CN105536730B - A kind of composite nano adsorbent and its preparation method and application - Google Patents
A kind of composite nano adsorbent and its preparation method and application Download PDFInfo
- Publication number
- CN105536730B CN105536730B CN201510918587.9A CN201510918587A CN105536730B CN 105536730 B CN105536730 B CN 105536730B CN 201510918587 A CN201510918587 A CN 201510918587A CN 105536730 B CN105536730 B CN 105536730B
- Authority
- CN
- China
- Prior art keywords
- sediment
- pva
- composite nano
- dissolved
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—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
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
-
- 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
- B01J20/22—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
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
-
- 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
-
- 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
-
- 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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/322—Volatile compounds, e.g. benzene
Abstract
A kind of composite nano adsorbent and its preparation method and application, belong to environment functional material technical field.Using P (HB HO), CS, pore-foaming agent, PVA as raw material；It is dissolved according to P (HB HO) in organic phase；CS is put into acetum and dissolved, pore-foaming agent mixing is added, high-speed homogenization, forms colostric fluid；Part PVA is taken, is dissolved into the PVA aqueous solution, then is mixed with colostric fluid, high-speed homogenization, forms double emulsion, being sufficiently stirred makes organic phase volatilize, double emulsion high speed centrifugation, abandons supernatant, collects sediment；Remaining PVA is dissolved into the PVA aqueous solution, the sediment of collection is scattered in shaken overnight in the PVA aqueous solution, washes away the remaining pore-foaming agent in sediment, high speed centrifugation collects sediment, the sediment of collection is freeze-dried, obtains P (HB HO)/CS composite nano adsorbents.The present invention has nano adsorber particle diameter distribution uniform, good dispersion degree, has loose structure, stability is good, non-secondary pollution, can remove heavy metal and hydrophobic organic compound in sewage simultaneously, improve treatment effeciency.
Description
Technical field
The invention belongs to environment functional material technical field, and in particular to a kind of composite nano adsorbent and preparation method thereof
And application.
Background technology
Water is one of for the survival of mankind three big vital principles.China's freshwater resources total amount is 28000 billion cubic meters, is accounted for
The 6% of global water resources.But water resources ownership per capita only has 2300m3, only the 1/4 of world average level, be the whole world per capita
One of poorest country of water resource.With industrialization rapid development and level of urbanization continuous improvement, water resource pollution is increasingly
Seriously, majority is the combined pollution combined by multiple pollutant.The a large amount of synthesis and discharge of hardly degraded organic substance, containing a huge sum of money
Belong to the presence of ion trade effluent so that the combined pollution of Heavy Metals in Waters-organic matter becomes a kind of commonplace show
As, such as the sludge of sewage treatment plant, city domestic refuse percolation liquid, runoff containing agricultural chemicals and coking, oil refining, plating and printing and dyeing
Pollution caused by the sewage such as industry, it is mostly heavy metal-organic matter combined pollution.The different journeys of the main rivers and lakes in China
Degree is polluted by heavy metal and organic matter.These pollutant toxicity are big, distribution is wide, difficult degradation, easily savings, to ecological environment
Destruction and harm to human health be potential and huge.At present, available for heavy metal in water-organic compound contaminated
Treatment process includes enhanced coagulation method, photochemical catalysis method, bioanalysis, embrane method and absorption method etc..Wherein, absorption method is because to a huge sum of money
Category and gas chromatography adsorption efficiency height, removal ability are strong, and sorbing material repeats the advantages that utilizing, increasingly by people's
Pay attention to.Research shows, is to solve water ring using the pollutant in sorbing material (such as activated carbon, resin, silica gel etc.) absorption effluent
A kind of processing method of high-efficient simple of border pollution.
