CN103212376A - Preparation method of nanometer CuS grafting modified bamboo powder capable of adsorbing heavy metal ions - Google Patents
Preparation method of nanometer CuS grafting modified bamboo powder capable of adsorbing heavy metal ions Download PDFInfo
- Publication number
- CN103212376A CN103212376A CN2013101363830A CN201310136383A CN103212376A CN 103212376 A CN103212376 A CN 103212376A CN 2013101363830 A CN2013101363830 A CN 2013101363830A CN 201310136383 A CN201310136383 A CN 201310136383A CN 103212376 A CN103212376 A CN 103212376A
- Authority
- CN
- China
- Prior art keywords
- bamboo powder
- cus
- nanometer
- preparation
- heavy metal
- 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
Abstract
The invention discloses a preparation method of nanometer CuS grafting modified bamboo powder capable of adsorbing heavy metal ions. The preparation method can be used for producing a heavy metal ion bio-adsorbent which is large in adsorption capacity, high in adsorption speed and good in stability. The preparation method comprises the steps of: synthesis of nanometer CuS colloid: slowly dropwise adding a thioacetamide aqueous alcohol solution into a copper sulphate aqueous alcohol solution with the same volume; pretreatment of bamboo powder: soaking the bamboo powder in a sodium hydroxide solution, and performing suction filtering and filter residue drying; preparation of nanometer CuS grafting modified bamboo powder: putting the pretreated bamboo powder into a thioglycolic acid aqueous solution, adding the nanometer CuS colloid and drying; and finally testing the adsorption performance. The preparation method provided by the invention is simple, convenient to operate, low in cost, high in adsorption rate with the average adsorption rate being as high as above 95%, and large in adsorption capacity. The nanometer CuS grafting modified bamboo powder can be recycled and is environment-friendly and pollution-free. The bio-adsorbent produced by using the preparation method can be widely applied to the treatment of water body containing heavy metal pollutants.
Description
Technical field
The present invention relates to the preparation method of the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions material and preparation method thereof, particularly a kind of Adsorption of Heavy Metal Ions.
Background technology
Along with industrialization and fast development of urbanization, a large amount of undressed heavy metal contaminants that contain enter water body, and the water environment pollution problem is more and more serious.Heavy metal contaminants has characteristics such as high toxicity, persistence, difficult degradation, is one of pollutant to environment and human survival harm maximum.Biosorption process has abundant raw materials as a kind of emerging heavy metal removal technology, and operating cost is low, and heavy metal is easy to separate advantages such as recovery, has become environmental pollution control field one big research focus.Chinese patent open (bulletin) number: CN 102247814A, " biomass adsorbent and the process for treating heavy-metal waste water that are used for heavy metal containing wastewater treatment " disclosed, this method is simple, and heavy metal ion in the water is had the good adsorption performance.But this type of biological adsorption agent also comes with some shortcomings on commercial Application: the one, and adsorption rate is slow, and absorption mainly depends on porous character and its limited active function groups of sorbing material itself; The 2nd, the saturated back of adsorbents adsorb is difficult for resolving, and reclaims heavy metal by chemical reduction method cost is increased; The 3rd, sorbing material can't regenerate and reuse, and tends to cause secondary pollution by incinerating to smelt.
Nano material is a kind of adsorbent efficiently that rose in recent years, it has dimensional effect, good dispersion, huge specific area and surface free energy, easy other functionalization functional group of grafting, can strengthen multiple interfacial reaction and other material incomparable features such as a large amount of adsorption sites, scholars have studied and have used TiO
2, nano materials such as MnS, ZnS, ZnO remove heavy metal ions in wastewater.
Summary of the invention
The invention provides a kind of preparation method of nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions, the production adsorption capacity is big, adsorption rate fast and the heavy metal ion biological adsorption agent of good stability.
