CN106861652A - A kind of preparation method of the magnetic mesoporous imprinted material of sandwich structure that can separate gold or silver - Google Patents
A kind of preparation method of the magnetic mesoporous imprinted material of sandwich structure that can separate gold or silver Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of the magnetic mesoporous imprinted material of sandwich structure that can separate gold or silver, superparamagnetism Fe is synthesized using hydro-thermal method3O4Nanocluster, with reference to hexadecane trimethyl ammonium bromide template, using gold or silver ion as template ion, using the siloxanes of band functional group as function monomer, there is the molecular engram mesoporous material of high selectivity to gold or silver ion using the synthesis of silicate class sol-gal process.The invention has the advantages that can separate gold or silver the magnetic mesoporous imprinted material of sandwich structure to gold or silver have specific recognition ability, with magnetic responsiveness high, high-adsorption-capacity, the rate of adsorption high, strong anti acid alkali performance, and can realize to gold or silver efficiently concentrating and while separation simplify solid-liquor separation flow.
Description
Technical field
The present invention relates to a kind of preparation method of the magnetic mesoporous imprinted material of sandwich structure that can separate gold or silver, belong to
Technical field of material.
Background technology
The high efficiency extraction of low-concentration gold or silver is separated and typically uses extraction in solution, the extraction of existing extraction gold or silver
Agent has thiocarbamide, cyanide, ethyl acetate, methyl iso-butyl ketone (MIBK), trioctyl phosphine oxide, tricaprylmethyl ammonium salt, dibutyl card
Must alcohol or tributyl phosphate, but existing process exist high cost, pollution environment, technological process is long, labour intensity is big, continuity
Differ from, be not easy to operation, separating effect and yield are also undesirable.Metal ingredient should be allowed to separate in process of production thorough, again
Allow its be easy to reclaim, and yield the higher the better.This is accomplished by improving or changing original correlation technique.Adsorption technology has power consumption
Low, simple to operate, good selective, golden or silver efficiently separates in achievable low concentration complex system.Therefore, it is necessary to
Research is suitable for the imprinted material of adsorption of Low Concentration gold or silver.
The content of the invention
It is an object of the invention to provide a kind of system of the magnetic mesoporous imprinted material of sandwich structure that can separate gold or silver
Preparation Method.
To achieve these goals, the present invention by the following method realize by scheme：A kind of sandwich that can separate gold or silver
The preparation method of the mesoporous imprinted material of structure magnetic, comprises the following steps：
（1）Nanometer Fe3O4The preparation of cluster：By FeCl3 .6H2O：Sodium acetate：The mass ratio of polyethylene glycol is（2.2~3.2）：
（6.5~7.8）：（1.5~2.5）, take FeCl3 .6H2O, sodium acetate and polyethylene glycol, then by above-mentioned three and the quality of ethylene glycol
Volume ratio g/mL is calculated as（10.2~13.5）：（5~500）, by FeCl3 .6H2O, sodium acetate and polyethylene glycol are added in ethylene glycol,
Magnetic agitation is allowed to dissolve, and the homogeneous yellow mixed solution that will be obtained is sealed in being transferred to polytetrafluoro hydrothermal reaction kettle, is heated to
6~72h is reacted at 160~250 DEG C, after naturally cool to room temperature, black particle thing is obtained, is washed for several times with ethanol, then carry out
Freeze-drying or vacuum drying, that is, obtain nanometer Fe3O4Cluster；This step is with ethylene glycol as solvent, polyethylene glycol as stabilizer,
Iron chloride is source of iron, controllable using solvent-thermal method size（1~600nm）, the nanometer Fe that the intensity of magnetization is high and monodispersity is good3O4
Cluster；
（2）Core shell structure Fe3O4@nSiO2The preparation of carrier：By step（1）Gained nanometer Fe3O4The cluster salt of 0.1mol/L