Chitosan (CS) is chitin deacetylation product, is a kind of positively charged natural polymer, has
It is the advantages that good biological degradability, biocompatibility, non-secondary pollution, extensive in fields such as medicine, chemical industry, food, environment
Using.Substantial amounts of free amine group and hydroxyl in CS molecules be present, under certain pH can by hydrogen bond, coordinate bond or covalent bond with again
Complexation reaction occurs for metal ion etc., turns into a kind of adsorbent of function admirable in sewage disposal.Hydroxybutyric acid and Hydroxyoctanoic acid
EVA [P (HB-HO)] is a kind of new polyhydroxyl alkanoic acid (PHAs), be produced by the fermented mode of microorganism it is hydrophobic
Property macromolecule polyester.The material has good physics characteristic (such as thermoplasticity, piezoelectricity, optical activity, mechanics mechanical performance
Deng) and excellent biological characteristics (such as biodegradability, biocompatibility, catabolite nontoxicity and surface modificability
Deng), it has also become one of important candidate material of current ecological environment material nd and bio-medical material.Existing poly butyric
(PHB) document report as the single organic matter of sorbent treatment water body (chlorobenzene or o-chloronitrobenzene), but the ratio of the adsorbent
Smaller (the 58.78m of surface area2·g-1), reach the time required to adsorption equilibrium longer (36h), limited sorption capacity.
The content of the invention
The purpose of the present invention is the deficiency for limited sorption capacity existing for above-mentioned existing adsorbent, there is provided a kind of compound
Nano adsorber and its preparation method and application.
To achieve the above object, the technical solution adopted in the present invention is：A kind of composite nano adsorbent, wherein：Below
The matrix of row parts by weight is raw material：
3~30 parts of P (HB-HO), CS1~15 part, 5~30 parts of pore-foaming agent, PVA11~25 part；
Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is
Polyvinyl alcohol.
A kind of method for preparing described composite nano adsorbent, wherein：Comprise the following steps：
(1) P (HB-HO) of above-mentioned parts by weight is dissolved in organic phase, and described P (HB-HO) is dense in organic phase
Spend for 1~10%；
(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, added above-mentioned heavy
After the pore-foaming agent mixing for measuring number, 5~10min of high-speed homogenization under 10000~15000rpm rotating speed, colostric fluid is formed；
(3) 1~15 part of PVA is first taken, is dissolved into the PVA aqueous solution that concentration is 0.1~1.5%, then be made with step (2)
Colostric fluid mixed after, 5~10min of high-speed homogenization under 10000~15000rpm rotating speed, formed double emulsion；
(4) double emulsion made from step (3) is sufficiently stirred 5~8h, organic phase is volatilized completely, double emulsion is existed
High speed centrifugation 10min under 15000rpm rotating speed, supernatant is abandoned, collect sediment；
(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in
In the PVA aqueous solution, shaken overnight, wash away the remaining pore-foaming agent in sediment, then under 15000rpm rotating speed at a high speed from
After heart 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C, obtained
To P (HB-HO)/CS composite nano adsorbents.
Further preferred scheme, described organic phase are chloroform or dichloromethane.
Described pore-foaming agent is any one in sodium chloride, sodium acid carbonate or hydrogen peroxide.
Composite nano adsorbent of the present invention is applied in absorption effluent simultaneously in heavy metal and hydrophobic organic compound.
Compared with prior art, there is advantages below：First, the present invention is using CS and P (HB-HO) as main carriers, and two
Kind material is easy to get, and cost is relatively low, degradable.Second, the present invention is prepared for P (HB-HO)/CS is compound using emulsion homogenate method and received
Rice adsorbent, the nano adsorber particle diameter distribution is homogeneous, good dispersion degree, has loose structure, and stability is preferable, without secondary dirt
Dye.3rd, with heavy metal ion complexation reaction, P (HB- can occur for the free amine group of CS molecules, hydroxyl in adsorbent of the present invention
HO) there is extremely strong hydrophobicity, confirmed through adsorption test, by good adsorbent performance and the P (HB-HO) of CS heavy metals to hydrophobic
The property distinctive affinity of organic matter is combined, and can be removed the heavy metal and hydrophobic organic compound in sewage simultaneously, be substantially increased
To the treatment effeciency of combined pollution in sewage.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of P (HB-HO)/CS composite nano adsorbents.
Fig. 2 is the grain size distribution of P (HB-HO)/CS composite nano adsorbents.
Embodiment
Embodiment 1：
A kind of composite nano adsorbent of the present embodiment, wherein：Using the matrix of following parts by weight as raw material：
3 parts of P (HB-HO), CS1 parts, 30 parts of sodium chloride, PVA11 parts；
Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is
Polyvinyl alcohol.
