CN106902777B - A kind of magnetism dissaving polymer or derivatives thereof blood adsorbent for heavy metal and its preparation method and application - Google Patents
A kind of magnetism dissaving polymer or derivatives thereof blood adsorbent for heavy metal and its preparation method and application Download PDFInfo
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- CN106902777B CN106902777B CN201710269729.2A CN201710269729A CN106902777B CN 106902777 B CN106902777 B CN 106902777B CN 201710269729 A CN201710269729 A CN 201710269729A CN 106902777 B CN106902777 B CN 106902777B
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Abstract
The present invention provides a kind of magnetic dissaving polymer or derivatives thereof blood adsorbent for heavy metal and preparation method thereof, this method comprises: 1) obtain magnetic ferroferric oxide-poly-dopamine in magnetic ferroferric oxide nano-particles surface modification poly-dopamine layer;2) by magnetic ferroferric oxide-poly-dopamine and crosslinking agent, in a solvent then hybrid reaction, adjusting pH value of solution to 7.5-9 are added dissaving polymer, are stirred to react, and magnetism dissaving polymer or derivatives thereof adsorbent for heavy metal is made.Trace heavy metal ion in the adsorbent energy efficient capture blood, and biocompatibility is high, can be realized the selective absorption to heavy metal ion, avoids the influence to the non-specific adsorption and adsorbent itself of elements other in blood to blood constituent;Preparation method simple process of the present invention, synthesis condition is mild, with short production cycle, is suitable for industrialization production, has broad application prospects in medical domain.
Description
Technical field
The present invention relates to a kind of biomedical materials and its preparation method and application, and in particular to a kind of magnetism hyperbranched poly
Close object or derivatives thereof adsorbent for heavy metal and its preparation method and application.
Background technique
With industrialized fast-developing and mankind's destructive activity aggravation, the pollutant containing heavy metal ion is more next
It is diffused into big gas and water, soil (food chain) more, and thus enters human body and deposits.In addition, there is also a huge sum of moneys for drug therapy
Belong to the risk being enriched in gas ions, such as platinum in chemotherapy, the bismuth agent that often contains in stomach medicine.Research shows that: heavy metal can make
The structure of protein changes, to influence histocyte normal function.After internal heavy metal deposition is more than a certain amount of, by
With very high toxicity, non-biodegradable, bioconcentration and the characteristics such as body metabolism cannot be participated in it, one can be generated
The toxicity reaction of series causes physiological disorders so as to cause various diseases, such as kidney failure, liver function damage, neurological disorders, swells
Tumor etc. causes irreversible health hazard to human body.
It is all at present by washing the treatment of blood method, i.e. dimercaptosuccinic acid (DMSA) to the clinical solution of heavy metal poisoning
Injection, ethylenediamine tetra-acetic acid (EDTA) drop, suppository method and oral porphyrazyme (porphyrin enzyme), are all based on and heavy metal
The chelating effect of ion and the removal for realizing heavy metal ion.It is existing to wash blood method there is apparent side reaction big (diarrhea, evil
The heart, liver and kidney dysfunction etc.), treatment time too long disadvantage.Therefore, exploitation the efficient blood excess heavy metal of new type of safe from
Sub- absorption-remover has very important life medical value.
It includes: that 1, ion concentration is low that the challenge of heavy metal ion is adsorbed in blood: content of beary metal is far below dirt in blood
Heavy metal ion content in water, according to People's Republic of China's Occupational sanitary standard, " occupational chronic lead poisoning is diagnosed
Standard " in data analysis, blood lead content is more than the starting point that 0.6ppm is diagnosis lead poisoning, and plumbum ion concentration in common sewage
For 10-100ppm;2, competitive Adsorption: since heavy metal ion is distributed in two ways in blood: i. is mainly and hemoglobin
It is complexed with albumin etc.;Ii. part exists in the form of free state, and there is also dynamic is flat between both existence forms
Weighing apparatus, external adsorbent should can faster sequestration free state heavy metal ion, and need and protein competition absorption complex state a huge sum of money
Belong to the ability of ion;3, blood compatibility requirement: adsorbent for heavy metal must have excellent blood compatibility in blood, right
The ingredients such as red blood cell, blood platelet do not have destruction;4, selective absorption: only selective absorption heavy metal ion, in blood
Normal metal ion (such as sodium, potassium plasma) is without suction-operated.Above-mentioned challenge is so that the heavy metal ion being usually used in water body is inhaled
Attached dose not can be used directly in blood.For in blood environment capture the exceeded heavy metal ion of trace adsorbent must have with
Lower feature: (1) strong low concentration adsorbing metal ions ability, (2) excellent blood compatibility;(3) without (low) cytotoxicity.
