CN109293859A - A kind of hydrophily sulindac molecular engram magnetic Nano resin balls and its preparation method and application - Google Patents
A kind of hydrophily sulindac molecular engram magnetic Nano resin balls and its preparation method and application Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/20—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with polyhydric phenols
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
The invention discloses a kind of hydrophily sulindac molecular engram magnetic Nano resin balls and its preparation method and application, belong to nano material preparation and Environmental Chemistry applied technical field.Hydro-thermal method one-step synthesis carboxyl magnetic nano-balls are used first；Then, carboxyl magnetic nano-balls, sulindac are added in ultrapure water, ammonium hydroxide is then added, obtain template-carrier compound；Add resorcinol, formaldehyde is polymerize, obtain solid polymer；Finally, solid polymer is separated by externally-applied magnetic field, after polymer elution, drying, be made hydrophily sulindac molecular engram magnetic Nano resin balls.Hydrophily sulindac molecular engram magnetic Nano resin balls produced by the present invention, its uniform particle diameter, structural stability are good, magnetic response is strong, reusable property is strong, good hydrophilic property, and, large amount of adsorption, rate of recovery height strong to the selective adsorption capacity of sulindac, lower cost for material simultaneously, preparation are simple.
Description
Technical field
Nano material preparation of the present invention and Environmental Chemistry applied technical field, are related to a kind of hydrophily sulindac molecular engram
Magnetic Nano resin balls and its preparation method and application.
Background technique
Since 21 century, with advances in technology with the transition in epoch, for pollutant in environment analytical technology just
It gradually improves, the environmental consciousness of people is also gradually reinforced, novel environmental pollutant --- drug and personal-care supplies (PPCPs)
Start to get more and more people's extensive concerning.PPCPs's is many kinds of, mainly includes all kinds of antibiotic, synthetic musk, analgesic
Medicine, depressor, contraceptive, somnifacient, slimming drugs, hair jelly, hair dye and fungicide etc..The chemical structure of PPCPs generally compares
Stablize, it is not degradable, and PPCPs present in environment can be constantly enriched in food chain, be transmitted step by step, and human health can be made
It is on the hazard, the ecosystem is destroyed.Anodyne is production and consumption in PPCPs as the common medicine in people's daily life
Biggish one kind is measured, and sulindac frequently appears in the waste water of pharmaceutical factory and hospital, life as the common ingredient in anodyne
In sewage and human urine.If will lead to nausea, headache, hepatic injury or anaphylaxis skin disease containing excessive sulindac in human body
Equal adverse reactions, serious person result even in anaphylactic shock and acute renal failure.
Mainly there are high performance liquid chromatography (HPLC), liquid chromatograph mass spectrography for the detection method of sulindac at present
The methods of method (LC-MS), capillary electrophoresis (CE).These methods are big since there are equipment investments, operating cost is high, sample is pre-
The disadvantages of processing is complicated limits its application in conventional analysis.
Molecular imprinting technology refers to obtain and polymerize on space structure and binding site with what template molecule exactly matched
The experiment technology of preparing of object.Since molecularly imprinted polymer (Molecularly Imprinted Polymers, MIPs) can be with
It is combined by the function monomer with specific functional groups with template molecule, the functional group of monomer institute band itself can basis and template
The needs of interaction of molecules adjust and form specific space conformation.Since molecularly imprinted polymer has high selectivity,
The advantages that unique physical and chemical stability, preparation process is simple and reusable, MIPs exists as solid phase extraction adsorbents
Good application prospect is illustrated in separation technology field.
Before never about the relevant report of sulindac molecularly imprinted polymer, in the detection process of sulindac mostly
It needs using a large amount of organic solvent, these not only can cause environmental pollution, and also cause the sulindac in water to be difficult to accurate
Detection.Therefore, the method for developing simple and effective preparation hydrophily sulindac molecularly imprinted polymer, in realization complex matrices
The efficiently concentrating of sulindac, effectively detection, quickly removal etc. has important research significance.