A kind of method for preparing described composite nano adsorbent, wherein：Comprise the following steps：
(1) P (HB-HO) of above-mentioned parts by weight is dissolved in dichloromethane, and described P (HB-HO) is in dichloromethane
Middle concentration is 1%；
(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, added above-mentioned heavy
After the sodium chloride mixing for measuring number, the high-speed homogenization 5min under 15000rpm rotating speed, colostric fluid is formed；
(3) first take 1 part of PVA, be dissolved into concentration be 0.1% the PVA aqueous solution, then with step (2) made from colostric fluid
After being mixed, the high-speed homogenization 5min under 15000rpm rotating speed, double emulsion is formed；
(4) double emulsion made from step (3) is sufficiently stirred 5h, dichloromethane is volatilized completely, double emulsion is existed
High speed centrifugation 10min under 15000rpm rotating speed, supernatant is abandoned, collect sediment；
(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in
In the PVA aqueous solution, shaken overnight, wash away the remaining sodium chloride in sediment, then under 15000rpm rotating speed at a high speed from
After heart 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C, obtained
To P (HB-HO)/CS composite nano adsorbents.
With grain size distribution as depicted in figs. 1 and 2, this receives the scanning electron microscope (SEM) photograph of P (HB-HO)/CS composite nano adsorbents
Rice adsorbent is spheroidal, and surface has loose structure, and particle diameter distribution is in 250-350nm or so.
P (the HB-HO)/CS composite nano adsorbents prepared with embodiment 1 are to toluene, Cr6+Compound sewage is carried out at absorption
Reason.Weigh 0.5gP (HB-HO)/CS composite nano adsorbents be placed in 200mL, initial concentration be 50mg/L toluene and Cr6+'s
In mixed solution, the water bath with thermostatic control vibration 24h under conditions of 30 DEG C and 150rpm, centrifuge and determine toluene in solution respectively
(high performance liquid chromatography) and Cr6+The concentration of (atomic absorption spectrophotometry).P (HB-HO)/CS composite nano adsorbents are to first
Benzene and Cr6+Adsorption rate be respectively 96.36%, 98.97%.
As control, by 0.5gCS, (CS and P (HB-HO) ratio of weight and number is 1 with P (HB-HO) intermingling material:3) make
For adsorbent, using method same as described above to toluene, Cr6+Compound sewage carries out adsorption treatment.Intermingling material adsorbent pair
Toluene and Cr6+Adsorption rate be respectively 20.28%, 30.74%.
As a result show：Prepared P (HB-HO)/CS composite nano adsorbents are to toluene, Cr6+Compound sewage adsorption effect
Significantly.
Embodiment 2：
A kind of composite nano adsorbent of the present embodiment, wherein：Using the matrix of following parts by weight as raw material：
25 parts of P (HB-HO), CS15 parts, 6 parts of sodium acid carbonate, PVA15 parts；
Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is
Polyvinyl alcohol.
A kind of method for preparing described composite nano adsorbent, wherein：Comprise the following steps：
(1) P (HB-HO) of above-mentioned parts by weight is dissolved in dichloromethane, and described P (HB-HO) is in dichloromethane
Middle concentration is 8.3%；
(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, added above-mentioned heavy
After the sodium acid carbonate mixing for measuring number, the high-speed homogenization 6min under 13000rpm rotating speed, colostric fluid is formed；
(3) first take 5 parts of PVA, be dissolved into concentration be 0.5% the PVA aqueous solution, then with step (2) made from colostric fluid
After being mixed, the high-speed homogenization 6min under 13000rpm rotating speed, double emulsion is formed；
(4) double emulsion made from step (3) is sufficiently stirred 6h, dichloromethane is volatilized completely, double emulsion is existed
High speed centrifugation 10min under 15000rpm rotating speed, supernatant is abandoned, collect sediment；
(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in
In the PVA aqueous solution, shaken overnight, the remaining sodium acid carbonate in sediment is washed away, then under 15000rpm rotating speed at a high speed
After centrifuging 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C,
Obtain P (HB-HO)/CS composite nano adsorbents.
P (the HB-HO)/CS composite nano adsorbents prepared with embodiment 2 are to naphthalene, Pb2+Compound sewage carries out adsorption treatment.