Ultrasonically treated 5~the 20min of acid solution, then alternately washed for several times, then by nanometer Fe with ethanol and deionized water3O4Cluster and water
The solid-to-liquid ratio g/mL for solving liquid is calculated as（0.05~0.15）:（90~100）, by the nanometer Fe after washing3O4Cluster is distributed to hydrolyzate
In, then 1~100mmol/L containing silicon ion in silicon source to system is slowly added dropwise, and 1~72h is stirred, it is scrubbed, obtain nucleocapsid knot
Structure Fe3O4@nSiO2Carrier；Add generation silicone hydroxyl (Si-OH) and Fe in the hydrolytic process of silicon source3O4The hydroxyl on surface there occurs
Condensation reaction, constantly hydrolytic condensation, finally in nanometer Fe3O4Cluster surface forms the nSiO of densification2Clad；According to waiting to locate
The acidity of solution is managed, the consumption and reaction time for changing silicon source regulate and control nSiO2The thickness of clad, if the acid of pending solution
Spend bigger, required nSiO2The thickness of clad is thicker, then the corresponding amount for adding silicon source is bigger, and the reaction time is more long；
（3）The preparation of function monomer-template molecule host-guest coordination compound：By the functional polyorganosiloxane monomer and gold or silver of band functional group
The mol ratio of ion is 1：（1.2~1.5）, the functional polyorganosiloxane monomer of band functional group is mixed with target gold or silver ion solution
Close, obtain function monomer-template molecule host-guest coordination compound；
（4）The preparation of polymer matrix：By core shell structure Fe3O4@nSiO2The ratio g/mmol of carrier and complex is calculated as（0.05~
0.15）:（0.15~0.25）, by step（3）Gained function monomer-template molecule host-guest coordination compound and step（2）Gained core
Shell structure Fe3O4@nSiO2Support dispersion is in condensation liquid, then the silicon source of 0.3~0.5 mass parts to system is added dropwise in stirring
In, and 1~72h is stirred, it is scrubbed to obtain polymer matrix；In slow hydrolytic condensation, progressively aggregate into containing CTAB certainly
The polymer matrix of assembling micella and gold or silver ion dual mould plate；
（5）By acetone extraction method removing step（4）CTAB in resulting polymers parent, leaves orderly on polymer matrix
It is mesoporous, back extraction is carried out as the eluant, eluent of target gold or silver ion using complexing agent or acid solution and removes gold or silver ion, leave with
The micropore that target gold or silver ion space structure and action site are mutually matched, that is, obtain that the sandwich knot of gold or silver can be separated
The magnetic mesoporous imprinted material IIP-Fe of structure3O4@nSiO2@mSiO2。
The step（1）Polyethylene glycol and ethylene glycol be it is purchased in market analysis it is pure.
The step（2）With（4）Silicon source for tetraethyl orthosilicate, methyl silicate, butyl silicate, positive silicic acid propyl ester or
Other silicate class, are analysis purchased in market pure.
The step（2）Hydrolyzate be made up of the component of following parts by volume：75~85 parts of ethanol, deionized water 15~25
Part, concentration are 0.5~1.5 part of the ammoniacal liquor of 28wt%.
The step（2）Ethanol for it is purchased in market analysis it is pure.
The step（3）Functional polyorganosiloxane monomer with functional group is F-CH2CH2-NHCH2CH2CH2Si(OMe)3。
The F is-COOH ,-NH2,-POOH or-SH.
The step（3）Target gold or silver ion solution be containing target gold or the mol/L of silver ion 0.1~2 it is molten
Liquid, target gold or silver ion are provided by its simple substance, oxide, nitric acid thing or chloride etc., by soluble solvent（Such as water or nothing
Machine acid）Target gold or silver ion solution are obtained after dissolving.
The step（4）Condensation liquid including following parts by volume component：55~65 parts of ethanol, deionized water 75~85
Part, concentration are 0.5~1.5 part of the ammoniacal liquor of 28wt%, and the CTAB of 0.1~0.4 mass parts is added in liquid mixed above.
The step（5）Complexing agent be thiocarbamide, cyanide, ethyl acetate, methyl tert-butyl that concentration is 0.1~2mol/L
Base ketone, tri octyl phosphine type oxide, tricaprylmethyl ammonium salt, dibutyl carbitol (DBC) or tributyl phosphate.