Obviously, it is good and the adsorbent of heavy metal ion can need newly in efficient capture blood to prepare blood compatibility
Theory and new technology.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of magnetic dissaving polymer or derivatives thereof heavy metal ion to inhale
Attached dose and its preparation method and application, it is based on heavy metal adsorption principle and blood compatibility technology, is provided a kind of with good blood
Liquid phase capacitive, low cytotoxicity, heavy metal ion selection high adsorption and magnetic dissaving polymer or derivatives thereof a huge sum of money
Belong to the preparation method of ion adsorbent, magnetism dissaving polymer made from this method or derivatives thereof adsorbent for heavy metal
The efficient capture to heavy metal ion is realized by using the high dissaving polymer of functional group densities, and uses magnetic technique
Realize being separated from each other for adsorbent and blood, the method preparation process is simple, and absorption property is good, has in medical domain wide
Application prospect.
Technical solution: the present invention provides a kind of system of magnetic dissaving polymer or derivatives thereof adsorbent for heavy metal
Preparation Method, the preparation method the following steps are included:
1) in magnetic ferroferric oxide nano-particles surface modification poly-dopamine layer, it is poly- more to obtain magnetic ferroferric oxide-
Bar amine;
2) magnetic ferroferric oxide-poly-dopamine made from step 1) is mixed in a solvent with crosslinking agent, at 4-50 DEG C
It is stirred to react 6-24h, pH value of solution is adjusted after reaction to 7.5-9, dissaving polymer is then added, is stirred at 4-50 DEG C anti-
6-24h is answered, the magnetic dissaving polymer or derivatives thereof adsorbent for heavy metal is made;The crosslinking agent is glutaraldehyde
Or glutaryl chlorine.
In step 1), magnetic ferroferric oxide surface is modified using dopamine, on magnetic ferroferric oxide surface
It forms poly-dopamine cross-linked layer strength and is attached to matrix surface, magnetic ferroferric oxide hydrophily is enhanced;Due to poly- DOPA
Organo-functional group (such as amino) rich in, the ferroso-ferric oxide being modified by dopamine surface can be further by functions in amine layer
Change.
Dopamine is easily oxidized in aqueous solution, is then caused from poly- cross-linking reaction, usually that substrate to be modified is direct
It is put into the aqueous dopamine solution of fresh configuration and impregnates certain time, the amine-modified ferroso-ferric oxide of DOPA can be obtained.Step
1) in, magnetic ferroferric oxide nano-particles surface modification poly-dopamine layer method be arranged are as follows: by concentration be 1-50mg
ml-1Magnetic ferroferric oxide-chloroformic solution and concentration be 10-100mgml-1Dopamine Tris-HCl buffer solution it is mixed
It closes, makes the mass ratio 0.1-1 of ferriferrous oxide nano-particle and dopamine in mixed solution, the reaction mixture that will be obtained
In 50-80 DEG C of reaction 5-36h, solid is isolated after reaction, by the solid isolated washing, vacuum drying, obtains magnetism
Ferroso-ferric oxide-poly-dopamine;The partial size of magnetic ferroferric oxide nano-particles is 5-50nm.
In step 2), dissaving polymer is ultrabranching polyamide, hyper-branched polyester, ultrabranching polyamide end group modification obtain
To the obtained derivative of derivative or hyper-branched polyester end group modification;The ultrabranching polyamide is two generations hyperbranched polyamides
Amine, three generations's ultrabranching polyamide or four generation ultrabranching polyamides;The hyper-branched polyester is two generation hyper-branched polyesters, three generations's over-expense
Change polyester or four generation hyper-branched polyesters.