Weigh 0.5gP (HB-HO)/CS composite nano adsorbents be placed in 200mL, initial concentration be 50mg/L naphthalene and Pb2+Mixing
In solution, the water bath with thermostatic control vibration 24h under conditions of 30 DEG C and 150rpm, is centrifuged and naphthalene is (efficient in measure solution respectively
Liquid chromatography) and Pb2+The concentration of (atomic absorption spectrophotometry).P (HB-HO)/CS composite nano adsorbents are to naphthalene and Pb2 +Adsorption rate be respectively 95.76%, 97.13%.
As control, by CS, (CS and P (HB-HO) ratio of weight and number is 3 with P (HB-HO) intermingling material:5) as suction
Attached dose, using method same as described above to naphthalene, Pb2+Compound sewage carries out adsorption treatment.Intermingling material adsorbent is to naphthalene and Pb2 +Adsorption rate be respectively 21.39%, 27.32%.
As a result show：Prepared P (HB-HO)/CS composite nano adsorbents are to naphthalene, Pb2+Compound sewage adsorption effect shows
Write.
Embodiment 3：
A kind of composite nano adsorbent of the present embodiment, wherein：Using the matrix of following parts by weight as raw material：
12 parts of P (HB-HO), CS1 parts, 10 parts of hydrogen peroxide, PVA25 parts；
Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is
Polyvinyl alcohol.
A kind of method for preparing described composite nano adsorbent, wherein：Comprise the following steps：
(1) P (HB-HO) of above-mentioned parts by weight is dissolved in chloroform, and described P (HB-HO) is in chloroform
Middle concentration is 4%；
(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, added above-mentioned heavy
After the hydrogen peroxide mixing for measuring number, the high-speed homogenization 8min under 12000rpm rotating speed, colostric fluid is formed；
(3) first take 15 parts of PVA, be dissolved into concentration be 1.5% the PVA aqueous solution, then with step (2) made from colostric fluid
After being mixed, the high-speed homogenization 8min under 12000rpm rotating speed, double emulsion is formed；
(4) double emulsion made from step (3) is sufficiently stirred 7h, chloroform is volatilized completely, double emulsion is existed
High speed centrifugation 10min under 15000rpm rotating speed, supernatant is abandoned, collect sediment；
(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in
In the PVA aqueous solution, shaken overnight, the residual hydrogen peroxide in sediment is washed away, then under 15000rpm rotating speed at a high speed
After centrifuging 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C,
Obtain P (HB-HO)/CS composite nano adsorbents.
P (the HB-HO)/CS composite nano adsorbents prepared with embodiment 3 are to o-dichlorohenzene, Zn2+Compound sewage is inhaled
Attached processing.Weigh 0.5gP (HB-HO)/CS composite nano adsorbents be placed in 200mL, initial concentration be 50mg/L adjacent dichloro
Benzene and Zn2+Mixed solution in, water bath with thermostatic control vibration 24h, centrifuges and simultaneously determines respectively under conditions of 30 DEG C and 150rpm
O-dichlorohenzene (high performance liquid chromatography) and Zn in solution2+The concentration of (atomic absorption spectrophotometry).P (HB-HO)/CS is compound
Nano adsorber is to o-dichlorohenzene and Zn2+Adsorption rate be respectively 96.10%, 98.69%.
As control, by CS, (CS and P (HB-HO) ratio of weight and number is 1 with P (HB-HO) intermingling material:12) as suction
Attached dose, using method same as described above to o-dichlorohenzene, Zn2+Compound sewage carries out adsorption treatment.Intermingling material adsorbent pair
O-dichlorohenzene and Zn2+Adsorption rate be respectively 19.91%, 28.38%.
As a result show：Prepared P (HB-HO)/CS composite nano adsorbents are to o-dichlorohenzene, Zn2+Compound sewage adsorbs
Significant effect.
Embodiment 4：
A kind of composite nano adsorbent of the present embodiment, wherein：Using the matrix of following parts by weight as raw material：
24 parts of P (HB-HO), CS8 parts, 20 parts of sodium acid carbonate, PVA20 parts；
Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is
Polyvinyl alcohol.
