CN109485052A - A kind of preparation method of macropore superparamagnetism array type earth silicon material - Google Patents
A kind of preparation method of macropore superparamagnetism array type earth silicon material Download PDFInfo
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- 239000002210 silicon-based material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims abstract description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004816 latex Substances 0.000 claims abstract description 7
- 229920000126 latex Polymers 0.000 claims abstract description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 6
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 5
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229940056319 ferrosoferric oxide Drugs 0.000 claims abstract description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 claims description 9
- 238000005457 optimization Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 4
- 239000012074 organic phase Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 claims description 3
- 229960003656 ricinoleic acid Drugs 0.000 claims description 3
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 2
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 238000010557 suspension polymerization reaction Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 239000011148 porous material Substances 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000005815 base catalysis Methods 0.000 abstract description 2
- 230000008878 coupling Effects 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000004088 foaming agent Substances 0.000 abstract 1
- 239000000725 suspension Substances 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 238000000034 method Methods 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- 238000007445 Chromatographic isolation Methods 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 230000000699 topical effect Effects 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of preparation methods of macropore superparamagnetism array type earth silicon material, belong to field of material technology.The preparation method is to be co-precipitated that nanoscale, superparamagnetic ferroso-ferric oxide is made under base catalysis by ferric trichloride and ferrous chloride, then again using it as magnetic core, microemulsion suspension polymerisation is carried out with styrene, divinylbenzene, prepare the superparamagnetism latex of favorable dispersibility, secondly tetraethyl orthosilicate is hydrolyzed in water/Alcohol system, surface cure is carried out by base unit of the latex, array is finally hydrolyzed by tetraethyl orthosilicate under Magnetic guidance coupling, prepares material body by pore-foaming agent of n-hexane.The result shows that being in the array structure and even pore distribution along magnetic direction to the material that upper type is prepared, pressure drop is small, is a kind of good separation material.
Description
Technical field
The invention belongs to field of material technology, design and close in particular to a kind of large pore material that compound with regular structure is unified
At in particular to a kind of new method of macropore superparamagnetism array type earth silicon material preparation.
Background technique
Large pore material is since it is with biggish reference area, excellent liquid communication and the extensive use of strong mass-transfer performance
In fields such as Industrial Catalysis, chromatographic isolation, membrane technology, organizational projects.Sound construction is prepared, hole path is uniformly dredged, material
The large pore material of high surface activity is always the hot spot in application material field.
In general, can using tetraethyl orthosilicate acid or base catalysis under hydrolysis prepare nanometer grade silica material come,
Or it is compound as silicon dioxide composite material with other nonmetallic materials, since silica has extremely strong attractability of metal
And its surface is rich in silicone hydroxyl, can be carried out grafting processing, so being a kind of good separation material skeleton.However, this side
The earth silicon material shape size that formula prepares is irregular, and build stack is at random unordered, and distribution of pores is uneven.Its disadvantage
It is: is carrying out among mass transport process, it is uneven to go out pressure drop distribution, local collapse.In addition, this traditional silicon dioxide material hole
Gap and specific surface area are relatively little, significantly limit its service performance.
In order to make up the disadvantage in composite silicon dioxide materials process made above, the present invention devises a kind of novel preparation
Method, to prepare high efficiency macropore superparamagnetism array type earth silicon material.The key point of the preparation method is: in original
On the basis of having composite silicon dioxide materials synthesis, superparamagnetic iron oxide is firstly introduced into as magnetic core, passes through magnetic coupling pole-coupling
It is the array type skeleton structure along magnetic induction line direction that pole, which acts on directional array in magnetic field,.Based on this thinking, we pass through four
Step has synthesized macropore superparamagnetism array type earth silicon material.Development process is as follows: (1) it is suitable to prepare excess of export by coprecipitation
Magnetic ferroferric oxide；(2) the uniform Magnetic adhesive of dispersibility is prepared by styrene-divinylbenzene microemulsion suspension polymerization
Cream；(3) hydrolysis precipitation under tetraethyl orthosilicate solutions of weak acidity；(4) n-hexane dispersion pore and magnetic array process.
