CN108854991A - A kind of poly-dopamine cladding polyethylene sieve plate and its application - Google Patents
A kind of poly-dopamine cladding polyethylene sieve plate and its application Download PDFInfo
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- CN108854991A CN108854991A CN201810345633.4A CN201810345633A CN108854991A CN 108854991 A CN108854991 A CN 108854991A CN 201810345633 A CN201810345633 A CN 201810345633A CN 108854991 A CN108854991 A CN 108854991A
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- 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
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The present invention provides a kind of poly-dopamine cladding polyethylene sieve plate, and the poly-dopamine cladding polyethylene sieve plate is synthesized by dopamine auto polymerization reaction modifying hydrophobic polyethylene sieve plate.The present invention also provides a kind of preparation methods of poly-dopamine cladding polyethylene sieve plate, include the following steps：It is cleaned using organic solvent and soaks polyethylene sieve plate；Polyethylene sieve plate and Dopamine hydrochloride are added in the tris solution of alkalinity, after reacting a period of time, catalyst are added to get to stable poly-dopamine and coats polyethylene sieve plate.Poly-dopamine cladding polyethylene sieve plate provided by the invention can be used to evaluate the biological effectiveness of organic pollutant in environment in conjunction with hydroxypropyl-β-cyclodextrin solution.Poly-dopamine cladding polyethylene sieve plate synthesis technology provided by the invention is simple, high-efficient, obvious to organic pollutant bioavailability assessment effect, environmental-friendly, cheap.
Description
Technical field
The present invention relates to Environmental Chemistry technical field more particularly to a kind of poly-dopamine cladding polyethylene sieve plate and its answer
With.
Background technique
The measurement of organic contaminants in soil biological effectiveness is of great significance for environmental risk assessment.It is right both at home and abroad
In the evaluation method of organic pollutant biological effectiveness mainly include biology and chemical method two major classes.Biological method refer to by
Organism is directly exposed in pollution environment, and the content that pollutant is enriched in organism is directly measured after being enriched with balance.Biology
Method can directly react the biological effectiveness of pollutant in soil, but this method is longer there are the test period, test species
Between difference and experiment condition the problems such as being affected.Common chemical method include mild solvent extraction, cyclodextrin extract,
Tenax resin extraction etc..Chemical method has the advantages that easy to operate, strong operability, quickly easy.But reported
In method, mild solvent extraction compared with vulnerable to type of solvent, solid water than the operating conditions such as, extraction time limitation；Cyclodextrin
The biological effectiveness of organic contaminants in soil can be underestimated by extracting capacity limit；The extraction of Tenax resin is presently the most common and comments
Valence method, but it is expensive, is not readily separated and the operation cycle is long.In conclusion in environment organic pollutant biologically effective
Property prediction technique exploitation be still faced with many challenges, formed, researched and developed novel there has been no generally acknowledged mature method
Fiber material and method are of great significance.
Summary of the invention
In view of this, the present invention provides the poly-dopamines that one kind is capable of effectively save cost to coat polyethylene sieve plate, also
Provide a kind of application of the poly-dopamine cladding polyethylene sieve plate in evaluation environment in the biological effectiveness of organic pollutant.
The present invention provides a kind of poly-dopamine cladding polyethylene sieve plate, and the poly-dopamine cladding polyethylene sieve plate passes through more
The synthesis of bar amine auto polymerization reaction modifying hydrophobic polyethylene sieve plate.
The present invention also provides a kind of preparation methods of above-mentioned poly-dopamine cladding polyethylene sieve plate, include the following steps：
S101 is cleaned using organic solvent and is soaked polyethylene sieve plate；
Polyethylene sieve plate and Dopamine hydrochloride are added in the tris solution of alkalinity, constant temperature by S102
After shaking table oscillation, Dopamine hydrochloride is added, after persistent oscillation, catalyst is added, polyethylene sieve plate is taken out in oscillation after a certain period of time,
Dopamine auto polymerization synthesizes poly-dopamine in polyethylene floor lever of sieve tray；
S103 cleans polyethylene sieve plate using deionized water and organic solvent, dries in a vacuum drying oven poly- to get arriving
Dopamine coats polyethylene sieve plate.
Further, in step S101 and S103, the organic solvent is acetone.