A kind of method for preparing described composite nano adsorbent, wherein：Comprise the following steps：
(1) P (HB-HO) of above-mentioned parts by weight is dissolved in chloroform, and described P (HB-HO) is in chloroform
Middle concentration is 8%；
(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, added above-mentioned heavy
After the sodium acid carbonate mixing for measuring number, the high-speed homogenization 10min under 10000rpm rotating speed, colostric fluid is formed；
(3) first take 10 parts of PVA, be dissolved into concentration be 1% the PVA aqueous solution, then with step (2) made from colostric fluid enter
After row mixing, the high-speed homogenization 10min under 10000rpm rotating speed, double emulsion is formed；
(4) double emulsion made from step (3) is sufficiently stirred 8h, chloroform is volatilized completely, double emulsion is existed
High speed centrifugation 10min under 15000rpm rotating speed, supernatant is abandoned, collect sediment；
(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in
In the PVA aqueous solution, shaken overnight, the remaining sodium acid carbonate in sediment is washed away, then under 15000rpm rotating speed at a high speed
After centrifuging 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C,
Obtain P (HB-HO)/CS composite nano adsorbents.
With P (HB-HO)/CS composite nano adsorbents prepared by embodiment 4 to luxuriant and rich with fragrance, Cd2+Compound sewage carries out adsorption treatment.
Weigh 0.5gP (HB-HO)/CS composite nano adsorbents be placed in 200mL, initial concentration be 50mg/L phenanthrene and Cd2+Mixing
In solution, the water bath with thermostatic control vibration 24h under conditions of 30 DEG C and 150rpm, centrifuge and determine solution China and Philippines respectively (efficiently
Liquid chromatography) and Cd2+The concentration of (atomic absorption spectrophotometry).P (HB-HO)/CS composite nano adsorbents are to luxuriant and rich with fragrance and Cd2 +Adsorption rate be respectively 97.71%, 97.99%.
As control, by CS, (CS and P (HB-HO) ratio of weight and number is 1 with P (HB-HO) intermingling material:3) as suction
Attached dose, using method same as described above to luxuriant and rich with fragrance, Cd2+Compound sewage carries out adsorption treatment.Intermingling material adsorbent is to luxuriant and rich with fragrance and Cd2 +Adsorption rate be respectively 20.76%, 29.82%.
As a result show：Prepared P (HB-HO)/CS composite nano adsorbents are to luxuriant and rich with fragrance, Cd2+Compound sewage adsorption effect shows
Write.
Embodiment 5：
A kind of composite nano adsorbent of the present embodiment, wherein：Using the matrix of following parts by weight as raw material：
5 parts of P (HB-HO), CS2 parts, 5 parts of sodium acid carbonate, PVA18 parts；
Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is
Polyvinyl alcohol.
A kind of method for preparing described composite nano adsorbent, wherein：Comprise the following steps：
(1) P (HB-HO) of above-mentioned parts by weight is dissolved in dichloromethane, and described P (HB-HO) is in dichloromethane
Middle concentration is 1.7%；
(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, added above-mentioned heavy
After the sodium acid carbonate mixing for measuring number, the high-speed homogenization 7min under 11000rpm rotating speed, colostric fluid is formed；
(3) first take 5 parts of PVA, be dissolved into concentration be 0.8% the PVA aqueous solution, then with step (2) made from colostric fluid
After being mixed, the high-speed homogenization 7min under 11000rpm rotating speed, double emulsion is formed；
(4) double emulsion made from step (3) is sufficiently stirred 6h, dichloromethane is volatilized completely, double emulsion is existed
High speed centrifugation 10min under 15000rpm rotating speed, supernatant is abandoned, collect sediment；
(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in
In the PVA aqueous solution, shaken overnight, the remaining sodium acid carbonate in sediment is washed away, then under 15000rpm rotating speed at a high speed
After centrifuging 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C,
Obtain P (HB-HO)/CS composite nano adsorbents.
P (the HB-HO)/CS composite nano adsorbents prepared with embodiment 5 are to naphthalene, Pb2+Compound sewage carries out adsorption treatment.
Weigh 0.5gP (HB-HO)/CS composite nano adsorbents be placed in 200mL, initial concentration be 50mg/L naphthalene and Pb2+Mixing
In solution, the water bath with thermostatic control vibration 24h under conditions of 30 DEG C and 150rpm, is centrifuged and naphthalene is (efficient in measure solution respectively
Liquid chromatography) and Pb2+The concentration of (atomic absorption spectrophotometry).P (HB-HO)/CS composite nano adsorbents are to naphthalene and Pb2 +Adsorption rate be respectively 96.11%, 97.89%.