The step（5）Acid solution be nitric acid and/or hydrochloric acid solution that concentration is 0.1~2mol/L, nitric acid and hydrochloric acid
Mixed liquor be arbitrary proportion mixing.
Gained can separate gold or the magnetic mesoporous imprinted material of sandwich structure of silver can realize target metal ions from waiting to inhale
Efficiently separated in attached liquid, be specifically added to imprinted material as adsorbent in the liquid to be adsorbed containing target gold or silver ion
（Target gold or silver ion in liquid to be adsorbed are low concentration, 0.1~100mmol/L）, absorption 10min or so, surveyed with ICP-OES
The concentration of metal ion, calculates adsorption rate, up to more than 90% in the front and rear liquid to be adsorbed of amount absorption.
The adsorbent for terminating is adsorbed to be reclaimed using Magneto separate, and the washing that adds water is subsequently adding complexing agent or acid to weakly acidic pH
Solution carries out desorption gold or silver as stripping liquid（Stripping liquid is consistent with the eluant, eluent used when synthesizing the adsorbent）, when different
Between sample, measure concentration of metal ions, adsorption rate, up to more than 90% in stripping liquid with ICP-OES.After desorption terminates, adsorbent
Reclaimed using Magneto separate, dried after being washed to weakly acidic pH, you can recycle.
The present invention is with superparamagnetic core-shell structure Fe3O4@SiO2It is core, it is with gold or silver ion trace and mesoporous with rule
Structure SiO2It is shell, the magnetic mesoporous imprinted material (IIP-Fe of the sandwich structure obtained by preparation3O4@nSiO2@mSiO2) can be in magnetic
Solution efficiently separates after nm of gold or silver-colored adsorbent being realized under power auxiliary and being adsorbed.
The invention has the advantages that：（1）The magnetic mesoporous imprinted material of sandwich structure of gained, not only material structure set
Meter is novel, and the technology of preparing of material functional has innovation, is capable of achieving the efficiently concentrating to gold or silver and letter while separation
Change solid-liquor separation flow.（2）Gained can separate gold or silver the magnetic mesoporous imprinted material of sandwich structure have magnetic responsiveness high,
High-adsorption-capacity, the rate of adsorption high, strong anti acid alkali performance, and have specific recognition ability to gold or silver.
Specific embodiment
The present invention is further specifically described below by specific embodiment, but is not to be construed as protecting the present invention
Protect the restriction of scope.
Embodiment 1
（1）Nanometer Fe3O4The preparation of cluster：By FeCl3 .6H2O：Sodium acetate：The mass ratio of polyethylene glycol is 2.2：6.5：1.5,
Take FeCl3 .6H2O, sodium acetate and polyethylene glycol, then it is calculated as 10.2 by the mass volume ratio g/mL of above-mentioned three and ethylene glycol：5,
By FeCl3 .6H2O, sodium acetate and polyethylene glycol are added in ethylene glycol, and magnetic agitation is allowed to dissolve, and the homogeneous yellow that will be obtained is mixed
Close during solution is transferred to polytetrafluoro hydrothermal reaction kettle and seal, 72h is reacted at being heated to 160 DEG C, after naturally cool to room temperature, obtain
Black particle thing, is washed 6 times with ethanol, then carries out freeze-drying or vacuum drying, that is, obtain nanometer Fe3O4Cluster；
（2）Core shell structure Fe3O4@nSiO2The preparation of carrier：By step（1）Gained nanometer Fe3O4The cluster salt of 0.1mol/L
The ultrasonically treated 5min of acid solution, then with alternately washing 6 times of ethanol and deionized water, then by nanometer Fe3O4Cluster and hydrolyzate
