application, received than single mineral
The adsorption efficiency of rice fiber powder improves 150%, and there is not yet has the report of correlative study.
(2) what prepared by the inventive method is porous for adsorbing the composite light weight of heavy metal ion in stain disease, and is
Block, is highly convenient for recycling.
(3) it is cheap and with the mineral fibres powder of good adsorption effect that the inventive method chooses raw material, and it is entered
Row deep processing is processed, and prepares the mineral nano fiber powder with inner porosity, then many with lightweight prepared by template
Hole foamy carbon is combined, and is fired into block, and the adsorbent absorption for being currently used for heavy metal-containing wastewater treatment is overcome well
Complicated condition that inefficient, preparation technology needs, big power consumption, high cost and it is not easy to the defect for reclaiming.
Specific embodiment
Embodiment 1
The first step, prepares the mineral nano fiber powder with inner porosity：
Take 300g and crossed the sepiolite fibre powder of 20 mesh sieves and be placed in the beaker of 5000mL, add the deionization of 2500mL
Water and the hydrochloric acid solution that 250mL mass percent concentrations are 36%, 0.5h is disperseed at a high speed with the rotating speed of 1200r/min into slurries,
By slurries filtering and washing repeatedly, until pH value is neutrality, filter cake is obtained；The filter cake is placed in baking oven and is dried at a temperature of 60 DEG C
To drying, then ground 20 mesh sieve, then the treatment of supersonic airstream depth solution beam is carried out with airflow milling is obtained in having 24h
The sepiolite nanometer fibre powder of portion's loose structure, its granularity is 10nm~50nm, and aperture is 2nm~50nm, stand-by；
Second step, template prepares light weight and porous foamy carbon：
(2.1) polyamic acid solution is prepared：In 500mL beakers, analytically pure DMA 96mL is added,
Again by concentration for the polyamic acid solution 20mL of 24wt% pours into this beaker, after stirring, the polyamides that concentration is 5wt% is obtained
Amino acid solution,
(2.2) dipping of polyurethane foam：By the polyurethane foam of 0.1g in the polyamic acid solution obtained by (2.1) step
Dipping 0.5h, obtains the compound foams of polyurethane foam and liquid carbon source,
(2.3) extruding of compound foams：The polyurethane foam that polyamic acid solution is obtained is impregnated in taking-up (2.2) step
With the compound foams of liquid carbon source, extruded under 10MPa with mould,
(2.4) drying of compound foams：Compound foams after (2.3) step is extruded are put into vacuum drying chamber,
12h is dried at 60 DEG C, vacuum is 100Pa,
(2.5) charing of compound foams：Compound foams after solidification are placed in quartz boat, in tubular electric resistance
Heated up with the speed of 15 DEG C/min in stove, charing process is carried out in gas flow rate is for the nitrogen atmosphere of 30mL/min, condition is, charcoal
It is 800 DEG C to change final temperature, and constant temperature time is 2h, and light weight and porous foamy carbon is obtained after then naturally cooling to room temperature；
3rd step, mineral nano fiber powder is combined with foamy carbon：
Sepiolite nanometer fibre powder with inner porosity obtained in the first step is placed in 500mL beakers, plus
Deionized water is made into mixed liquor, and solid-liquid mass ratio is 1:10, light weight obtained in second step and porous foamy carbon are put into above-mentioned
Taken out after 1h is impregnated in mixed liquor, sepiolite nanometer fibre powder and light weight and porous foamy carbon with inner porosity
Mass ratio be 1:1, being put into batch-type furnace carries out 400 DEG C of sintering, is incubated 3h, is obtained for adsorbing heavy metal ion in stain disease
Composite, the composite is the composite of sepiolite nanometer fibre powder and foamy carbon.