Further, in step S102, the temperature of constant-temperature table is 25 DEG C, and the catalyst of revolving speed 200rpm, addition are
Copper sulphate/hydrogen peroxide catalyst, the concentration of the Dopamine hydrochloride of addition is 0.5~2mg/mL, after Dopamine hydrochloride is added every time,
Duration of oscillation is 6~18h, and duration of oscillation is 3~12h after catalyst is added.
Further, in step S102, the molar concentration of the tris solution is 10mmol/L, pH value
It is 8.5.
The present invention also provides a kind of application of above-mentioned poly-dopamine cladding polyethylene sieve plate, the poly-dopamine coats poly- second
Alkene sieve plate can be used to evaluate the biological effectiveness of organic pollutant in environment in conjunction with hydroxypropyl-β-cyclodextrin solution.
Further, being evaluated in environment using poly-dopamine cladding polyethylene sieve plate and hydroxypropyl-β-cyclodextrin solution is had
The process of the biological effectiveness of machine pollutant is：
Poly-dopamine cladding polyethylene sieve plate and hydroxypropyl-β-cyclodextrin solution are added in soil, to soil by S201
Middle addition deionized water is then placed within constant-temperature table and vibrates 4~48h；
S202 takes out poly-dopamine and coats polyethylene sieve plate, after cleaning sieve plate using deionized water, using acetone or just oneself
Alkane solution carries out desorption to sieve plate and is concentrated to get concentrate；
S203, using the organic pollutant in gas-chromatography Tandem Mass Spectrometry Analysis concentrate.
Further, in step S201, the temperature of constant-temperature table is 25 DEG C, revolving speed 60rpm, the hydroxy propyl-Beta-ring
The concentration and volume of dextrin solution are determined according to realistic objective analyte and soil content, when the life of measurement PAHs in soil
When object validity, the concentration of hydroxypropyl-β-cyclodextrin solution is 75g/L, and volume is 10~30mL.
Further, the dosage of the poly-dopamine cladding polyethylene sieve plate is 1~4.
Technical solution bring beneficial effect provided by the invention is：
1, poly-dopamine provided by the invention cladding polyethylene sieve plate synthesis technology it is simple, it is high-efficient, to organic pollutant
Effect of extracting it is obvious, it is environmental-friendly, it is cheap；
2, the preparation method of poly-dopamine cladding polyethylene sieve plate provided by the invention is simple and efficient to handle, mild condition,
Material is cheap and easily-available, it is easy to accomplish industrialized production；
3, poly-dopamine cladding polyethylene sieve plate combination hydroxypropyl-β-cyclodextrin solution provided by the invention can be applied to
Biological effectiveness measurement, wherein poly-dopamine cladding polyethylene sieve plate is as reception source, and hydroxypropyl-β-cyclodextrin solution is as biography
Defeated medium, not only easy to operate, save the cost and time, but also overcome time and effort consuming in previous methods, be not readily separated and give birth to
The shortcomings that object active principle is underestimated；
4, poly-dopamine cladding polyethylene sieve plate combination hydroxypropyl-β-cyclodextrin solution provided by the invention is suitable for a variety of
Measurement, such as polycyclic aromatic hydrocarbon, Polychlorinated biphenyls of organic contaminants in soil validity of type etc., in different organic pollutants and
Have wide practical use in varying environment medium.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the preparation method of poly-dopamine cladding polyethylene sieve plate of the present invention.
Fig. 2 is a kind of reaction process schematic diagram of the preparation method of poly-dopamine cladding polyethylene sieve plate of the present invention.
Fig. 3 is biological effectiveness of the present invention using organic pollutant in poly-dopamine cladding polyethylene sieve plate evaluation environment
Process schematic.
Fig. 4 is the scanning electron microscope (SEM) photograph of polyethylene sieve plate and poly-dopamine cladding polyethylene sieve plate of the invention.
Fig. 5 is polycyclic aromatic hydrocarbon in polyethylene sieve plate and poly-dopamine cladding polyethylene sieve plate absorption HPCD solution of the invention
Comparison diagram.
Fig. 6 is the relational graph of poly-dopamine cladding polyethylene sieve plate combination HPCD solution and Tenax extraction of the present invention.
Fig. 7 is the result figure of the embodiment of the present invention and comparative example measurement PAHs in soil.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is further described.
Fig. 1 and Fig. 2 are please referred to, the embodiment provides a kind of poly-dopamines to coat polyethylene sieve plate (PDA@
PESP), synthesized by dopamine auto polymerization reaction modifying hydrophobic polyethylene sieve plate.