The preparation method who is used for the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions provided by the invention may further comprise the steps:
A. synthesis of nano CuS colloid: the thioacetamide water-alcohol solution slowly is added drop-wise in the equal-volume copper sulphate water-alcohol solution, stir, both mol ratios are 3:1 or 1:3, drip and finish back continuation stirring, be transferred to after reacting completely in the micro-wave digestion reactor, micro-wave digestion, reaction obtains nanometer CuS colloid after finishing, and the taking-up lucifuge is standby;
B. bamboo powder preliminary treatment: at first to clean the back through running water and deionized water dry for the bamboo powder, mistake 80 mesh sieves.Then the bamboo powder is immersed in 0.1～0.5mol/L sodium hydroxide solution, magnetic agitation is suction filtration after 12～24 hours, and it is that neutral back is dry that filter residue is washed till pH with deionized water, gets preliminary treatment bamboo powder;
C. prepare nanometer CuS grafting modification bamboo powder: it is 2.5～10% TGA aqueous solution that preliminary treatment bamboo powder is placed weight percent concentration, add 2～5mL acetate and 0.2～0.5mL concentrated sulfuric acid, behind stirring at room 10～20h, add nanometer CuS colloid 25～50mL, mix the back and slowly stir 15～30min, filter, it is that neutral back is dry that filter residue is washed till pH with deionized water, gets nanometer CuS grafting modification bamboo powder;
D. detect absorption property: at ambient temperature, getting 0.05g nanometer CuS grafting modification bamboo powder, to join 25mL concentration respectively be 50mg/L Cu
2+, 50mg/L Cd
2+, 50mg/L Mn
2+, 50mg/L Zn
2+, 50mg/L Ni
2+With 100mg/L Pb
2+In the solution.Filter behind the ultrasonic concussion 15min,, calculate adsorption rate η (%) according to following formula with the heavy metal solution concentration before and after the atomic absorption spectroscopy determination absorption:
In the formula: C
0Be the initial concentration of metal ion, mg/L; C
eThe concentration of metal ion during for adsorption equilibrium, mg/L.
Described thioacetamide water-alcohol solution of step a and copper sulphate water-alcohol solution are with thioacetamide and copper sulphate joins deionized water respectively and the ethanol ratio is formulated in the water-alcohol solution of 1:1.
The present invention compares its significant beneficial effect with existing similar technology and is embodied in:
1. the preparation method is simple, and is easy to operate, with low cost.The present invention adopt one-step method the direct grafting of nanometer CuS to bamboo powder surface, and the bamboo powder is the byproduct of bamboo deep processing, raw material sources are extensive, and are cheap and easy to get, compare cost with conventional resins type sorbing material and reduce significantly.
2. adsorption rate height, adsorption capacity is big.The nanometer CuS grafting modification bamboo powder that obtains through the present invention has demonstrated the good adsorption performance to heavy metal ion, as Cu
2+, Cd
2+, Mn
2+, Zn
2+, Ni
2+, Pb
2+Deng, average adsorption rate is up to more than 95%.
3. adsorption rate is fast, and regeneration is simple, can be recycled, and is environment friendly and pollution-free.Compare with sorbing materials such as traditional active carbon, mineral matters, the biological adsorption agent of this method preparation can reach adsorption equilibrium in 30 minutes, used nanometer CuS grafting modification bamboo powder can be regenerated with the ultrasonic concussion of acid solution, nanometer CuS grafting modification bamboo powder is reusable, and can not produce secondary pollution to environment.
The specific embodiment
With embodiment the present invention is described in further details below.
Embodiment 1
Be used for the preparation method of the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions, the small-scale production step is as follows:
(1) thioacetamide and copper sulphate are joined deionized water and ethanol respectively than in the water-alcohol solution of 1:1, be mixed with thioacetamide water-alcohol solution and copper sulphate water-alcohol solution;
(2) with 100mL concentration be 210mol/L thioacetamide water-alcohol solution slowly to be added drop-wise to 100mL concentration be in the 70mmol/L copper sulphate water-alcohol solution, stir simultaneously.Drip and finish back continuation stirring 30min, make to react completely.Be transferred to then in the micro-wave digestion reactor, under power 180W, micro-wave digestion 1h.Microwave naturally cools to room temperature after finishing, and gets nanometer CuS colloid, and low-temperature dark is standby;
(3) the bamboo powder is cleaned the back through running water and deionized water dry 24h in 70 ℃ of drying box, and mistake 80 mesh sieves are standby;
(4) get 25g bamboo powder in the 500mL conical flask, adding 500mL concentration is the 0.1mol/L sodium hydroxide solution, magnetic agitation 24h, suction filtration and to be washed till pH with deionized water be neutral subsequently, 70 ℃ of oven dry 24h in drying box, preliminary treatment bamboo powder;
(5) getting 10g preliminary treatment bamboo powder, to place the 100mL volumetric concentration be 5% TGA solution, add the 5mL acetate and the 0.5mL concentrated sulfuric acid, behind the stirring at room 20h, add nanometer CuS colloid 50mL, mix the back and slowly stir 30min, filter, it is neutral back in 60 ℃ of vacuum drying chamber inner dryings that filter residue is washed till pH with deionized water, gets nanometer CuS grafting modification bamboo powder.After testing, this nanometer CuS grafting modification bamboo powder is to Cu
2+, Cd
2+, Mn
2+, Zn
2+, Ni
2+And Pb
2+Adsorption rate be respectively 97.8%, 99.0%, 97.5%, 96.5%, 95.5% and 98.3%.