In step 2), magnetic ferroferric oxide-poly-dopamine of addition and the mass ratio of crosslinking agent are 10-1;Hyperbranched poly
Closing concentration of the object in reactant mixed solution is 1-10mgml-1;The mass ratio of dissaving polymer and crosslinking agent is 0.01-
2。
Another aspect of the present invention provides a kind of magnetic dissaving polymer or derivatives thereof adsorbent for heavy metal, this is heavy
Metal ion adsorbent is made by above-mentioned preparation method.The adsorbent for heavy metal has biocompatibility, and in blood
Heavy metal ion has adsorptive selectivity.
Another aspect of the invention provides above-mentioned magnetic dissaving polymer or derivatives thereof adsorbent for heavy metal and is inhaling
Application in attached blood in heavy metal ion, for adsorb in blood include Pb2+, Hg2+, Cd2+, Mn2+, Cr3+Heavy metal
Ion.
The utility model has the advantages that the present invention is using dopamine combination hydrophobicity ferroso-ferric oxide and then aldimine condensation mechanism is used to prepare
A kind of novel, multi-functional magnetic dissaving polymer or derivatives thereof adsorbent for heavy metal, this method are directed to mesh
Preceding blood concentration of heavy metal ion is low, blood environment is complicated requires high, adsorbent scarcity status to adsorbent, provides one kind
Can trace heavy metal ion and the high adsorbent of biocompatibility in efficient capture blood, which, which uses, has sp act
The dissaving polymer of group is absorption main component, can be realized selective absorption of the adsorbent to heavy metal ion, avoids
To the non-specific adsorption of elements other in blood, influence of the adsorbent to blood constituent itself is avoided.System of the invention
Preparation Method simple process, synthesis condition is mild, with short production cycle, is suitable for industrialization production, there is wide application in medical domain
Prospect.
Detailed description of the invention
Fig. 1 is magnetic dissaving polymer or derivatives thereof preparation flow figure;
Fig. 2 is the saturating of magnetic ferroferric oxide nano-particles and two generation magnetism ultrabranching polyamide adsorbent for heavy metal
Penetrate electron microscope;
Fig. 3 is the FT-IR map of two generation magnetism ultrabranching polyamide adsorbent for heavy metal.
Specific embodiment
Embodiment 1
(1) preparation of magnetic ferroferric oxide nano-particles
Weigh six water of 3.4g and iron chloride and tetra- water of 1.5g and frerrous chloride, be dissolved in 33.6ml water, obtain iron chloride and
The mixed aqueous solution of frerrous chloride.To being continually fed into N in the mixed aqueous solution of iron chloride and frerrous chloride2, after being warming up to 25 DEG C,
13.8ml ammonium hydroxide (ammonium hydroxide 26%) is rapidly joined, is vigorously stirred, 1.5g oil is added dropwise in the reaction was continued after being warming up to 80 DEG C 1h dropwise
Acid continues in 80 DEG C of reaction 1h.After cooled to room temperature, magnetic separation pours out water, with ethyl alcohol, acetone supersound washing, magnetic
Solid product is collected in power separation, and 70 DEG C are dried in vacuo 3 hours, obtains magnetic ferroferric oxide nano-particles.Gained four oxygen of magnetism
The transmission electron microscope picture for changing three Fe nanometer particles is as shown in Figure 2 A, by Fig. 2A it is found that magnetic ferroferric oxide nano-particles partial size is
3-10nm。
(2) ferroso-ferric oxide-dopamine nanoparticle is prepared
Magnetic ferroferric oxide nano-particles prepared by step (1) are dispersed in chloroform, 10mgml is prepared-1Four oxygen
Change three-iron-chloroformic solution, takes the 5ml 10mgml-1Ferroso-ferric oxide-chloroformic solution and 10ml 50mgml-1DOPA
Amine Tris-HCl buffer solution is mixed, and reacts 12h, and reaction temperature is 60 DEG C, obtains ferroso-ferric oxide-dopamine nanoparticle
Son.