Solid-to-liquid ratio g/mL is calculated as 0.05:90, by the nanometer Fe after washing3O4Cluster is distributed in hydrolyzate, then is slowly added dropwise positive silicic acid second
1mmol/L containing silicon ion in ester to system, and 1h is stirred, it is scrubbed, obtain core shell structure Fe3O4@nSiO2Carrier；The hydrolysis
Liquid is made up of the component of following parts by volume：75 parts of ethanol, 15 parts of deionized water, concentration are 0.5 part of the ammoniacal liquor of 28wt%；
（3）The preparation of function monomer-template molecule host-guest coordination compound：By the functional polyorganosiloxane monomer and gold ion of band functional group
Mol ratio be 1：1.2, by COOH-CH2CH2-NHCH2CH2CH2Si(OMe)3Mix with target gold ion solution, obtain function
Monomer-template molecule host-guest coordination compound；Wherein, target gold ion solution is the solution containing gold ion 0.1mol/L；
（4）The preparation of polymer matrix：By core shell structure Fe3O4@nSiO2The ratio g/mmol of carrier and complex is calculated as 0.05:
0.15, by step（3）Gained function monomer-template molecule host-guest coordination compound and step（2）Gained core shell structure Fe3O4@
nSiO2Support dispersion is in condensation liquid, then is added dropwise in the tetraethyl orthosilicate of 0.3 mass parts to system in stirring, and stirs 1h,
It is scrubbed to obtain polymer matrix；The condensation liquid includes the component of following parts by volume：It is 55 parts of ethanol, 75 parts of deionized water, dense
0.5 part of the ammoniacal liquor for 28wt% is spent, and the CTAB of 0.1 mass parts is added in liquid mixed above；
（5）By acetone extraction method removing step（4）CTAB in resulting polymers parent, leaves orderly on polymer matrix
Mesoporous, the thiocarbamide using concentration as 0.1mol/L carries out back extraction and removes gold ion as the eluant, eluent of gold ion, leaves and target gold
The ion space micropore that structurally and functionally site mutually matches, that is, obtain that the magnetic mesoporous trace of sandwich structure of gold can be separated
Material IIP-Fe3O4@nSiO2@mSiO2。
The magnetic mesoporous imprinted material of sandwich structure that gained can separate gold can realize target metal ions from liquid to be adsorbed
In efficiently separate, be specifically added to imprinted material as adsorbent in the liquid to be adsorbed containing target gold ion（It is to be adsorbed
Target gold ion concentration in liquid is 0.1mmol/L）, absorption 10min or so, measure the front and rear liquid to be adsorbed of absorption with ICP-OES
The concentration of middle metal ion, calculates adsorption rate, up to 97%.
The adsorbent for terminating is adsorbed to be reclaimed using Magneto separate, and the washing that adds water is subsequently adding complexing agent or acid to weakly acidic pH
Solution carries out desorption gold as stripping liquid（Stripping liquid is consistent with the eluant, eluent used when synthesizing the adsorbent）, taken in different time
Sample, with concentration of metal ions, adsorption rate, up to 96% in ICP-OES measurement stripping liquids.After desorption terminates, adsorbent uses Magneto separate
Reclaim, dried after being washed to weakly acidic pH, you can recycle.
Embodiment 2
（1）Nanometer Fe3O4The preparation of cluster：By FeCl3 .6H2O：Sodium acetate：The mass ratio of polyethylene glycol is 2.7：7.2：2, take
FeCl3 .6H2O, sodium acetate and polyethylene glycol, then it is calculated as 11.9 by the mass volume ratio g/mL of above-mentioned three and ethylene glycol：100,
By FeCl3 .6H2O, sodium acetate and polyethylene glycol are added in ethylene glycol, and magnetic agitation is allowed to dissolve, and the homogeneous yellow that will be obtained is mixed
Close during solution is transferred to polytetrafluoro hydrothermal reaction kettle and seal, 36h is reacted at being heated to 200 DEG C, after naturally cool to room temperature, obtain