Embodiment 2
Be used for the preparation method of the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions, the small-scale production step is as follows:
(1) with embodiment 1;
(2) with embodiment 1;
(3) with embodiment 1;
(4) get 25g bamboo powder in the 500mL conical flask, adding 200mL concentration is the 0.5mol/L sodium hydroxide solution, magnetic agitation 24h, suction filtration and to be washed till pH with deionized water be neutral subsequently, 70 ℃ of oven dry 24h in drying box, preliminary treatment bamboo powder;
(5) getting 10g preliminary treatment bamboo powder, to place the 100mL volumetric concentration be 10% TGA solution, add the 5mL acetate and the 0.5mL concentrated sulfuric acid, behind the stirring at room 20h, add nanometer CuS colloid 50mL, mix the back and slowly stir 30min, filter, it is neutral back in 60 ℃ of vacuum drying chamber inner dryings that filter residue is washed till pH with deionized water, gets nanometer CuS grafting modification bamboo powder.After testing, this nanometer CuS grafting modification bamboo powder is to Cu
2+, Cd
2+, Mn
2+, Zn
2+, Ni
2+And Pb
2+Adsorption rate be respectively 98.8%, 99.0%, 98.2%, 97.7%, 96.7% and 99.0%.
Embodiment 3
Be used for the preparation method of the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions, the small-scale production step is as follows:
(1) with embodiment 1;
(2) with embodiment 1;
(3) with embodiment 1;
(4) get 10g bamboo powder in the 500mL conical flask, adding 100mL concentration is the 0.5mol/L sodium hydroxide solution, magnetic agitation 24h, suction filtration and to be washed till pH with deionized water be neutral subsequently, 70 ℃ of oven dry 24h in drying box, preliminary treatment bamboo powder;
(5) getting 5g preliminary treatment bamboo powder, to place the 100mL volumetric concentration be 2.5% TGA solution, add the 2mL acetate and the 0.2mL concentrated sulfuric acid, behind the stirring at room 10h, add nanometer CuS colloid 25mL, mix the back and slowly stir 15min, filter, it is neutral back in 60 ℃ of vacuum drying chamber inner dryings that filter residue is washed till pH with deionized water, gets nanometer CuS grafting modification bamboo powder.After testing, this nanometer CuS grafting modification bamboo powder is to Cu
2+, Cd
2+, Mn
2+, Zn
2+, Ni
2+And Pb
2+Adsorption rate be respectively 97.3%, 99.5%, 98.5%, 98.1%, 97.2% and 98.4%.
Embodiment 4
Be used for the preparation method of the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions, the small-scale production step is as follows:
(1) with embodiment 1;
(2) with 100mL concentration be 70mol/L thioacetamide water-alcohol solution slowly to be added drop-wise to 100mL concentration be in the 210mmol/L copper sulphate water-alcohol solution, stir simultaneously.Drip and finish back continuation stirring 30min, make to react completely.Be transferred to then in the micro-wave digestion reactor, under power 180W, micro-wave digestion 1h.Microwave naturally cools to room temperature after finishing, and gets nanometer CuS colloid, and low-temperature dark is standby;
(3) with embodiment 1;
(4) with embodiment 1;
(5) getting 10g preliminary treatment bamboo powder, to place the 100mL volumetric concentration be 5% TGA solution, add the 5mL acetate and the 0.5mL concentrated sulfuric acid, behind the stirring at room 20h, add nanometer CuS colloid 50mL, mix the back and slowly stir 30min, filter, it is neutral back in 60 ℃ of vacuum drying chamber inner dryings that filter residue is washed till pH with deionized water, gets nanometer CuS grafting modification bamboo powder.After testing, this nanometer CuS grafting modification bamboo powder is to Cu
2+, Cd
2+, Mn
2+, Zn
2+, Ni
2+And Pb
2+Adsorption rate be respectively 97.2%, 98.8%, 97.9%, 96.9%, 95.3% and 97.7%.