The embodiments of the present invention also provide a kind of preparation methods of above-mentioned poly-dopamine cladding polyethylene sieve plate, including with
Lower step：
Step S101 is cleaned using organic solvent and is soaked polyethylene sieve plate；Generally preferable organic solvent be acetone, third
Ketone is cheap and toxicity is smaller, and the size of polyethylene sieve plate can select according to the actual situation.
Polyethylene sieve plate and concentration are that the Dopamine hydrochloride of 0.5~2mg/mL is added to three hydroxyls of alkalinity by step S102
In aminomethane solution, the molar concentration of tris solution is preferably 10mmol/L, perseverance under certain temperature
After warm shaking table sufficiently vibrates 6~18h, Dopamine hydrochloride is added, after 6~18h of persistent oscillation, catalyst is added, vibrates 3~12h
Polyethylene sieve plate is taken out afterwards, and dopamine auto polymerization synthesizes poly-dopamine in polyethylene floor lever of sieve tray；Dopamine hydrochloride is in batches multiple
Being added can make the coating of package more uniform, and the catalyst of addition keeps the structure of polymer more stable.
Specifically, in step S102, the temperature of shaking table is preferably 25 DEG C, and the revolving speed of shaking table is set as 200rpm, addition
Catalyst is copper sulphate/hydrogen peroxide catalyst.
Step S103 cleans polyethylene sieve plate using deionized water and acetone repeatedly, until solution is clarified, then in vacuum
It is dried in drying box to get poly-dopamine cladding polyethylene sieve plate smooth to surface, in disc-shaped, color for black.
With reference to Fig. 3, poly-dopamine cladding polyethylene sieve plate and hydroxypropyl-β-cyclodextrin solution (HPCD) provided by the invention
In conjunction with the biological effectiveness that can effectively evaluate organic pollutant in environment, evaluation procedure is：
Step S201, be prepared 1~4 poly-dopamine cladding polyethylene sieve plate and hydroxypropyl-β-cyclodextrin is molten
Liquid is added in soil, and deionized water is added into soil, is then placed within the constant temperature that temperature is 25 DEG C, revolving speed is 60rpm and is shaken
4~48h is vibrated in bed；Poly-dopamine coats the dosage of polyethylene sieve plate according to the decision of the content of practical soil, hydroxy propyl-Beta-ring
The concentration and volume of dextrin solution are determined according to realistic objective analyte and soil content, when the life of measurement PAHs in soil
When object validity, the concentration of hydroxypropyl-β-cyclodextrin solution is 75g/L, and volume is 10~30mL.
Step S202 takes out poly-dopamine and coats polyethylene sieve plate after oscillation, after cleaning sieve plate using deionized water,
Desorption is carried out to sieve plate using acetone or hexane solution and is concentrated to get concentrate, such as 0.5mL can be concentrated into using nitrogen,
Then 1 μ L sample is taken.
Step S203, using the organic pollutant in gas-chromatography tandem mass spectrum (GC-MS/MS) analysis concentrate.
Below with reference to embodiment and comparative example to the preparation method of poly-dopamine provided by the invention cladding polyethylene sieve plate
It is described in detail with application.
(1) addition 20mL pH after 20 polyethylene sieve plates (diameter 9.1mm, with a thickness of 1.6mm) are cleaned with acetone is chosen
Value is the tris solution that 8.5, molar concentration is 10mmol/L, then 30mg Dopamine hydrochloride is then added
(DA), it after constant-temperature table (temperature is 25 DEG C, revolving speed 200rpm) oscillation 12h, adds 15mg DA and adds after persistent oscillation 6h
It is taken out after entering catalyst (20mg copper sulphate and 50 μ l hydrogen peroxide) subsequent persistent oscillation 3h.
(2) after removing reaction solution, the poly-dopamine cladding polyethylene sieve plate of synthesis is cleaned straight for several times with deionized water
It clarifies to solution, is dried in (60 DEG C) of vacuum oven.