The composite for adsorbing heavy metal ion in stain disease is obtained with the present embodiment, to containing Ag+、Cd2+、Cr3+
Waste water etc. heavy metal ion is adsorbed, and concentration of heavy metal ion is 100mg/L, and the consumption of composite is waste water weight
1.2%.It is 3 to adjust pH value with dilute HCl (0.1mol/L) and NaOH (0.1mol/L), composite and waste water dispersed with stirring 30
After minute, sedimentation filtration, heavy metal ion content in analysis supernatant.Wherein Ag+Clearance be 90%, Cd2+Clearance
It is 92%, Cr3+Clearance be 87%.
Embodiment 2
The first step, prepares the mineral nano fiber powder with inner porosity：
Take 500g and crossed the palygorskite fiber powder of 20 mesh sieves and be placed in the beaker of 5000mL, add the deionization of 3000mL
Water and the hydrochloric acid solution that 300mL mass percent concentrations are 36%, 1h into slurries is disperseed at a high speed with the rotating speed of 1450r/min, will
Slurries filtering and washing repeatedly, until pH value is neutrality, obtains filter cake；The filter cake is placed in baking oven and is dried at a temperature of 70 DEG C
To drying, then ground 25 mesh sieve, then the treatment of supersonic airstream depth solution beam is carried out with airflow milling is obtained in having 24h
The Palygorskite Nanometer fiber powder of portion's loose structure, its granularity is 10nm~50nm, and aperture is 2nm~50nm, stand-by；
Second step, template prepares light weight and porous foamy carbon：
(2.1) polyamic acid solution is prepared：In 500mL beakers, analytically pure DMA 72mL is added,
Again by concentration for the polyamic acid solution 30mL of 24wt% pours into this beaker, after stirring, concentration gathering for 10wt% is obtained
Acid amides acid solution,
(2.2) dipping of polyurethane foam：By the polyurethane foam of 0.2g in the polyamic acid solution obtained by (2.1) step
Dipping 1h, obtains the compound foams of polyurethane foam and liquid carbon source,
(2.3) extruding of compound foams：The polyurethane foam that polyamic acid solution is obtained is impregnated in taking-up (2.2) step
With the compound foams of liquid carbon source, extruded under 12MPa with mould,
(2.4) drying of compound foams：Compound foams after (2.3) step is extruded are put into vacuum drying chamber,
10h is dried at 70 DEG C, vacuum is 100Pa,
(2.5) charing of compound foams：Compound foams after solidification are placed in quartz boat, in tubular electric resistance
Heated up with the speed of 15 DEG C/min in stove, charing process is carried out in gas flow rate is for the nitrogen atmosphere of 35mL/min, condition is, charcoal
It is 900 DEG C to change final temperature；Constant temperature time is 1.5h, and light weight and porous foamy carbon is obtained after then naturally cooling to room temperature；
3rd step, mineral nano fiber powder is combined with foamy carbon：
Palygorskite Nanometer fiber powder with inner porosity obtained in the first step is placed in 500mL beakers, plus
Deionized water is made into mixed liquor, and solid-liquid mass ratio is 1:10, light weight obtained in second step and porous foamy carbon are put into above-mentioned
Taken out after 1.5h is impregnated in mixed liquor, Palygorskite Nanometer fiber powder and light weight and porous foam with inner porosity
The mass ratio of carbon is 1:1.5, being put into batch-type furnace carries out 500 DEG C of sintering, is incubated 2.5h, is obtained for adsorbing a huge sum of money in stain disease
Belong to the composite of ion, the composite is the composite of Palygorskite Nanometer fiber powder and foamy carbon.
The composite for adsorbing heavy metal ion in stain disease is obtained with the present embodiment, to containing Ag+、Cd2+、Cr3+
Waste water etc. heavy metal ion is adsorbed, and concentration of heavy metal ion is 100mg/L, and the consumption of composite is waste water weight
1.2%.It is 3 to adjust pH value with dilute HCl (0.1mol/L) and NaOH (0.1mol/L), composite and waste water dispersed with stirring 30
After minute, sedimentation filtration, heavy metal ion content in analysis supernatant.Wherein Ag+Clearance be 91%, Cd2+Clearance
It is 93%, Cr3+Clearance be 89%.