Magnetic separation technique is the magnetic contrast according to substance, under the driving of magnetic force, magnetic component from
A kind of technology separated in the mixture of its non-magnetic components composition.Since Magnetic Isolation is easy to operate, by this technology
It is combined with molecular imprinting technology, is used for Solid Phase Extraction, must be installed into solid-phase extraction column instead of previous MIPs or consolidated
Using the process of centrifugation or filtering when mutually extracting, reduce the disadvantage that its separation process is time-consuming, complicated and lower efficiency.Fe3O4Magnetic
Property nanoparticle has the characteristics that good biocompatibility, higher magnetic susceptibility and low toxicity.With Fe3O4Magnetic nano particle
The MIPs that son is prepared as carrier only need to can complete adsorbent material and adsorption liquid by an additional magnet in several seconds
Separation.With modified Fe3O4Magnetic nano-particle is removed as the molecularly imprinted polymer that " core " is prepared to be had to object
Specific adsorption performance outside, also have many advantages, such as that large specific surface area, the rate of adsorption be fast and superparamagnetism, can be directly in complicated base
Selective enrichment object in matter, using extraction can be completed after the quick separating of magnetic field.
Currently, about the preparation of sulindac molecularly imprinted polymer and its in sewage, sulindac is directly separated not yet
With the relevant report applied in detection.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of hydrophily sulindac molecule prints
Mark magnetic Nano resin balls and its preparation method and application.
In order to achieve the above object, the present invention is achieved by the following scheme:
The invention discloses a kind of preparation methods of hydrophily sulindac molecular engram magnetic Nano resin balls, comprising: first
First, using hydro-thermal method one-step synthesis carboxyl magnetic nano-balls；Then, carboxyl magnetic nano-balls, sulindac are added to ultrapure water
In, ammonium hydroxide is then added, the compound of template-carrier is made；Resorcinol and first is added into template-carrier compound again
Aldehyde is polymerize, and solid polymer is obtained；Finally, being separated solid polymer by externally-applied magnetic field, consolidate what is isolated
After the elution of state polymer, drying, hydrophily sulindac molecular engram magnetic Nano resin balls are made.
Preferably, the above method specifically includes the following steps:
Step 1: by iron chloride, sodium acetate, Sodium Polyacrylate, ethylene glycol and diglycol according to (0.3~0.8)
G:(1.0~3.5) g:(0.02~0.06) g:(6.6~8.2) mL:(10~14) mL amount ratio, be placed in reaction kettle,
7~16h is reacted at 180~220 DEG C, after reaction, by reaction product washing, vacuum drying, carboxyl magnetic nano-balls is made；
Step 2: by carboxyl magnetic nano-balls, sulindac, ultrapure water and ammonium hydroxide according to being placed in reaction vessel, at room temperature
It is stirred to react 10~50min, resorcinol is added and stirs 0.5~2.5h, be eventually adding formaldehyde, at room temperature polymerization reaction 3
~8h, and solidify 6~12h；
Wherein, the amount ratio of carboxyl magnetic nano-balls, sulindac, ultrapure water, ammonium hydroxide, resorcinol and formaldehyde be (100~
500) mg:(10~50) mg:(5~35) mL:(1.8~6.5) mL:(0.01~2.8) g:(0.01~1.2) mL；
Step 3: the solid polymer generated in step 2 after reaction reaction solution is isolated by externally-applied magnetic field
Come, then the solid polymer isolated is eluted, is dried, hydrophily sulindac molecular engram magnetic Nano resin is made
Ball.
It is further preferred that in step 1, reaction product is washed to neutrality using ultrapure water, then 30~60 DEG C,
Under conditions of 0.05~0.09MPa, it is dried in vacuo 3~8h.
It is further preferred that solidification temperature is 18~60 DEG C in step 2.
It is further preferred that the eluent eluted to the solid polymer isolated is that volume ratio is in step 3
(92~98): the dehydrated alcohol of (8~2) and the mixed solution of acetic acid.
It is further preferred that drying temperature is 30~60 DEG C in step 3, drying time is 3~8h.
The invention also discloses using hydrophily sulindac molecular engram magnetic Nano tree made from above-mentioned preparation method
Rouge ball, which is characterized in that the partial size of the hydrophily sulindac molecular engram magnetic Nano resin balls is 130~150nm.
Preferably, which is that can adsorb analgesic type drug sulindac
Magnetic molecularly imprinted nanometer resin ball, be 33.82~36.17mg/g to the adsorbance of sulindac.