Fig. 4 is the scanning electron microscope (SEM) photograph that polyethylene sieve plate of the invention and poly-dopamine coat polyethylene sieve plate, and Fig. 4 (a) is
The scanning electron microscope (SEM) photograph of polyethylene floor lever of sieve tray, Fig. 4 (b) are the scanning electron microscope (SEM) photograph that poly-dopamine coats polyethylene floor lever of sieve tray, Fig. 4
It (c) is the scanning electron microscope (SEM) photograph of polyethylene sieve plate section, Fig. 4 (d) is the scanning electron microscope that poly-dopamine coats polyethylene sieve plate section
Figure, poly-dopamine has successfully been coated in the surface and inside of polyethylene sieve plate as can be seen from Figure 4.
Fig. 5 is polycyclic aromatic hydrocarbon in polyethylene sieve plate and poly-dopamine cladding polyethylene sieve plate absorption HPCD solution of the invention
Comparison diagram, Fig. 5 (a) be polyethylene sieve plate absorption result figure, Fig. 5 (b) be poly-dopamine coat polyethylene sieve plate absorption
Result figure, as can be seen from Figure 5 poly-dopamine modification after polyethylene sieve plate due to hydrophily it is stronger, show stronger absorption
Ability and better reproducibility.
Fig. 6 is the relational graph that poly-dopamine of the present invention coats polyethylene sieve plate combination HPCD solution and Tenax extraction, from figure
6 it can be seen that method provided by the invention has good correlation with Tenax extracting process.
Embodiment 1：
The hydroxyl for being 75g/L by the poly-dopamine cladding polyethylene sieve plate and 20mL concentration of two panels above-mentioned (1)-(2) synthesis
Propyl-beta-cyclodextrin solution is added in the practical soil of 1g selection, and the total content of organic carbon of soil is 0.797% (referred to as
LTS), mixture is taken out poly- after constant-temperature table (temperature is 25 DEG C, revolving speed 60rpm) oscillation 12h using antimagnetic type tweezer
Dopamine coats polyethylene sieve plate, after clear water cleaning, after acetone soln desorption concentration, with gas-chromatography tandem mass spectrum (GC-
MS/MS it) analyzes.
Comparative example 1：
Comparative example 1 and the difference of embodiment 1 are only that：Hydroxypropyl-β-cyclodextrin solution is added without in soil；Remaining condition
It is substantially the same manner as Example 1.
Embodiment 2：
Embodiment 2 and the difference of embodiment 1 are only that the total content of organic carbon in soil is 22.014% (referred to as HTS)；
Remaining condition is substantially the same manner as Example 1.
Comparative example 2：
Comparative example 2 and the difference of embodiment 2 are only that：Hydroxypropyl-β-cyclodextrin solution is added without in soil；Remaining condition
It is substantially the same manner as Example 2.
Fig. 7 is the result figure of the embodiment of the present invention and comparative example measurement PAHs in soil, and Fig. 7 (a) is 2 He of embodiment
Comparative example 2 measures the comparing result figure of PAHs in soil, and Fig. 7 (b) is polycyclic in embodiment 1 and the measurement soil of comparative example 1
The comparing result figure of aromatic hydrocarbons, it can be seen that the polyethylene sieve plate and the compound extraction of HPCD of poly-dopamine modification from the comparison diagram of Fig. 7
It takes and significantly improves the extraction total amount of polycyclic aromatic hydrocarbon；And the number of rings of polycyclic aromatic hydrocarbon is higher, soil organic carbon more high effect more
Obviously.
Poly-dopamine cladding polyethylene sieve plate provided by the invention passes through simple dopamine original position auto polymerization reaction modifying
The hydrophobic polyethylene sieve plate of commercialization synthesizes, while catalyst is added in reasonable time and makes synthesized material more steady
Fixed, synthesis process is quicker.
Poly-dopamine cladding polyethylene sieve plate synthesis technology provided by the invention is simple, high-efficient, to organic pollutant
Effect of extracting is obvious, environmental-friendly, cheap；The preparation method behaviour of poly-dopamine cladding polyethylene sieve plate provided by the invention
Make simple and efficient, mild condition, material is cheap and easily-available, it is easy to accomplish industrialized production；Poly-dopamine cladding provided by the invention
Polyethylene sieve plate combination hydroxypropyl-β-cyclodextrin solution can be applied to biological effectiveness measurement, and wherein poly-dopamine cladding is poly-
Ethylene sieve plate as reception source, hydroxypropyl-β-cyclodextrin solution as transmission medium, not only easy to operate, save the cost and when
Between, and overcome time and effort consuming in previous methods, be not readily separated and the shortcomings that biologically effective component is underestimated；The present invention provides
Poly-dopamine coat the organic contamination suitable for a plurality of types of soil of polyethylene sieve plate combination hydroxypropyl-β-cyclodextrin solution
Measurement of object validity, such as polycyclic aromatic hydrocarbon, Polychlorinated biphenyls etc. have extensively in different organic pollutants and varying environment medium
Application prospect.