As control, by CS, (CS and P (HB-HO) ratio of weight and number is 2 with P (HB-HO) intermingling material:5) as suction
Attached dose, using method same as described above to naphthalene, Pb2+Compound sewage carries out adsorption treatment.Intermingling material adsorbent is to naphthalene and Pb2 +Adsorption rate be respectively 22.74%, 29.38%.
As a result show：Prepared P (HB-HO)/CS composite nano adsorbents are to naphthalene, Pb2+Compound sewage adsorption effect shows
Write.
Embodiment 6：
A kind of composite nano adsorbent of the present embodiment, wherein：Using the matrix of following parts by weight as raw material：
30 parts of P (HB-HO), CS6 parts, 28 parts of sodium chloride, PVA15 parts；
Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is
Polyvinyl alcohol.
A kind of method for preparing described composite nano adsorbent, wherein：Comprise the following steps：
(1) P (HB-HO) of above-mentioned parts by weight is dissolved in chloroform, and described P (HB-HO) is in chloroform
Middle concentration is 10%；
(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, added above-mentioned heavy
After the sodium chloride mixing for measuring number, the high-speed homogenization 8min under 12000rpm rotating speed, colostric fluid is formed；
(3) first take 1 part of PVA, be dissolved into concentration be 0.5% the PVA aqueous solution, then with step (2) made from colostric fluid
After being mixed, the high-speed homogenization 8min under 12000rpm rotating speed, double emulsion is formed；
(4) double emulsion made from step (3) is sufficiently stirred 5h, chloroform is volatilized completely, double emulsion is existed
High speed centrifugation 10min under 15000rpm rotating speed, supernatant is abandoned, collect sediment；
(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in
In the PVA aqueous solution, shaken overnight, wash away the remaining sodium chloride in sediment, then under 15000rpm rotating speed at a high speed from
After heart 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C, obtained
To P (HB-HO)/CS composite nano adsorbents.
P (the HB-HO)/CS composite nano adsorbents prepared with embodiment 6 are to toluene, Cr6+Compound sewage is carried out at absorption
Reason.Weigh 0.5gP (HB-HO)/CS composite nano adsorbents be placed in 200mL, initial concentration be 50mg/L toluene and Cr6+'s
In mixed solution, the water bath with thermostatic control vibration 24h under conditions of 30 DEG C and 150rpm, centrifuge and determine toluene in solution respectively
(high performance liquid chromatography) and Cr6+The concentration of (atomic absorption spectrophotometry).P (HB-HO)/CS composite nano adsorbents are to first
Benzene and Cr6+Adsorption rate be respectively 97.38%, 98.76%.
As control, by 0.5gCS, (CS and P (HB-HO) ratio of weight and number is 1 with P (HB-HO) intermingling material:5) make
For adsorbent, using method same as described above to toluene, Cr6+Compound sewage carries out adsorption treatment.Intermingling material adsorbent pair
Toluene and Cr6+Adsorption rate be respectively 21.35%, 30.58%.
As a result show：Prepared P (HB-HO)/CS composite nano adsorbents are to toluene, Cr6+Compound sewage adsorption effect
Significantly.
Claims (5)
- A kind of 1. composite nano adsorbent, it is characterised in that：Using the matrix of following parts by weight as raw material：3~30 parts of P (HB-HO), CS1~15 part, 5~30 parts of pore-foaming agent, PVA11~25 part；Described P (HB-HO) is hydroxybutyric acid and Hydroxyoctanoic acid EVA；Described CS is chitosan；Described PVA is poly- second Enol；Described pore-foaming agent is any one in sodium chloride, sodium acid carbonate or hydrogen peroxide；Wherein specific preparation method comprises the following steps：(1) P (HB-HO) of above-mentioned parts by weight is dissolved in organic phase, and described P (HB-HO) concentration in organic phase is 1 ~10%；(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, add above-mentioned parts by weight After several pore-foaming agent mixing, 5~10min of high-speed homogenization under 10000~15000rpm rotating speed, colostric fluid is formed；(3) first take 1~15 part of PVA, be dissolved into concentration be 0.1~1.5% the PVA aqueous solution, then with step (2) made from just After emulsion is mixed, 5~10min of high-speed homogenization under 10000~15000rpm rotating speed, double emulsion is formed；(4) double emulsion made from step (3) is sufficiently stirred 5~8h, organic phase is volatilized completely, make double emulsion in 15000rpm Rotating speed under high speed centrifugation 10min, abandon supernatant, collect sediment；(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in the PVA In the aqueous solution, shaken overnight, the remaining pore-foaming agent in sediment is washed away, then the high speed centrifugation under 15000rpm rotating speed After 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C, obtains P (HB-HO)/CS composite nano adsorbents.