Embodiment 5
Be used for the preparation method of the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions, the small-scale production step is as follows:
(1) with embodiment 1;
(2) with 100mL concentration be 70mol/L thioacetamide water-alcohol solution slowly to be added drop-wise to 100mL concentration be in the 210mmol/L copper sulphate water-alcohol solution, stir simultaneously.Drip and finish back continuation stirring 30min, make to react completely.Be transferred to then in the micro-wave digestion reactor, under power 180W, micro-wave digestion 1h.Microwave naturally cools to room temperature after finishing, and gets nanometer CuS colloid, and low-temperature dark is standby;
(3) with embodiment 1;
(4) get 10g bamboo powder in the 500mL conical flask, adding 100mL concentration is the 0.5mol/L sodium hydroxide solution, magnetic agitation 24h, suction filtration and to be washed till pH with deionized water be neutral subsequently, 70 ℃ of oven dry 24h in drying box, preliminary treatment bamboo powder;
(5) getting 5g preliminary treatment bamboo powder, to place the 100mL volumetric concentration be 2.5% TGA solution, add the 2mL acetate and the 0.2mL concentrated sulfuric acid, behind the stirring at room 10h, add nanometer CuS colloid 25mL, mix the back and slowly stir 15min, filter, it is neutral back in 60 ℃ of vacuum drying chamber inner dryings that filter residue is washed till pH with deionized water, gets nanometer CuS grafting modification bamboo powder.After testing, this nanometer CuS grafting modification bamboo powder is to Cu
2+, Cd
2+, Mn
2+, Zn
2+, Ni
2+And Pb
2+Adsorption rate be respectively 97.7%, 98.0%, 97.3%, 97.2%, 95.9% and 98.1%.
Claims (2)
1. preparation method who is used for the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions is characterized in that this may further comprise the steps:
A. synthesis of nano CuS colloid: the thioacetamide water-alcohol solution slowly is added drop-wise in the equal-volume copper sulphate water-alcohol solution, stir, both mol ratios are 3:1 or 1:3, drip and finish back continuation stirring, be transferred to after reacting completely in the micro-wave digestion reactor, micro-wave digestion, reaction obtains nanometer CuS colloid after finishing, and the taking-up lucifuge is standby;
B. bamboo powder preliminary treatment: at first the bamboo powder is cleaned the back drying through running water and deionized water, cross 80 mesh sieves, then the bamboo powder is immersed in 0.1～0.5mol/L sodium hydroxide solution, magnetic agitation is suction filtration after 12～24 hours, it is that neutral back is dry that filter residue is washed till pH with deionized water, gets preliminary treatment bamboo powder;
C. prepare nanometer CuS grafting modification bamboo powder: it is 2.5～10% TGA aqueous solution that preliminary treatment bamboo powder is placed weight percent concentration, add 2～5mL acetate and 0.2～0.5mL concentrated sulfuric acid, behind stirring at room 10～20h, add nanometer CuS colloid 25～50mL, mix the back and slowly stir 15～30min, filter, it is that neutral back is dry that filter residue is washed till pH with deionized water, gets nanometer CuS grafting modification bamboo powder;
D. detect absorption property: at ambient temperature, getting 0.05g nanometer CuS grafting modification bamboo powder, to join 25mL concentration respectively be 50mg/L Cu
2+, 50mg/L Cd
2+, 50mg/L Mn
2+, 50mg/L Zn
2+, 50mg/L Ni
2+With 100mg/L Pb
2+In the solution, the pH value 5.5～6.5 of regulator solution is filtered behind the ultrasonic concussion 15min, with the heavy metal solution concentration before and after the atomic absorption spectroscopy determination absorption, calculates adsorption rate η (%) according to following formula:
In the formula: C
0Be the initial concentration of metal ion, mg/L; C
eThe concentration of metal ion during for adsorption equilibrium, mg/L.