The invention also discloses above-mentioned hydrophily sulindac molecular engram magnetic Nano resin balls as analgesic type drug
The application of sulindac adsorbent.
The invention also discloses above-mentioned hydrophily sulindac molecular engram magnetic Nano resin balls to detect and separate dirt
Application in water in sulindac.
Compared with prior art, the invention has the following advantages:
The preparation method of the first public hydrophily sulindac molecular engram magnetic Nano resin balls of the present invention, firstly, using
Hydro-thermal method one-step synthesis carboxyl magnetic nano-balls；Then, carboxyl magnetic nano-balls and sulindac are added to ammonia aqueous solution
In, after being sufficiently stirred at room temperature, resorcinol is added and carries out initial reaction, adds formaldehyde and is polymerize；Finally, by outer
Add magnet to separate the polymer of generation, arrives target product after eluting, drying.The invention has the following advantages that
(1) it both may be implemented in the quick separating of solid-liquid under externally-applied magnetic field as carrier using carboxyl magnetic nano-balls, ensure that carrier
Good dispersion；(2) simultaneously using resorcinol and formaldehyde as miscellaneous function monomer and crosslinking agent, hydrogen bond and π-π can be passed through
Effect is sufficiently acted on template molecule, and reacts simple easily operated；(3) phenolic resin is due to low with synthesis material price
Honest and clean, the advantages that chemical corrosion resistance is strong, thermal stability is high and hydrophily is strong and used as molecular engram layer.The present invention
In, it is rich that selective absorption is carried out to the sulindac in sewage using emerging pollutant sulindac magnetic molecularly imprinted nanosphere for the first time
Collection.
Through hydrophily sulindac molecular engram magnetic Nano resin balls, uniform particle diameter, structure made from the method for the present invention
Stability is good, magnetic response is strong, reusable property is strong, good hydrophilic property, and the strong, adsorbance to the selective adsorption capacity of sulindac
Greatly, the rate of recovery is high, while lower cost for material, and preparation is simple, is sulindac in a kind of high-selectivity enrichment and removal sewage
Method, in sewage the Selective Separation of emerging pollutant sulindac, enrichment, in terms of show wide application before
Scape.
Realizing for the first time through hydrophily sulindac molecular engram magnetic Nano resin balls made from the method for the present invention can be direct
Sulindac in selective absorption sewage, sample are not necessarily to any pretreatment, reduce the consumption of organic solvent.The magnetism of acquisition point
Sub- trace nanometer resin ball shows high binding capacity, the fast rate of adsorption, good power of regeneration and good choosing to sulindac
Selecting property.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the carboxyl magnetic nano-balls of 1 step 1 of embodiment of the present invention synthesis.
Fig. 2 is the transmission electron microscope of hydrophily sulindac molecular engram magnetic Nano resin balls made from the embodiment of the present invention 1
Figure.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work
It encloses.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Cover it is non-exclusive include, for example, the process, method, system, product or equipment for containing a series of steps or units are not necessarily limited to
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that equipment is intrinsic.
The invention will be described in further detail with reference to the accompanying drawing:
Embodiment 1
A kind of preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls, comprising the following steps:
Step 1: by 0.30g iron chloride, 1.00g sodium acetate, 0.02g Sodium Polyacrylate, 6.6mL ethylene glycol and 10mL mono-
Diglycol ethylene is placed in reaction kettle, and 7h is reacted at 180 DEG C, after reaction, by reaction product milli-Q water into
Property.Then, products therefrom is dried in vacuo to 3h at 30 DEG C, 0.05MPa to get carboxyl magnetic nano-balls are arrived.As shown in Figure 1,
The partial size of carboxyl magnetic nano-balls obtained is about 110~120nm.
Step 2: 100mg carboxyl magnetic nano-balls, 10mg sulindac, 5mL ultrapure water and 1.8mL ammonium hydroxide are placed in reaction
In container, it is stirred to react 10min at room temperature, adds 0.01g resorcinol stirring 0.5h, is eventually adding 0.01mL formaldehyde,
Polymerization reaction 3h at room temperature, and solidify 6h at 18 DEG C.