In the absence of conflict, the feature in embodiment and embodiment herein-above set forth can be combined with each other.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of poly-dopamine coats polyethylene sieve plate, which is characterized in that the poly-dopamine cladding polyethylene sieve plate passes through more
The synthesis of bar amine auto polymerization reaction modifying hydrophobic polyethylene sieve plate.
2. a kind of preparation method of poly-dopamine cladding polyethylene sieve plate described in claim 1, which is characterized in that including following
Step：
S101 is cleaned using organic solvent and is soaked polyethylene sieve plate；
Polyethylene sieve plate and Dopamine hydrochloride are added in the tris solution of alkalinity, constant-temperature table by S102
After oscillation, Dopamine hydrochloride is added, after persistent oscillation, catalyst is added, polyethylene sieve plate, DOPA are taken out in oscillation after a certain period of time
Amine auto polymerization synthesizes poly-dopamine in polyethylene floor lever of sieve tray；
S103 cleans polyethylene sieve plate using deionized water and organic solvent, is dried in a vacuum drying oven to get poly- DOPA is arrived
Amine coats polyethylene sieve plate.
3. the preparation method of poly-dopamine as claimed in claim 2 cladding polyethylene sieve plate, which is characterized in that step S101 and
In S103, the organic solvent is acetone.
4. the preparation method of poly-dopamine cladding polyethylene sieve plate as claimed in claim 2, which is characterized in that step S102
In, the temperature of constant-temperature table is 25 DEG C, revolving speed 200rpm, and the catalyst of addition is copper sulphate/hydrogen peroxide catalyst, addition
The concentration of Dopamine hydrochloride is 0.5~2mg/mL, and after Dopamine hydrochloride is added every time, duration of oscillation is 6~18h, and catalysis is added
Duration of oscillation is 3~12h after agent.
5. the preparation method of poly-dopamine cladding polyethylene sieve plate as claimed in claim 2, which is characterized in that step S102
In, the molar concentration of the tris solution is 10mmol/L, pH value 8.5.
6. a kind of application of poly-dopamine cladding polyethylene sieve plate described in any one of claim 1 to 5, which is characterized in that institute
Stating poly-dopamine cladding polyethylene sieve plate can be used to evaluate organic pollutant in environment in conjunction with hydroxypropyl-β-cyclodextrin solution
Biological effectiveness.
7. the application of poly-dopamine cladding polyethylene sieve plate as claimed in claim 6, which is characterized in that utilize poly-dopamine packet
It covers polyethylene sieve plate and the process of the biological effectiveness of organic pollutant in hydroxypropyl-β-cyclodextrin solution evaluation environment is：
Poly-dopamine cladding polyethylene sieve plate and hydroxypropyl-β-cyclodextrin solution are added in soil, add into soil by S201
Enter deionized water, is then placed within constant-temperature table and vibrates 4~48h；
S202 takes out poly-dopamine and coats polyethylene sieve plate, molten using acetone or n-hexane after cleaning sieve plate using deionized water
Liquid carries out desorption to sieve plate and is concentrated to get concentrate；
S203, using the organic pollutant in gas-chromatography Tandem Mass Spectrometry Analysis concentrate.
8. the application of poly-dopamine cladding polyethylene sieve plate as claimed in claim 7, which is characterized in that permanent in step S201
The temperature of warm shaking table is 25 DEG C, and revolving speed 60rpm, the concentration and volume of the hydroxypropyl-β-cyclodextrin solution are according to practical mesh
It marks analyte and soil content determines, when measuring the biological effectiveness of PAHs in soil, hydroxypropyl-β-cyclodextrin solution
Concentration be 75g/L, volume be 10~30mL.
9. the application of poly-dopamine cladding polyethylene sieve plate as claimed in claim 7, which is characterized in that the poly-dopamine packet
The dosage for covering polyethylene sieve plate is 1~4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112892486A (en) * | 2021-01-19 | 2021-06-04 | 西南科技大学 | Preparation method of inorganic heavy metal waste liquid adsorption material, adsorption material and application |
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