2. a kind of preparation method who is used for the nanometer CuS grafting modification bamboo powder of Adsorption of Heavy Metal Ions according to claim 1, it is characterized in that described thioacetamide water-alcohol solution of step a and copper sulphate water-alcohol solution, is that thioacetamide and copper sulphate are joined deionized water and ethanol respectively than for formulated in the water-alcohol solution of 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101363830A CN103212376A (en) | 2013-04-18 | 2013-04-18 | Preparation method of nanometer CuS grafting modified bamboo powder capable of adsorbing heavy metal ions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101363830A CN103212376A (en) | 2013-04-18 | 2013-04-18 | Preparation method of nanometer CuS grafting modified bamboo powder capable of adsorbing heavy metal ions |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103212376A true CN103212376A (en) | 2013-07-24 |
Family
ID=48810728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101363830A Pending CN103212376A (en) | 2013-04-18 | 2013-04-18 | Preparation method of nanometer CuS grafting modified bamboo powder capable of adsorbing heavy metal ions |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103212376A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105003059A (en) * | 2015-07-06 | 2015-10-28 | 安徽以诺木塑板材科技有限公司 | Wood-plastic floor produced by crop straws and production method of wood-plastic floor |
| CN108654562A (en) * | 2018-05-08 | 2018-10-16 | 陕西科技大学 | A kind of heavy metal adsorption activated carbon and preparation method thereof of CuS nanoparticles modification |
| CN112934177A (en) * | 2021-02-03 | 2021-06-11 | 广东工业大学 | Manganese sulfide-phosphoric acid modified biochar composite material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070119300A1 (en) * | 2005-11-30 | 2007-05-31 | Yang Xiaolin D | Methods of manufacturing bentonite pollution control sorbents |
| CN102389778A (en) * | 2011-09-19 | 2012-03-28 | 济南大学 | Preparation method and use of sulfydryl flax |
-
2013
- 2013-04-18 CN CN2013101363830A patent/CN103212376A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070119300A1 (en) * | 2005-11-30 | 2007-05-31 | Yang Xiaolin D | Methods of manufacturing bentonite pollution control sorbents |
| CN102389778A (en) * | 2011-09-19 | 2012-03-28 | 济南大学 | Preparation method and use of sulfydryl flax |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105003059A (en) * | 2015-07-06 | 2015-10-28 | 安徽以诺木塑板材科技有限公司 | Wood-plastic floor produced by crop straws and production method of wood-plastic floor |
| CN108654562A (en) * | 2018-05-08 | 2018-10-16 | 陕西科技大学 | A kind of heavy metal adsorption activated carbon and preparation method thereof of CuS nanoparticles modification |
| CN112934177A (en) * | 2021-02-03 | 2021-06-11 | 广东工业大学 | Manganese sulfide-phosphoric acid modified biochar composite material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104226259B (en) | A kind of threonine modified attapulgite earth adsorbing and application thereof | |
| CN105056882A (en) | Preparation method of modified charcoal-based adsorbent for removing hydrogen sulfide | |
| CN102107980B (en) | Method for removing sulfonic-group-containing dye in alkaline waste water by using magnetic chitosan adsorbent | |
| CN109999752B (en) | Preparation method and application of multifunctional material for efficiently adsorbing and degrading organic pollutants | |
| CN110508243B (en) | Preparation method and application of biomass-based porous carbon loaded iron floc adsorption material | |
| CN103894156B (en) | A kind of method utilizing orange peel to make adsorbent for heavy metal | |
| CN104587956A (en) | Preparation method of coated nano zero-valent iron taking multilayer activated-carbon-coated graphene oxide composite powder as carrier | |
| CN102949979A (en) | Process for modifying diatomite | |
| CN103752280A (en) | Composite modified walnut shell adsorbent as well as preparation method and application of composite modified walnut shell absorbent | |
| CN106311158B (en) | A kind of preparation method of maleic acid modified magnetic loofah adsorbent | |
| CN113842883A (en) | Lanthanum-loaded iron carbon nanotube film material for environmental remediation and preparation method and application thereof | |
| CN103212376A (en) | Preparation method of nanometer CuS grafting modified bamboo powder capable of adsorbing heavy metal ions | |
| CN103435737A (en) | Method for preparing adsorption resin through using (methyl)acrylic acid production wastewater as raw material | |
| CN104941573A (en) | Manganite-loaded adsorbent and preparation method thereof as well as application of manganite-loaded adsorbent in treating chemical nickel plating waste liquid | |
| CN113042004B (en) | Preparation method and application of modified carbon-based material | |
| CN104587973A (en) | Uranium extracting adsorption material taking cotton cloth as carrier and preparation method thereof | |
| CN109759024A (en) | A kind of preparation method of the light sorbent based on plant cellulose | |
| CN103521183B (en) | A kind of adsorbent processing acrylic nitrile waste water and preparation method thereof and application | |
| CN108355674A (en) | A kind of zinc sulphide composite photo-catalyst and preparation method for sewage disposal | |
| CN110064378B (en) | Magnetic chitosan carbon sphere with high adsorption performance and preparation method and application thereof | |
| CN104190375A (en) | Biomass absorbing agent for treating rose-bengal dyeing wastewater as well as preparation method and application of biomass absorbing agent | |
| US11638906B2 (en) | Phosphorus nitride adsorbent with high-efficiency selectivity and its applications in removing uranium pollution and extracting uranium from seawater | |
| CN102872794A (en) | Composite adsorption material for removing bromate from water and preparation method for adsorption material | |
| CN105295059A (en) | Immobilized cationized beta-cyclodextrin chloromethylated polystyrene polymer and method for adsorbing and recovering phenols in industrial wastewater | |
| CN111871367B (en) | Rush magnetic powder for dyeing wastewater treatment and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130724 |