Embodiment 3
The first step, prepares the mineral nano fiber powder with inner porosity：
Take 500g and crossed the sepiolite fibre powder of 30 mesh sieves and be placed in the beaker of 5000mL, add the deionization of 3500mL
Water and the hydrochloric acid solution that 350mL mass percent concentrations are 36%, 1.5h is disperseed at a high speed with the rotating speed of 1700r/min into slurries,
By slurries filtering and washing repeatedly, until pH value is neutrality, filter cake is obtained；The filter cake is placed in baking oven and is dried at a temperature of 80 DEG C
To drying, then ground 30 mesh sieve, then the treatment of supersonic airstream depth solution beam is carried out with airflow milling is obtained in having 24h
The sepiolite nanometer fibre powder of portion's loose structure, its granularity is 10nm~50nm, and aperture is 2nm~50nm, stand-by；
Second step, template prepares light weight and porous foamy carbon：
(2.1) polyamic acid solution is prepared：In 500mL beakers, analytically pure DMA 40mL is added,
Again by concentration for the polyamic acid solution 25mL of 24wt% pours into this beaker, after stirring, concentration gathering for 15wt% is obtained
Acid amides acid solution,
(2.2) dipping of polyurethane foam：By the polyurethane foam of 0.3g in the polyamic acid solution obtained by (2.1) step
Dipping 1.5h, obtains the compound foams of polyurethane foam and liquid carbon source,
(2.3) extruding of compound foams：The polyurethane foam that polyamic acid solution is obtained is impregnated in taking-up (2.2) step
With the compound foams of liquid carbon source, extruded under 15MPa with mould,
(2.4) drying of compound foams：Compound foams after (2.3) step is extruded are put into vacuum drying chamber,
8h is dried at 80 DEG C, vacuum is 100Pa,
(2.5) charing of compound foams：Compound foams after solidification are placed in quartz boat, in tubular electric resistance
Heated up with the speed of 20 DEG C/min in stove, charing process is carried out in gas flow rate is for the nitrogen atmosphere of 40mL/min, condition is, charcoal
It is 1000 DEG C to change final temperature；Constant temperature time is 1h, and light weight and porous foamy carbon is obtained after then naturally cooling to room temperature；
3rd step, mineral nano fiber powder is combined with foamy carbon：
Sepiolite nanometer fibre powder with inner porosity obtained in the first step is placed in 500mL beakers, plus
Deionized water is made into mixed liquor, and solid-liquid mass ratio is 1:10, light weight obtained in second step and porous foamy carbon are put into above-mentioned
Taken out after 0.5h is impregnated in mixed liquor, sepiolite nanometer fibre powder and light weight and porous foam with inner porosity
The mass ratio of carbon is 1:2, being put into batch-type furnace carries out 600 DEG C of sintering, is incubated 2h, be obtained for adsorb in stain disease heavy metal from
The composite of son, the composite is the composite of sepiolite nanometer fibre powder and foamy carbon.
The composite for adsorbing heavy metal ion in stain disease is obtained with the present embodiment, to containing Ag+、Cd2+、Cr3+
Waste water etc. heavy metal ion is adsorbed, and concentration of heavy metal ion is 100mg/L, and the consumption of composite is waste water weight
1.2%.It is 3 to adjust pH value with dilute HCl (0.1mol/L) and NaOH (0.1mol/L), composite and waste water dispersed with stirring 30
After minute, sedimentation filtration, heavy metal ion content in analysis supernatant.Wherein Ag+Clearance be 89%, Cd2+Clearance
It is 91%, Cr3+Clearance be 86%.
Embodiment 4
In addition to mineral fibres powder is palygorskite fiber powder, other are with embodiment 1.
Embodiment 5
In addition to mineral fibres powder is sepiolite fibre powder, other are with embodiment 2.
Embodiment 6
In addition to mineral fibres powder is palygorskite fiber powder, other are with embodiment 3.