(3) dissaving polymer is modified
Ferroso-ferric oxide-dopamine nanoparticle prepared by step (2) is dispersed in water, 10mgml is prepared-1Four
Fe 3 O-the dispersion liquid of dopamine nanoparticle in water, takes the 5ml 10mgml-1Ferroso-ferric oxide-dopamine nanometer
The glutaraldehyde water solution room temperature that the dispersion liquid of particle in water and 5ml mass fraction are 6% mixes, and is stirred to react 12h, reaction temperature
Degree is 25 DEG C.PH value of solution is adjusted after reaction to 7.5, and the two generation ultrabranching polyamides of 20mg are then added, continue 25 DEG C instead
After answering 12h, two generation magnetism ultrabranching polyamide adsorbent for heavy metal are obtained.Fig. 2 B is two generation magnetism ultrabranching polyamide weights
The transmission electron microscope picture of metal ion adsorbent.The two generation magnetism ultrabranching polyamide metal ion adsorbent it can be seen from Fig. 2 B
Particle size be about 20nm.Fig. 2 is the FT-IR map of two generation magnetism ultrabranching polyamide adsorbent for heavy metal.By this
Figure can be seen that sample in 2900 and 3200cm-1There is absorption peak in left and right, can be attributed to-CH2And-NH2Absorption peak, thus demonstrate,prove
Bright dissaving polymer is successfully connected.
(4) by two generation magnetism ultrabranching polyamide adsorbent for heavy metal made from step (3) to heavy metal in waste water
The absorption behavior of ion is studied:
10ppm, the lead ion solution of 2ppm, 1ppm, with feed ratio (i.e. every 3mL lead ion of 15mg/3mL are prepared respectively
Bis- generation of 15mg magnetism ultrabranching polyamide adsorbent for heavy metal is added in solution) absorption 1h, measure the composite material counterweight
The adsorbance of metal ion.The results show that two generation magnetism ultrabranching polyamide adsorbent for heavy metal are to 10ppm, 2ppm,
The heavy metal ion adsorbed removal rate of 1ppm is respectively 89%, 95%, 99%.Result explanation, the composite material can be used for height
Effect removal heavy metal ions in wastewater.
(5) by two generation magnetism ultrabranching polyamide adsorbent for heavy metal made from step (3) to heavy metal in blood
The absorption behavior of ion is studied:
Preparing plumbum ion concentration is respectively 1ppm, and the new fresh rabbit blood of 2ppm is hyperbranched by two generation magnetism made from embodiment 1
Polyamide adsorbent for heavy metal is added with the feed ratio of 15mg/3mL and (bis- generation of 15mg is added in i.e. every 3mL lead ion solution
Magnetic ultrabranching polyamide adsorbent for heavy metal), 37 DEG C of concussion 1h, Magnetic Isolation adsorbent collects supernatant, to blood
Resolution processing is carried out, residual plumbum ion concentration is detected using ICP-MS (inductivity coupled plasma mass spectrometry), acquired results are shown
For the adsorbent to 1ppm, the removal of heavy metal ions rate in the blood of 2ppm is respectively 89%, 83%.Result explanation, this is multiple
Condensation material can be used for efficiently removing heavy metal ions in wastewater.
Embodiment 2
(1) ferroso-ferric oxide-dopamine nanoparticle is prepared
10mgml is prepared with magnetic ferroferric oxide nano-particles prepared by 1 step of embodiment (1)-1Magnetism four aoxidize
Three-iron-chloroformic solution takes the 5ml 10mgml-1Ferroso-ferric oxide-chloroformic solution and 20ml25mgml-1Dopamine
Tris-HCl buffer solution is mixed, and reacts 6h, and reaction temperature is 80 DEG C, obtains ferroso-ferric oxide-dopamine nanoparticle.
(2) dissaving polymer is modified
Ferroso-ferric oxide-dopamine nanoparticle prepared by step (2) is dispersed in water, 10mgml is prepared-1Four
Fe 3 O-the dispersion liquid of dopamine nanoparticle in water takes the 5ml 10mg ml-1Ferroso-ferric oxide-dopamine nanometer
The glutaraldehyde water solution room temperature that the dispersion liquid of particle in water and 5ml mass fraction are 6% mixes, and is stirred to react 12h, reaction temperature
Degree is 4 DEG C.PH value of solution is adjusted after reaction to 9, and three generations's ultrabranching polyamide of 20mg is then added, continues 4 DEG C of reaction 12h
Afterwards, obtain three generations's magnetism ultrabranching polyamide adsorbent for heavy metal, the adsorbent can efficiently remove in blood heavy metal from
Son (such as Pb2+, Hg2+, Cd2+, Mn2+, Cr3+)。
Embodiment 3
(1) ferroso-ferric oxide-dopamine nanoparticle is prepared
10mgml is prepared with magnetic ferroferric oxide nano-particles prepared by 1 step of embodiment (1)-1Four oxidation three
Iron-chloroformic solution takes the 5ml 10mgml-1Ferroso-ferric oxide-chloroformic solution and 1ml 50mgml-1Dopamine
Tris-HCl buffer solution is mixed, and reacts 6h, and reaction temperature is 60 DEG C, obtains ferroso-ferric oxide-dopamine nanoparticle.