Summary of the invention
It is an object of the invention to be directed to the deficiency of conventional composite type earth silicon material, a kind of macropore superparamagnetism is provided
The preparation method of array type earth silicon material.Earth silicon material compound with regular structure that the method for the invention is prepared is unified,
Porosity distribution uniformly, large specific surface area the characteristics of, to realize that separation process pressure drop is uniform,.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of preparation method for the affinity chromatographic column that aglucon is reversibly modified, specifically comprises the following steps:
(1) it disperses ferrous chloride and ferric trichloride in 150ml deionized water, oil bath is warming up to 75-80 DEG C, in mechanical stirring
Lower 25% concentration ammonium hydroxide of dropwise addition 30ml cures 30 minutes, prepares the superparamagnetic iron oxide of partial size 7-15nm;
(2) it weighs and is walking gained nanometer superparamagnetic iron oxide, 5g styrene, 0.35g divinylbenzene, 0.12g on 2.5g just
Hexadecane, 0.01g AIBN are prepared into organic phase A；0.5g neopelex is weighed again is scattered in 50ml deionized water
In, dispersion obtains dispersed phase B；Mix A and B, 30 minutes formation microemulsions of ice-water bath ultrasonic disperse under mechanical stirring, then oil bath
60-80 DEG C reaction 4-6 hours, prepare superparamagnetism latex；
(3) it disperses 0.34g polyethylene glycol (600) in 5.5ml 1M glacial acetic acid solution, 0 DEG C of ice salt bath control system temperature,
1ml tetraethyl orthosilicate is added dropwise under mechanical stirring, 0.5 ml latex is added after hydrolyzing 30min, is vigorously stirred 2min formation table
Face cured layer；
(4) by the transfer of system obtained by upper step magnetic field, 0.5ml n-hexane is added, controls magnetic field strength 0.1-20mT, system temperature
0-60 DEG C, the reaction time 12 hours, obtain array backbone；
In the above-mentioned technical solutions, the magnetic core is nanoscale, superparamagnetic ferroso-ferric oxide, but is not limited only to this one kind.
In above-mentioned technical proposal, ricinoleic acid is added as superparamagnetic iron oxide surface in step (1) reaction optimization
Dispersing agent.
In above-mentioned technical proposal, step (2) reaction optimization temperature is 75 DEG C, and the optimization time is 6 hours.
In above-mentioned technical proposal, step (3) reaction system optimization is water/ethanol system, and hydrolyst is ammonium hydroxide.
In above-mentioned technical proposal, step (4) array process magnetic field strength is 20mT, and array temperature is 45 DEG C.
Compared with prior art, the present invention having the advantage that
(1) process of the present invention unit operation maturation, raw material are industrialization product, are easy to carry out industrialized production.
(2) present invention can adjust array structure skeleton length according to magnitude of field intensity, prepare the material of corresponding size.
(3) present invention can carry out grafting processing to silica surface, widen application range according to separation absorption demand.
(4) present invention has array structure, and separation process pressure drop is uniform.
(5) present invention has macroporous structure, separates large specific surface area.
Detailed description of the invention
Fig. 1 is the infrared transformation picture of 1 product Fourier of embodiment of the present invention.
Fig. 2 is 1 Product scan electron microscopic picture of embodiment of the present invention.
Specific embodiment
For a better understanding of the present invention, the present invention is further explained below in conjunction with embodiment and attached drawing.But
It should be strongly noted that embodiment is only used for that the present invention is further expalined, the scope of protection of present invention is simultaneously
It is not limited to the range of embodiment expression.
Embodiment 1
It takes 16.2g Iron(III) chloride hexahydrate, 5.9g tetra- to be hydrated ferrous chloride to be dissolved in 180ml deionized water, nitrogen purge gas 30
75 DEG C are warming up to after minute, 8.44g ricinoleic acid and 4.5g acetone blended liquid, mechanical stirring 10 are added under mechanical stirring
25% concentration ammonium hydroxide of 30ml is added dropwise after minute, Magneto separate obtains superparamagnetic iron oxide nano particle after curing 30 minutes.It takes
Step gained magnetic-particle, is added 7.98g styrene, 0.42g divinylbenzene, 9g ether, 0.25g n-hexane, 0.01gAIBN on 8g
It is prepared into organic phase A, takes 0.5g dodecyl sodium sulfate to be dissolved in 48ml deionized water and is prepared into dispersed phase B, ice salt bath machinery stirs
Mix it is lower A is added B, after ultrasonic 30 minutes formation microemulsions, oil bath is warming up to 75 DEG C, polymerization reaction 6 hours.The poly- second two of 0.34g
Alcohol (600) is dissolved in 5.5ml 1M glacial acetic acid, and 1ml TMOS hydrolysis is added at 0 DEG C, under mechanical stirring for ice-water bath control system temperature
It 30 minutes, adds and walks magnetic latex prepared by polymerization reaction and 0.5ml n-hexane on 0.3ml, put after being vigorously stirred 2 minutes
Enter in magnetic field, control temperature 45 C, array time 12 hours.3 times are embathed with 100ml ethyl alcohol again after Magneto separate, 24 hours every time,
Last cold take out 24 hours is prepared into finished product.