Claims (1)
1. be used for adsorb heavy metal ion in stain disease composite preparation method, it is characterised in that：The composite
It is the composite of mineral nano fiber powder and foamy carbon, comprises the following steps that：
The first step, prepares the mineral nano fiber powder with inner porosity：
Take 300~500g and crossed the mineral fibres powder of 20~30 mesh sieves and be placed in the beaker of 5000mL, add 2500~
The deionized water of 3500mL and the hydrochloric acid solution that 250~350mL mass percent concentrations are 36%, with 1200~1700r/min
Rotating speed 0.5~1.5h of dispersion into slurries, by slurries filtering and washing repeatedly, until pH value is neutrality, obtains filter cake at a high speed；Will
The filter cake is placed in baking oven and 24h to drying is dried at a temperature of 60~80 DEG C, then ground 20~30 mesh sieve, then is entered with airflow milling
The treatment of row supersonic airstream depth solution beam, is obtained the mineral nano fiber powder with inner porosity, and its granularity is
10nm~50nm, aperture is 2nm~50nm, stand-by；
Second step, template prepares light weight and porous foamy carbon：
(2.1) polyamic acid solution is prepared：In 500mL beakers, analytically pure 40~96mL of DMA is added,
Again by concentration for the 20~30mL of polyamic acid solution of 24wt% pours into this beaker, after stirring, obtain concentration for 5~
The polyamic acid solution of 15wt%,
(2.2) dipping of polyurethane foam：By the polyurethane foam of 0.1~0.3g in the polyamic acid solution obtained by (2.1) step
0.5~1.5h of middle dipping, obtains the compound foams of polyurethane foam and liquid carbon source,
(2.3) extruding of compound foams：Polyurethane foam and liquid that polyamic acid solution is obtained are impregnated in taking-up (2.2) step
The compound foams of state carbon source, are extruded with mould under 10~15MPa,
(2.4) drying of compound foams：Compound foams after (2.3) step is extruded are put into vacuum drying chamber, 60
8~12h is dried at~80 DEG C, vacuum is 100Pa,
(2.5) charing of compound foams：Compound foams after solidification are placed in quartz boat, in tube type resistance furnace
Heated up with the speed of 10~20 DEG C/min, charing process, condition are carried out in the nitrogen atmosphere that gas flow rate is 30~40mL/min
It is that charing final temperature is 800~1000 DEG C, and constant temperature time is 1~2h, then naturally cools to and be obtained after room temperature light weight and porous
Foamy carbon；
3rd step, mineral nano fiber powder is combined with foamy carbon：
Mineral nano fiber powder obtained in the first step is placed in 500mL beakers, plus deionized water is made into mixed liquor, solid-liquid matter
Amount is than being 1:10, light weight obtained in second step and porous foamy carbon are put into after impregnating 0.5-1.5h in above-mentioned mixed liquor and taken
Go out, mineral nano fiber powder is 1 with the mass ratio of foamy carbon:1~2, being put into batch-type furnace carries out 400~600 DEG C of sintering, protects
2~3h of temperature, is obtained the composite for adsorbing heavy metal ion in stain disease, and the composite is mineral nano fiber powder
The composite of body and foamy carbon.
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| CN107082467B (en) * | 2017-03-20 | 2020-10-30 | 中国科学院合肥物质科学研究院 | Iron oxyhydroxide nanorod/foam carbon composite material and preparation method and application thereof |
| CN108160033B (en) * | 2018-01-04 | 2020-07-28 | 河北工业大学 | Preparation method of activated clay reinforced ultra-light foam carbon |
| CN115403162A (en) * | 2022-08-03 | 2022-11-29 | 中国石油化工股份有限公司 | Foam carbon-based zero-valent iron material, preparation method thereof and application thereof in permeable reactive barrier |
| CN116332672B (en) * | 2023-05-19 | 2023-12-01 | 太仓百川水处理设备有限公司 | Ceramic-based multi-Kong Wu water treatment agent and preparation method thereof |
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