(2) dissaving polymer is modified
Ferroso-ferric oxide-dopamine nanoparticle prepared by step (2) is dispersed in water, 10mgml is prepared-1Four
Fe 3 O-the dispersion liquid of dopamine nanoparticle in water takes the 5ml 10mg ml-1Ferroso-ferric oxide-dopamine nanometer
The glutaraldehyde water solution room temperature that the dispersion liquid of particle in water and 5ml mass fraction are 6% mixes, and is stirred to react 12h, reaction temperature
Degree is 50 DEG C.PH value of solution is adjusted after reaction to 8, and the four generation ultrabranching polyamides of 20mg are then added, continue 50 DEG C of reactions
After 12h, four generation magnetism ultrabranching polyamide adsorbent for heavy metal are obtained, which can efficiently remove heavy metal in blood
Ion (such as Pb2+, Hg2+, Cd2+, Mn2+, Cr3+)。
Embodiment 4
(1) ferroso-ferric oxide-dopamine nanoparticle is prepared
The magnetic ferroferric oxide nano-particles that particle diameter distribution is 10-30nm are prepared into 50mgml-1Ferroso-ferric oxide-
Chloroformic solution takes the 2ml 50mgml-1Ferroso-ferric oxide-chloroformic solution and 1ml 100mgml-1Dopamine Tris-
HCl buffer solution is mixed, and reacts 36h, and reaction temperature is 50 DEG C, obtains ferroso-ferric oxide-dopamine nanoparticle.
(2) dissaving polymer is modified
Ferroso-ferric oxide-dopamine nanoparticle prepared by step (2) is dispersed in water, 10mgml is prepared-1Four
Fe 3 O-the dispersion liquid of dopamine nanoparticle in water takes the 5ml 10mg ml-1Ferroso-ferric oxide-dopamine nanometer
The glutaraldehyde water solution room temperature that the dispersion liquid of particle in water and 5ml mass fraction are 1% mixes, and is stirred to react for 24 hours, reaction temperature
Degree is 4 DEG C.PH value of solution is adjusted after reaction to 9, and three generations's ultrabranching polyamide of 100mg is then added, continues 4 DEG C of reactions
After for 24 hours, three generations's magnetism ultrabranching polyamide adsorbent for heavy metal is obtained, which can efficiently remove heavy metal in blood
Ion (such as Pb2+, Hg2+, Cd2+, Mn2+, Cr3+)。
Embodiment 5
(1) ferroso-ferric oxide-dopamine nanoparticle is prepared
The magnetic ferroferric oxide nano-particles that particle diameter distribution is 30-50nm are prepared into 1mgml-1Ferroso-ferric oxide-
Chloroformic solution takes the 30ml 1mgml-1Ferroso-ferric oxide-chloroformic solution and 1ml 100mgml-1Dopamine Tris-
HCl buffer solution is mixed, and reacts 5h, and reaction temperature is 75 DEG C, obtains ferroso-ferric oxide-dopamine nanoparticle.