- A kind of 2. method for preparing the composite nano adsorbent described in claim 1, it is characterised in that：Comprise the following steps：(1) P (HB-HO) of above-mentioned parts by weight is dissolved in organic phase, and described P (HB-HO) concentration in organic phase is 1 ~10%；(2) CS of above-mentioned parts by weight is put into the acetum that concentration is 2% again and dissolved, add above-mentioned parts by weight After several pore-foaming agent mixing, 5~10min of high-speed homogenization under 10000~15000rpm rotating speed, colostric fluid is formed；(3) first take 1~15 part of PVA, be dissolved into concentration be 0.1~1.5% the PVA aqueous solution, then with step (2) made from just After emulsion is mixed, 5~10min of high-speed homogenization under 10000~15000rpm rotating speed, double emulsion is formed；(4) double emulsion made from step (3) is sufficiently stirred 5~8h, organic phase is volatilized completely, make double emulsion in 15000rpm Rotating speed under high speed centrifugation 10min, abandon supernatant, collect sediment；(5) remaining PVA is dissolved into the PVA aqueous solution that concentration is 1%, the sediment that step (4) is collected is scattered in the PVA In the aqueous solution, shaken overnight, the remaining pore-foaming agent in sediment is washed away, then the high speed centrifugation under 15000rpm rotating speed After 10min, sediment is collected, the sediment of collection is freeze-dried 24h with freeze drier at a temperature of -50 DEG C, obtains P (HB-HO)/CS composite nano adsorbents.
- 3. the preparation method of composite nano adsorbent according to claim 2, it is characterised in that：Described organic phase is three Chloromethanes or dichloromethane.
- 4. the preparation method of composite nano adsorbent according to claim 2, it is characterised in that：Described pore-foaming agent is chlorine Change any one in sodium, sodium acid carbonate or hydrogen peroxide.
- 5. the application of composite nano adsorbent according to claim 1, it is characterised in that：Described composite nano adsorbent Applied in heavy metal and hydrophobic organic compound in absorption effluent simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510918587.9A CN105536730B (en) | 2015-12-11 | 2015-12-11 | A kind of composite nano adsorbent and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510918587.9A CN105536730B (en) | 2015-12-11 | 2015-12-11 | A kind of composite nano adsorbent and its preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105536730A CN105536730A (en) | 2016-05-04 |
| CN105536730B true CN105536730B (en) | 2018-01-19 |
Family
ID=55816568
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510918587.9A Active CN105536730B (en) | 2015-12-11 | 2015-12-11 | A kind of composite nano adsorbent and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105536730B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110178863B (en) * | 2019-04-24 | 2022-03-11 | 山东省农业科学院植物保护研究所 | Slow-release pesticide preparation for preventing woolly apple aphid and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648149A (en) * | 2004-12-24 | 2005-08-03 | 山西大学 | Hydroxy alkanoic acid polymer and its producing method |
| CN102284277A (en) * | 2011-07-28 | 2011-12-21 | 中国科学院新疆理化技术研究所 | Mercury ion adsorbent |
| CN103599761A (en) * | 2013-11-08 | 2014-02-26 | 王善良 | Mercury removing adsorbent |
| CN104722251A (en) * | 2015-04-23 | 2015-06-24 | 福建师范大学 | Preparation method of porous chitosan-based microspheres |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017019881A (en) * | 2013-11-25 | 2017-01-26 | 株式会社クラレ | Biopolymer adsorptive composition and water treatment method using the same |
-
2015
- 2015-12-11 CN CN201510918587.9A patent/CN105536730B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648149A (en) * | 2004-12-24 | 2005-08-03 | 山西大学 | Hydroxy alkanoic acid polymer and its producing method |