Step 3: the solid polymer generated in step 2 reaction solution is divided by externally-applied magnetic field after polymerization reaction
It separates out and；
Step 4: the solid-state isolated in the mixed liquor elution step three of the dehydrated alcohol and acetic acid that are 92:8 with volume ratio
Polymer.Solid polymer after elution dries 3h at 30 DEG C again to get hydrophily sulindac molecular engram magnetic Nano tree
Rouge ball.As shown in Fig. 2, the partial size of hydrophily sulindac molecular engram magnetic Nano resin balls obtained is about 130~150nm.
Hydrophily sulindac molecular engram magnetic Nano resin balls made from embodiment 1 are subjected to absorption property detection, tool
Body is as follows:
(1) hydrophily sulindac molecular engram magnetic Nano resin balls 10mg is added to 10mL concentration is 350 μ g/mL's
In the aqueous solution of sulindac, after vibrating 30min at room temperature, supernatant separation is come out by externally-applied magnetic field；
(2) concentration of sulindac in gained supernatant in (1) is measured with HPLC, then calculates hydrophily sulindac molecule print
Adsorbance of the mark magnetic Nano resin balls to sulindac；
The concentration of sulindac is 316.18 μ g/mL in measured supernatant.
Calculation formula of the hydrophily sulindac molecular engram magnetic Nano resin balls to the adsorbance of sulindac are as follows:
C in formulaeFor the concentration of sulindac in above-mentioned supernatant；
By calculating, adsorbance of the hydrophily sulindac molecular engram magnetic Nano resin balls to sulindac are as follows:
33.82mg/g。
Embodiment 2
A kind of preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls, comprising the following steps:
Step 1: 0.45g iron chloride, 1.5g sodium acetate, 0.03g Sodium Polyacrylate, 6.8mL ethylene glycol and 12mL mono- are contracted
Diethylene glycol is placed in reaction kettle, and 10h is reacted at 190 DEG C, after reaction, by reaction product milli-Q water into
Property.Then, will under 45 DEG C of products therefrom, 0.05MPa be dried in vacuo 4.5h to get arrive carboxyl magnetic nano-balls.
Step 2: 110mg carboxyl magnetic nano-balls, 12mg sulindac, 6mL ultrapure water and 1.85mL ammonium hydroxide are placed in reaction
In container, it is stirred to react 20min at room temperature, adds 0.04g resorcinol stirring 0.8h, is eventually adding 0.02mL formaldehyde,
Polymerization reaction 4h at room temperature, and solidify 8h at 20 DEG C.
Step 3: the solid polymer generated in step 2 reaction solution is divided by externally-applied magnetic field after polymerization reaction
It separates out and；
Step 4: the solid-state isolated in the mixed liquor elution step three of the dehydrated alcohol and acetic acid that are 93:7 with volume ratio
Polymer.Solid polymer after elution dries 4.5h at 45 DEG C again to get hydrophily sulindac molecular engram magnetic Nano
Resin balls.
Hydrophily sulindac molecular engram magnetic Nano resin balls made from embodiment 2 are subjected to absorption property detection, tool
Body is as follows:
(1) hydrophily sulindac molecular engram magnetic Nano resin balls 10mg is added to 10mL concentration is 350 μ g/mL's
In the aqueous solution of sulindac, after vibrating 30min at room temperature, supernatant separation is come out by externally-applied magnetic field；
(2) concentration of sulindac in gained supernatant in (1) is measured with HPLC, then calculates hydrophily sulindac molecule print
Adsorbance of the mark magnetic Nano resin balls to sulindac；
The concentration of sulindac is 315.04 μ g/mL in measured supernatant.
Calculation formula of the hydrophily sulindac molecular engram magnetic Nano resin balls to the adsorbance of sulindac are as follows:
In formula, CeFor the concentration of sulindac in above-mentioned supernatant；
By calculating, adsorbance of the hydrophily sulindac molecular engram magnetic Nano resin balls to sulindac are as follows:
34.96mg/g。
Embodiment 3
A kind of preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls, comprising the following steps:
Step 1: 0.504g iron chloride, 2.0g sodium acetate, 0.05g Sodium Polyacrylate, 7mL ethylene glycol and 13mL mono- are contracted
Diethylene glycol is placed in reaction kettle, and 11h is reacted at 200 DEG C, after reaction, by reaction product milli-Q water into
Property.Then, will under 50 DEG C of products therefrom, 0.05MPa be dried in vacuo 5.5h to get arrive carboxyl magnetic nano-balls.