(2) dissaving polymer is modified
Ferroso-ferric oxide-dopamine nanoparticle prepared by step (2) is dispersed in water, 10mgml is prepared-1Four
Fe 3 O-the dispersion liquid of dopamine nanoparticle in water takes the 5ml 10mg ml-1Ferroso-ferric oxide-dopamine nanometer
The glutaryl chlorine water solution room temperature that the dispersion liquid of particle in water and 5ml mass fraction are 20% mixes, and is stirred to react 6h, reacts
Temperature is 50 DEG C.PH value of solution is adjusted after reaction to 9, and the four generation ultrabranching polyamides of 10mg are then added, continue 50 DEG C instead
After answering 6h, four generation magnetism ultrabranching polyamide adsorbent for heavy metal are obtained, which can efficiently remove a huge sum of money in blood
Category ion (such as Pb2+, Hg2+, Cd2+, Mn2+, Cr3+)。
Claims (8)
1. a kind of magnetism dissaving polymer or derivatives thereof adsorbent for heavy metal is in absorption blood in heavy metal ion
Application, which is characterized in that the preparation method of the adsorbent for heavy metal includes the following steps:
1) in magnetic ferroferric oxide nano-particles surface modification poly-dopamine layer, magnetic ferroferric oxide-poly-dopamine is obtained;
2) magnetic ferroferric oxide-poly-dopamine is mixed in a solvent with crosslinking agent, it is stirred to react 6 at 4~50 DEG C~
For 24 hours, pH value of solution is adjusted after reaction to 7.5~9, and dissaving polymer is then added, it is stirred to react 6 at 4~50 DEG C~
For 24 hours, the magnetic dissaving polymer or derivatives thereof adsorbent for heavy metal is made;The crosslinking agent is glutaraldehyde or penta
Diacid chloride.
2. application according to claim 1, which is characterized in that in the step 1), the magnetic ferroferric oxide nanometer
The partial size of particle is 5~50nm.
3. application according to claim 1, which is characterized in that described to be received in magnetic ferroferric oxide in the step 1)
The method of rice corpuscles surface modification poly-dopamine layer are as follows: by concentration be 1~50mgml-1Magnetic ferroferric oxide-chloroform it is molten
Liquid and concentration are 10~100mgml-1Dopamine Tris-HCl buffer solution mixing, so that ferroso-ferric oxide in mixed solution is received
The mass ratio of rice corpuscles and dopamine is 0.1~1, by obtained reaction mixture in 50~80 DEG C of 5~36h of reaction, reaction
After isolate solid, by the solid isolated washing, vacuum drying, obtain the magnetic ferroferric oxide-poly-dopamine.
4. application according to claim 1, which is characterized in that in the step 2), the dissaving polymer is over-expense
The derivative or hyper-branched polyester end group modification that change polyamide, hyper-branched polyester, ultrabranching polyamide end group modification obtain obtain
Derivative, the ultrabranching polyamide be two generation ultrabranching polyamides, three generations's ultrabranching polyamide or four generations hyperbranched polyamides
Amine, the hyper-branched polyester are two generation hyper-branched polyesters, three generations's hyper-branched polyester or four generation hyper-branched polyesters.
5. application according to claim 1, which is characterized in that in the step 2), magnetic four oxidation three of addition
The mass ratio of iron-poly-dopamine and the crosslinking agent is 1~20.
6. application according to claim 1, which is characterized in that in the step 2), the concentration of the dissaving polymer
For 1~10mgml-1。
7. application according to claim 1, which is characterized in that in the step 2), the dissaving polymer with it is described
The mass ratio of crosslinking agent is 0.01~2.
8. application according to claim 1, which is characterized in that heavy metal ion includes Pb in the blood2+, Hg2+, Cd2 +, Mn2+, Cr3+。
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CN108906003A (en) * | 2018-08-02 | 2018-11-30 | 南通大学 | A kind of preparation method of the polypropylene-base adsorbent material based on poly-dopamine modified lithium |
CN109172908B (en) * | 2018-08-27 | 2020-10-16 | 南京师范大学 | Blood lead removing instrument for removing blood lead in vitro |
CN109331794B (en) * | 2018-10-15 | 2020-05-22 | 西安交通大学 | Dopamine and metabolite molecular imprinting magnetic nanosphere thereof, and preparation method and application thereof |
CN110251479B (en) * | 2019-06-06 | 2021-10-19 | 南京师范大学 | Erythrocyte membrane-wrapped bionic blood hexavalent chromium reduction remover/magnetic nano motor and preparation method and application thereof |
CN111312904B (en) * | 2020-03-09 | 2023-04-07 | 苏州大学 | High-performance environment-friendly lead-based perovskite solar cell and preparation method thereof |
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