Black particle thing, is washed 5 times with ethanol, then carries out freeze-drying or vacuum drying, that is, obtain nanometer Fe3O4Cluster；
（2）Core shell structure Fe3O4@nSiO2The preparation of carrier：By step（1）Gained nanometer Fe3O4The cluster salt of 0.1mol/L
The ultrasonically treated 10min of acid solution, then with alternately washing 5 times of ethanol and deionized water, then by nanometer Fe3O4Cluster and hydrolyzate
Solid-to-liquid ratio g/mL be calculated as 0.1:95, by the nanometer Fe after washing3O4Cluster is distributed in hydrolyzate, then is slowly added dropwise positive silicic acid
10mmol/L containing silicon ion in methyl esters to system, and 36h is stirred, it is scrubbed, obtain core shell structure Fe3O4@nSiO2Carrier；It is described
Hydrolyzate is made up of the component of following parts by volume：80 parts of ethanol, 20 parts of deionized water, concentration are 1 part of the ammoniacal liquor of 28wt%；
（3）The preparation of function monomer-template molecule host-guest coordination compound：By the functional polyorganosiloxane monomer and gold or silver of band functional group
The mol ratio of ion is 1：1.3, by NH2-CH2CH2-NHCH2CH2CH2Si(OMe)3Mix with target silver ion solution, obtain work(
Can monomer-template molecule host-guest coordination compound；Wherein, target silver ion solution is the solution containing silver ion 1mol/L；
（4）The preparation of polymer matrix：By core shell structure Fe3O4@nSiO2The ratio g/mmol of carrier and complex is calculated as 0.1:
0.2, by step（3）Gained function monomer-template molecule host-guest coordination compound and step（2）Gained core shell structure Fe3O4@nSiO2
Support dispersion is in condensation liquid, then is added dropwise in the methyl silicate of 0.4 mass parts to system in stirring, and stirs 36h, through washing
Wash and obtain polymer matrix；The condensation liquid includes the component of following parts by volume：60 parts of ethanol, 80 parts of deionized water, concentration are
1 part of the ammoniacal liquor of 28wt%, and the CTAB of 0.3 mass parts is added in liquid mixed above；
（5）By acetone extraction method removing step（4）CTAB in resulting polymers parent, leaves orderly on polymer matrix
Mesoporous, the salpeter solution using concentration as 1mol/L carries out back extraction and removes silver ion as the eluant, eluent of silver ion, leaves and target
The micropore that silver ion space structure and action site are mutually matched, that is, obtain the magnetic mesoporous print of sandwich structure of energy separation of Silver
Mark material IIP-Fe3O4@nSiO2@mSiO2。
The magnetic mesoporous imprinted material of sandwich structure of gained energy separation of Silver can realize target metal ions from liquid to be adsorbed
In efficiently separate, be specifically added to imprinted material as adsorbent in the liquid to be adsorbed containing target silver ion（It is to be adsorbed
Target concentration of silver ions in liquid is 10mmol/L）, absorption 10min or so, with the ICP-OES front and rear liquid to be adsorbed of measurement absorption
The concentration of metal ion, calculates adsorption rate, up to 98%.
The adsorbent for terminating is adsorbed to be reclaimed using Magneto separate, and the washing that adds water is subsequently adding complexing agent or acid to weakly acidic pH
Solution carries out desorption silver as stripping liquid（Stripping liquid is consistent with the eluant, eluent used when synthesizing the adsorbent）, taken in different time
Sample, with concentration of metal ions, adsorption rate, up to 98% in ICP-OES measurement stripping liquids.After desorption terminates, adsorbent uses Magneto separate
Reclaim, dried after being washed to weakly acidic pH, you can recycle.