Hold Step 2: 250mg carboxyl magnetic nano-balls, 20mg sulindac, 10mL ultrapure water and 2mL ammonium hydroxide are placed in reaction
In device, it is stirred to react 30min at room temperature, adds 0.1g resorcinol stirring 1.2h, 0.05mL formaldehyde is eventually adding, in room temperature
Lower polymerization reaction 6h, and solidify 10h at 25 DEG C.
Step 3: the solid polymer generated in step 2 reaction solution is divided by externally-applied magnetic field after polymerization reaction
It separates out and；
Step 4: the solid-state isolated in the mixed liquor elution step three of the dehydrated alcohol and acetic acid that are 95:5 with volume ratio
Polymer.Solid polymer after elution dries 5h at 50 DEG C again to get hydrophily sulindac molecular engram magnetic Nano tree
Rouge ball.
Hydrophily sulindac molecular engram magnetic Nano resin balls made from embodiment 3 are subjected to absorption property detection, tool
Body is as follows:
(1) hydrophily sulindac molecular engram magnetic Nano resin balls 10mg is added to 10mL concentration is 350 μ g/mL's
In the aqueous solution of sulindac, after vibrating 30min at room temperature, supernatant separation is come out by externally-applied magnetic field；
(2) concentration of sulindac in gained supernatant in (1) is measured with HPLC, then calculates hydrophily sulindac molecule print
Adsorbance of the mark magnetic Nano resin balls to sulindac；
The concentration of sulindac is 314 μ g/mL in measured supernatant.
Calculation formula of the hydrophily sulindac molecular engram magnetic Nano resin balls to the adsorbance of sulindac are as follows:
C in formulaeFor the concentration of sulindac in above-mentioned supernatant；
By calculating, adsorbance of the hydrophily sulindac molecular engram magnetic Nano resin balls to sulindac are as follows: 36mg/g.
Embodiment 4
A kind of preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls, comprising the following steps:
Step 1: by 0.60g iron chloride, 2.50g sodium acetate, 0.05g Sodium Polyacrylate, 8mL ethylene glycol and 13.5mL mono-
Diglycol ethylene is placed in reaction kettle, and 12.5h is reacted at 200 DEG C, after reaction, extremely with milli-Q water by reaction product
It is neutral.Then, will under 55 DEG C of products therefrom, 0.07MPa be dried in vacuo 5.5h to get arrive carboxyl magnetic nano-balls.
Step 2: 300mg carboxyl magnetic nano-balls, 30mg sulindac, 30mL ultrapure water and 2.5mL ammonium hydroxide are placed in reaction
In container, it is stirred to react 40min at room temperature, adds 0.2g resorcinol stirring 1.8h, 0.09mL formaldehyde is eventually adding, in room
The lower polymerization reaction 5h of temperature, and solidify 9h at 35 DEG C.
Step 3: the solid polymer generated in step 2 reaction solution is divided by externally-applied magnetic field after polymerization reaction
It separates out and；
Step 4: the solid-state isolated in the mixed liquor elution step three of the dehydrated alcohol and acetic acid that are 97:3 with volume ratio
Polymer.Solid polymer after elution dries 5.5h at 55 DEG C again to get hydrophily sulindac molecular engram magnetic Nano
Resin balls.
Hydrophily sulindac molecular engram magnetic Nano resin balls made from embodiment 4 are subjected to absorption property detection, tool
Body is as follows:
(1) hydrophily sulindac molecular engram magnetic Nano resin balls 10mg is added to 10mL concentration is 350 μ g/mL's
In the aqueous solution of sulindac, after vibrating 30min at room temperature, supernatant separation is come out by externally-applied magnetic field；
(2) concentration of sulindac in gained supernatant in (1) is measured with HPLC, then calculates hydrophily sulindac molecule print
Adsorbance of the mark magnetic Nano resin balls to sulindac；
The concentration of sulindac is 314.32 μ g/mL in measured supernatant.