By the infrared transformation map (Fig. 1) of Fourier, 594 cm-1Place is the Fe-O stretching vibration of ferroso-ferric oxide, 696cm-1
For phenyl ring absorption peak, 1090cm-1It is the antisymmetric stretching vibration of Si-O-Si, 806cm-1It is the symmetrical stretching vibration of Si-O-Si.
The scanning electron microscopic picture of Fig. 2 macropore superparamagnetism array type earth silicon material, as seen from Figure 2, the linear battle array of the structure
Column type structure, and runner is evenly distributed, it is irregular to avoid stacked silicon materials Topical Dispersion, the non-uniform situation of pressure drop.
Embodiment 2
Firstly, 1.36g Iron(III) chloride hexahydrate is dissolved in 40ml ethylene glycol under mechanical stirring, 3.6g sodium acetate, 1mlPEG is added,
It is prepared within strength mechanical stirring 1 hour rufous clear solution, then upper step acquired solution is transferred to 100ml band polytetrafluoroethylene (PTFE)
The autoclave of liner, 210 DEG C are reacted 8 hours.After being cooled to room temperature, Magneto separate is carried out, dehydrated alcohol elutes three times, then by gained
Superparamagnetic iron oxide be scattered in 10ml dehydrated alcohol, then by step (2), to obtain macropore super suitable for (3) (4) reaction
Magnetic array type earth silicon material.
Claims (6)
1. a kind of preparation method of macropore superparamagnetism array type earth silicon material, it is characterised in that include the following steps:
(1) it disperses ferrous chloride and ferric trichloride in 150ml deionized water, oil bath is warming up to 75-80 DEG C, in mechanical stirring
Lower 25% concentration ammonium hydroxide of dropwise addition 30ml cures 30 minutes, prepares the superparamagnetic iron oxide of partial size 7-15nm;
(2) it weighs and is walking gained nanometer superparamagnetic iron oxide, 5g styrene, 0.35g divinylbenzene, 0.12g on 2.5g just
Hexadecane, 0.01g AIBN are prepared into organic phase A；0.5g neopelex is weighed again is scattered in 50ml deionized water
In, dispersion obtains dispersed phase B；Mix A and B, 30 minutes formation microemulsions of ice-water bath ultrasonic disperse under mechanical stirring, then oil bath
60-80 DEG C reaction 4-6 hours, prepare superparamagnetism latex；
(3) it disperses 0.34g polyethylene glycol (600) in 5.5ml 1M glacial acetic acid solution, 0 DEG C of ice salt bath control system temperature,
1ml tetraethyl orthosilicate is added dropwise under mechanical stirring, 0.5 ml latex is added after hydrolyzing 30min, is vigorously stirred 2min formation table
Face cured layer；
(4) by the transfer of system obtained by upper step magnetic field, 0.5ml n-hexane is added, controls magnetic field strength 0.1-50mT, system temperature
0-60 DEG C, the reaction time 12 hours, obtain array backbone.
2. a kind of preparation method of macropore superparamagnetism array type earth silicon material according to claim 1, feature
It is that magnetic core used is nanoscale, superparamagnetic ferroso-ferric oxide, but is not limited only to this one kind.
3. a kind of preparation method of macropore superparamagnetism array type earth silicon material according to claim 1, feature
It is that step (1) reaction process optimization technique is that ricinoleic acid is added in ferric trichloride and ferrous chloride solution system, helps
In the polymerization reaction of magnetic core and organic phase in subsequent microemulsion suspension polymerization.
4. a kind of preparation method of macropore superparamagnetism array type earth silicon material according to claim 1, feature
It is that the reaction time is optimized for 6 hours in step (2), 75 DEG C of reaction temperature.
5. a kind of preparation method of macropore superparamagnetism array type earth silicon material according to claim 1, feature
It is that step (3) reaction system can be ethanol/water system, ammonium hydroxide is hydrolyst.
6. a kind of preparation method of macropore superparamagnetism array type earth silicon material according to claim 1, feature
The magnetic field strength optimization range for being step (4) is 20mT, and temperature optimization range is 45 DEG C.
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2018
- 2018-09-20 CN CN201811097117.0A patent/CN109485052A/en active Pending
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