Embodiment 3
（1）Nanometer Fe3O4The preparation of cluster：By FeCl3 .6H2O：Sodium acetate：The mass ratio of polyethylene glycol is 3.2： 7.8：2.5,
Take FeCl3 .6H2O, sodium acetate and polyethylene glycol, then it is calculated as 13.5 by the mass volume ratio g/mL of above-mentioned three and ethylene glycol：
500, by FeCl3 .6H2O, sodium acetate and polyethylene glycol are added in ethylene glycol, and magnetic agitation is allowed to dissolve, the homogeneous Huang that will be obtained
Mixture of colours solution is sealed in being transferred to polytetrafluoro hydrothermal reaction kettle, and 1h is reacted at being heated to 250 DEG C, after naturally cool to room temperature,
Black particle thing is obtained, is washed for several times with ethanol, then carry out freeze-drying or vacuum drying, that is, obtain nanometer Fe3O4Cluster；
（2）Core shell structure Fe3O4@nSiO2The preparation of carrier：By step（1）Gained nanometer Fe3O4The cluster salt of 0.1mol/L
The ultrasonically treated 20min of acid solution, then alternately washed for several times, then by nanometer Fe with ethanol and deionized water3O4Cluster and hydrolyzate
Solid-to-liquid ratio g/mL be calculated as 0.15:100, by the nanometer Fe after washing3O4Cluster is distributed in hydrolyzate, then is slowly added dropwise positive silicon
100mmol/L containing silicon ion in acid butyl ester to system, and 72h is stirred, it is scrubbed, obtain core shell structure Fe3O4@nSiO2Carrier；
The hydrolyzate is made up of the component of following parts by volume：85 parts of ethanol, 25 parts of deionized water, concentration are the ammoniacal liquor 1.5 of 28wt%
Part；
（3）The preparation of function monomer-template molecule host-guest coordination compound：By the functional polyorganosiloxane monomer and gold or silver of band functional group
The mol ratio of ion is 1：1.5, by SH-CH2CH2-NHCH2CH2CH2Si(OMe)3Mix with target gold ion solution, obtain work(
Can monomer-template molecule host-guest coordination compound；Wherein, target gold ion solution is the solution containing gold ion 2mol/L；
（4）The preparation of polymer matrix：By core shell structure Fe3O4@nSiO2The ratio g/mmol of carrier and complex is calculated as 0.15:
0.25, by step（3）Gained function monomer-template molecule host-guest coordination compound and step（2）Gained core shell structure Fe3O4@
nSiO2Support dispersion is in condensation liquid, then is added dropwise in the butyl silicate of 0.5 mass parts to system in stirring, and stirs
72h, it is scrubbed to obtain polymer matrix；The condensation liquid includes the component of following parts by volume：65 parts of ethanol, deionized water 85
Part, concentration are 1.5 parts of the ammoniacal liquor of 28wt%, and the CTAB of 0.4 mass parts are added in liquid mixed above；
（5）By acetone extraction method removing step（4）CTAB in resulting polymers parent, leaves orderly on polymer matrix
Mesoporous, the tricaprylmethyl ammonium salt using concentration as 2mol/L carries out back extraction and removes gold ion as the eluant, eluent of target gold ion,
The micropore mutually matched with target gold ion space structure and action site is left, that is, obtains that the sandwich structure of gold can be separated
Magnetic mesoporous imprinted material IIP-Fe3O4@nSiO2@mSiO2。
The magnetic mesoporous imprinted material of sandwich structure that gained can separate gold can realize target metal ions from liquid to be adsorbed
In efficiently separate, be specifically added to imprinted material as adsorbent in the liquid to be adsorbed containing target gold ion（It is to be adsorbed
Gold ion concentration in liquid is 100mmol/L）, absorption 10min or so, measure golden in liquid to be adsorbed before and after adsorbing with ICP-OES
Belong to the concentration of ion, calculate adsorption rate, up to 96%.
The adsorbent for terminating is adsorbed to be reclaimed using Magneto separate, and the washing that adds water is subsequently adding complexing agent or acid to weakly acidic pH
Solution carries out desorption gold as stripping liquid（Stripping liquid is consistent with the eluant, eluent used when synthesizing the adsorbent）, taken in different time
Sample, with concentration of metal ions, adsorption rate, up to 97% in ICP-OES measurement stripping liquids.After desorption terminates, adsorbent uses Magneto separate
Reclaim, dried after being washed to weakly acidic pH, you can recycle.
Claims (9)
1. a kind of energy separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver, it is characterised in that including such as
Lower step：
（1）Nanometer Fe3O4The preparation of cluster：By FeCl3 .6H2O：Sodium acetate：The mass ratio of polyethylene glycol is（2.2~3.2）：
（6.5~7.8）：（1.5~2.5）, take FeCl3 .6H2O, sodium acetate and polyethylene glycol, then by above-mentioned three and the quality of ethylene glycol
Volume ratio g/mL is calculated as（10.2~13.5）：（5~500）, by FeCl3 .6H2O, sodium acetate and polyethylene glycol are added in ethylene glycol,
Magnetic agitation is allowed to dissolve, the mixed solution sealing that will be obtained, and 6~72h is reacted at being heated to 160~250 DEG C, treats natural cooling
To room temperature, black particle thing is obtained, washed for several times with ethanol, then carry out freeze-drying or vacuum drying, that is, obtain nanometer Fe3O4
Cluster；
（2）Core shell structure Fe3O4@nSiO2The preparation of carrier：By step（1）Gained nanometer Fe3O4The cluster hydrochloric acid of 0.1mol/L
Ultrasonically treated 5~the 20min of solution, then alternately washed for several times, then by nanometer Fe with ethanol and deionized water3O4Cluster and hydrolysis
The solid-to-liquid ratio g/mL of liquid is calculated as（0.05~0.15）:（90~100）, by the nanometer Fe after washing3O4Cluster is distributed to hydrolyzate
In, then 1~100mmol/L containing silicon ion in silicon source to system is slowly added dropwise, and 1~72h is stirred, it is scrubbed, obtain nucleocapsid knot
Structure Fe3O4@nSiO2Carrier；
（3）The preparation of function monomer-template molecule host-guest coordination compound：By the functional polyorganosiloxane monomer and gold or silver of band functional group
The mol ratio of ion is 1：（1.2~1.5）, the functional polyorganosiloxane monomer of band functional group is mixed with target gold or silver ion solution
Close, obtain function monomer-template molecule host-guest coordination compound；
The functional polyorganosiloxane monomer with functional group is F-CH2CH2-NHCH2CH2CH2Si(OMe)3；
（4）The preparation of polymer matrix：By core shell structure Fe3O4@nSiO2The ratio g/mmol of carrier and complex is calculated as（0.05~
0.15）:（0.15~0.25）, by step（3）Gained function monomer-template molecule host-guest coordination compound and step（2）Gained core
Shell structure Fe3O4@nSiO2Support dispersion is in condensation liquid, then the silicon source of 0.3~0.5 mass parts to system is added dropwise in stirring
In, and 1~72h is stirred, it is scrubbed to obtain polymer matrix；
（5）By acetone extraction method removing step（4）CTAB in resulting polymers parent, using complexing agent or acid solution as washing
De- agent carries out back extraction and removes gold or silver ion, that is, obtain that the magnetic mesoporous imprinted material of sandwich structure of gold or silver can be separated.
2. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：It is pure that the polyethylene glycol, ethylene glycol and ethanol are analysis purchased in market.
3. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：The step（2）With（4）Silicon source be tetraethyl orthosilicate, methyl silicate, butyl silicate, positive silicic acid third
Ester or other silicate class, are analysis purchased in market pure.
4. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：The step（2）Hydrolyzate be made up of the component of following parts by volume：75~85 parts of ethanol, deionized water 15
~25 parts, 0.5~1.5 part of the ammoniacal liquor that concentration is 28wt%.
5. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：The F is-COOH ,-NH2,-POOH or-SH.
6. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：The step（3）Target gold or silver ion solution be contain target gold or the mol/L of silver ion 0.1~2
Solution.
7. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：The step（4）Condensation liquid including following parts by volume component：55~65 parts of ethanol, deionized water 75~
85 parts, 0.5~1.5 part of the ammoniacal liquor that concentration is 28wt%, and the CTAB of 0.1~0.4 mass parts is added in liquid mixed above.
8. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：The step（5）Complexing agent be thiocarbamide, cyanide, ethyl acetate, methyl that concentration is 0.1~2mol/L
Isobutyl ketone, tri octyl phosphine type oxide, tricaprylmethyl ammonium salt, dibutyl carbitol (DBC) or tributyl phosphate.
9. energy according to claim 1 separates the preparation method of the magnetic mesoporous imprinted material of sandwich structure of gold or silver,
It is characterized in that：The step（5）Acid solution be nitric acid and/or hydrochloric acid solution that concentration is 0.1~2mol/L.
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Application publication date: 20170620 |