Calculation formula of the hydrophily sulindac molecular engram magnetic Nano resin balls to the adsorbance of sulindac are as follows:
C in formulaeFor the concentration of sulindac in above-mentioned supernatant；
By calculating, adsorbance of the hydrophily sulindac molecular engram magnetic Nano resin balls to sulindac are as follows:
35.68mg/g。
Embodiment 5
A kind of preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls, comprising the following steps:
Step 1: by 0.65g iron chloride, 3.0g sodium acetate, 0.055g Sodium Polyacrylate, 8.1mL ethylene glycol and 13.8mL
Diglycol is placed in reaction kettle, and 13h is reacted at 200 DEG C, after reaction, extremely with milli-Q water by reaction product
It is neutral.Then, will under 60 DEG C of products therefrom, 0.09MPa be dried in vacuo 6h to get arrive carboxyl magnetic nano-balls.
Step 2: 350mg carboxyl magnetic nano-balls, 40mg sulindac, 33mL ultrapure water and 3.0mL ammonium hydroxide are placed in reaction
In container, it is stirred to react 45min at room temperature, adds 0.25g resorcinol stirring 2.2h, is eventually adding 0.10mL formaldehyde,
Polymerization reaction 7h at room temperature, and solidify 11h at 45 DEG C.
Step 3: the solid polymer generated in step 2 reaction solution is divided by externally-applied magnetic field after polymerization reaction
It separates out and；
Step 4: the solid-state isolated in the mixed liquor elution step three of the dehydrated alcohol and acetic acid that are 98:2 with volume ratio
Polymer.Solid polymer after elution dries 6h at 60 DEG C again to get hydrophily sulindac molecular engram magnetic Nano tree
Rouge ball.
Hydrophily sulindac molecular engram magnetic Nano resin balls made from embodiment 5 are subjected to absorption property detection, tool
Body is as follows:
(1) hydrophily sulindac molecular engram magnetic Nano resin balls 10mg is added to 10mL concentration is 350 μ g/mL's
In the aqueous solution of sulindac, after vibrating 30min at room temperature, supernatant separation is come out by externally-applied magnetic field；
(2) concentration of sulindac in gained supernatant in (1) is measured with HPLC, then calculates hydrophily sulindac molecule print
Adsorbance of the mark magnetic Nano resin balls to sulindac；
The concentration of sulindac is 314.22 μ g/mL in measured supernatant.
Calculation formula of the hydrophily sulindac molecular engram magnetic Nano resin balls to the adsorbance of sulindac are as follows:
C in formulaeFor the concentration of sulindac in above-mentioned supernatant；
By calculating, adsorbance of the hydrophily sulindac molecular engram magnetic Nano resin balls to sulindac are as follows:
35.78mg/g。
Embodiment 6
A kind of preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls, comprising the following steps:
Step 1: 0.80g iron chloride, 3.5g sodium acetate, 0.06g Sodium Polyacrylate, 8.2mL ethylene glycol and 14mL mono- are contracted
Diethylene glycol is placed in reaction kettle, and 14h is reacted at 200 DEG C, after reaction, by reaction product milli-Q water into
Property.Then, will under 58 DEG C of products therefrom, 0.08MPa be dried in vacuo 8h to get arrive carboxyl magnetic nano-balls.
Step 2: 500mg carboxyl magnetic nano-balls, 50mg sulindac, 35mL ultrapure water and 6.5mL ammonium hydroxide are placed in reaction
In container, it is stirred to react 50min at room temperature, adds 2.8g resorcinol stirring 2.5h, 1.2mL formaldehyde is eventually adding, in room
The lower polymerization reaction 8h of temperature, and solidify 12h at 60 DEG C.
Step 3: the solid polymer generated in step 2 reaction solution is divided by externally-applied magnetic field after polymerization reaction
It separates out and；
Step 4: the solid-state isolated in the mixed liquor elution step three of the dehydrated alcohol and acetic acid that are 94:6 with volume ratio
Polymer.Solid polymer after elution dries 8h at 48 DEG C again to get hydrophily sulindac molecular engram magnetic Nano tree
Rouge ball.
Hydrophily sulindac molecular engram magnetic Nano resin balls made from embodiment 6 are subjected to absorption property detection, tool
Body is as follows:
(1) hydrophily sulindac molecular engram magnetic Nano resin balls 10mg is added to 10mL concentration is 350 μ g/mL's
In the aqueous solution of sulindac, after vibrating 30min at room temperature, supernatant separation is come out by externally-applied magnetic field；
(2) concentration of sulindac in gained supernatant in (1) is measured with HPLC, then calculates hydrophily sulindac molecule print
Adsorbance of the mark magnetic Nano resin balls to sulindac；
The concentration of sulindac is 313.83 μ g/mL in measured supernatant.
Calculation formula of the hydrophily sulindac molecular engram magnetic Nano resin balls to the adsorbance of sulindac are as follows:
C in formulaeFor the concentration of sulindac in above-mentioned supernatant；
By calculating, adsorbance of the hydrophily sulindac molecular engram magnetic Nano resin balls to sulindac are as follows:
36.17mg/g。
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. a kind of preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls characterized by comprising firstly,
Using hydro-thermal method one-step synthesis carboxyl magnetic nano-balls；Then, carboxyl magnetic nano-balls, sulindac are added in ultrapure water,
Ammonium hydroxide is then added, the compound of template-carrier is made；Resorcinol and formaldehyde is added into template-carrier compound again
It is polymerize, obtains solid polymer；Finally, solid polymer is separated by externally-applied magnetic field, the solid-state that will be isolated
After polymer elution, drying, hydrophily sulindac molecular engram magnetic Nano resin balls are made.
2. the preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls according to claim 1, feature
It is, comprising the following steps:
Step 1: by iron chloride, sodium acetate, Sodium Polyacrylate, ethylene glycol and diglycol according to (0.3~0.8) g:
(1.0~3.5) g:(0.02~0.06) g:(6.6~8.2) mL:(10~14) and mL amount ratio, be placed in reaction kettle, 180
7~16h is reacted at~220 DEG C, after reaction, by reaction product washing, vacuum drying, carboxyl magnetic nano-balls is made；
Step 2: carboxyl magnetic nano-balls, sulindac, ultrapure water and ammonium hydroxide are stirred at room temperature according to being placed in reaction vessel
10~50min is reacted, resorcinol is added and stirs 0.5~2.5h, be eventually adding formaldehyde, at room temperature 3~8h of polymerization reaction,
And solidify 6~12h；
Wherein, the amount ratio of carboxyl magnetic nano-balls, sulindac, ultrapure water, ammonium hydroxide, resorcinol and formaldehyde is (100~500)
Mg:(10~50) mg:(5~35) mL:(1.8~6.5) mL:(0.01~2.8) g:(0.01~1.2) mL；
Step 3: separated the solid polymer generated in step 2 after reaction reaction solution by externally-applied magnetic field, then
The solid polymer isolated is eluted, is dried, hydrophily sulindac molecular engram magnetic Nano resin balls are made.
3. the preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls according to claim 2, feature
It is, in step 1, is washed reaction product to neutrality, then in 30~60 DEG C, the item of 0.05~0.09MPa using ultrapure water
Under part, it is dried in vacuo 3~8h.
4. the preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls according to claim 2, feature
It is, in step 2, solidification temperature is 18~60 DEG C.
5. the preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls according to claim 2, feature
It is, in step 3, the eluent eluted to the solid polymer isolated is that volume ratio is (92~98): (8~2)
The mixed solution of dehydrated alcohol and acetic acid.
6. the preparation method of hydrophily sulindac molecular engram magnetic Nano resin balls according to claim 2, feature
It is, in step 3, drying temperature is 30~60 DEG C, and drying time is 3~8h.
7. magnetic using hydrophily sulindac molecular engram made from preparation method described in any one of claim 1~6
Nanometer resin ball, which is characterized in that the partial size of the hydrophily sulindac molecular engram magnetic Nano resin balls is 130~150nm.
8. hydrophily sulindac molecular engram magnetic Nano resin balls according to claim 7, which is characterized in that this is hydrophilic
Property sulindac molecular engram magnetic Nano resin balls are that can adsorb the magnetic molecularly imprinted nanotrees of analgesic type drug sulindac
Rouge ball, the adsorbance to sulindac are 33.82~36.17mg/g.
9. hydrophily sulindac molecular engram magnetic Nano resin balls are as analgesic type drug Shu Lin described in claim 7 or 8
The application of sour adsorbent.
10. hydrophily sulindac molecular engram magnetic Nano resin balls described in claim 7 or 8 are being detected and are being separated in sewage
Application in sulindac.
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