| CN102284277A (en) * | 2011-07-28 | 2011-12-21 | 中国科学院新疆理化技术研究所 | Mercury ion adsorbent |
| CN103599761A (en) * | 2013-11-08 | 2014-02-26 | 王善良 | Mercury removing adsorbent |
| CN104722251A (en) * | 2015-04-23 | 2015-06-24 | 福建师范大学 | Preparation method of porous chitosan-based microspheres |
Non-Patent Citations (2)
| Title |
|---|
| Enrichment of chlorobenzene and o-nitrochlorobenzene on biomimetic adsorbent prepared by poly-3-hydroxybutyrate(PHB);Xiaoxuan Zhang,et al;《Journal of Hazardous Materials》;20091221;第177卷(第1期);文章摘要 * |
| 静电纺壳聚糖/聚乙烯醇纳米纤维膜对Cu2+、Ni2+及Cd2+的吸附特性;张慧敏等;《环境科学学报》;20150131;第35卷(第1期);文章摘要，第185页2.2节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105536730A (en) | 2016-05-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Adsorption of antibiotics from water by using Chinese herbal medicine residues derived biochar: Preparation and properties studies | |
| Mousavi et al. | Pb (II) removal from synthetic wastewater using Kombucha Scoby and graphene oxide/Fe3O4 | |
| Wen et al. | A novel biosorbent prepared by immobilized Bacillus licheniformis for lead removal from wastewater | |
| Prakasham et al. | Biosorption of chromium VI by free and immobilized Rhizopus arrhizus | |
| Wu et al. | Biosorption of 2, 4-dichlorophenol by immobilized white-rot fungus Phanerochaete chrysosporium from aqueous solutions | |
| Chen et al. | Uranium removal by novel graphene oxide-immobilized Saccharomyces cerevisiae gel beads | |
| Chen et al. | Biosorption of lead, cadmium and mercury by immobilized Microcystis aeruginosa in a column | |
| CN101816923A (en) | Method for preparing metal ion adsorbent | |
| CN103041787B (en) | Preparation method of crosslinked chitosan-manganese dioxide composite adsorbing material | |
| Kamal et al. | Adsorption of Fe ions by modified carrageenan beads with tricarboxy cellulose: kinetics study and four isotherm models | |
| Sun et al. | Adsorption of boron by CA@ KH-550@ EPH@ NMDG (CKEN) with biomass carbonaceous aerogels as substrate | |
| Figueiredo et al. | Natural waste materials containing chitin as adsorbents for textile dyestuffs: Batch and continuous studies | |
| CN101314123A (en) | Magnetic biological adsorption agent and preparation method thereof | |
| CN103933936A (en) | Preparation method and application of antibiotic composite adsorbent | |
| Rostamian et al. | Preparation and neutralization of forcespun chitosan nanofibers from shrimp shell waste and study on its uranium adsorption in aqueous media | |
| CN106824071A (en) | C@SiO of the one kind for Cr (VI) Adsorption2The preparation method of hollow ball | |
| Nguyen et al. | Biochar derived from the spent coffee ground for ammonium adsorption from aqueous solution | |
| Wang et al. | Continuous fixed bed adsorption of Cu (II) by halloysite nanotube–alginate hybrid beads: an experimental and modelling study | |
| CN103910402A (en) | Granular Schwertmannite and its preparation method and use | |
| Tang et al. | Magnetic powdery acrylic polymer with ultrahigh adsorption capacity for atenolol removal: Preparation, characterization, and microscopic adsorption mechanism | |
| CN108514864A (en) | A kind of chitin/graphene oxide composite sponge and the preparation method and application thereof | |
| Aziz et al. | Composite nanofibers of polyacrylonitrile/natural clay for decontamination of water containing Pb (II), Cu (II), Zn (II) and pesticides | |
| CN105536730B (en) | A kind of composite nano adsorbent and its preparation method and application | |
| CN106512933B (en) | A kind of while the adsorbent of adsorbing and removing carbamazepine and sulfamethoxazole preparation method | |
| CN106622160A (en) | Multifunctional water-purifying sand, 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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |