CN103745794A - Step-by-step-prepared magnetic liquid with magnetic nanoparticles wrapped by polyaniline derivatives - Google Patents
Step-by-step-prepared magnetic liquid with magnetic nanoparticles wrapped by polyaniline derivatives Download PDFInfo
- Publication number
- CN103745794A CN103745794A CN201410016751.2A CN201410016751A CN103745794A CN 103745794 A CN103745794 A CN 103745794A CN 201410016751 A CN201410016751 A CN 201410016751A CN 103745794 A CN103745794 A CN 103745794A
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- CN
- China
- Prior art keywords
- magnetic
- magnetic liquid
- liquid
- particle
- polyaniline derivative
- Prior art date
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- 239000007788 liquid Substances 0.000 title claims abstract description 52
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 30
- 239000002122 magnetic nanoparticle Substances 0.000 title abstract description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- RWZYAGGXGHYGMB-UHFFFAOYSA-N anthranilic acid Chemical compound NC1=CC=CC=C1C(O)=O RWZYAGGXGHYGMB-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011246 composite particle Substances 0.000 claims abstract description 12
- 239000006249 magnetic particle Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000013049 sediment Substances 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 3
- -1 DBSA Chemical compound 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000178 monomer Substances 0.000 abstract description 4
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract 5
- 239000002105 nanoparticle Substances 0.000 abstract 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 abstract 1
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 239000002322 conducting polymer Substances 0.000 description 3
- 229920001940 conductive polymer Polymers 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Landscapes
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention provides a method for preparing magnetic liquid with magnetic nanoparticles wrapped by polyaniline derivatives step by step. According to the method, in a dispersion environment of Massart magnetic liquid, o-aminobenzoic acid and aniline monomers are polymerized by the in-situ polymerization method to achieve the effect that the polyaniline derivatives are tightly wrapped on Fe3O4 (ferroferric oxide) nanoparticles in the Massart magnetic liquid in a chemical bond mode. The method specifically includes preparing the Massart magnetic liquid, modifying the surfaces of the Fe3O4 nanoparticles by the o-aminobenzoic acid, adding the aniline monomers to polymerize the aniline monomers and the o-aminobenzoic acid to form the polyaniline derivatives, and connecting dodecylbenzene sulfonic acid, which stably disperses in nonpolar-group carrier liquid according to alkane nonpolar features, to the surfaces of Fe3O4/polyaniline derivative composite particles to obtain the magnetic liquid with the Fe3O4 magnetic nanoparticles wrapped by the polyaniline derivatives. Under the action of a regularly-changed magnetic field, the magnetic liquid is also regularly changed in terms of photoelectric property, in other words, the objective of controllably adjusting performance indexes of the photoelectric property of the magnetic liquid can be finally achieved through adjustment of the magnetic field strength. A novel small branch available for research is developed in the field of research on the magnetic liquid, and the method has significant research and application value.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic liquid of conducting polymer parcel nano magnetic particle, relate in particular to the preparation method that polyaniline derivative parcel nano magnetic particle magnetic liquid is prepared in a kind of substep assembling.
Technical background
Magnetic liquid refers to nano magnetic particle highly dispersed that size magnitude is less than single magnetic domain in liquid base load liquid and the colloidal solution of a kind of high stability forming, the dispersant of general magnetic liquid is organic polymer chain, do not possess special performance, once and superscribe after one deck organic semiconductor at original nano magnetic particle and dispersant joining place in magnetic liquid, a kind of novel organic inorganic hybridization magnetic liquid just arises at the historic moment, organic semiconductor is by after organically combining with magnetic liquid, organic semi-conductor performance just can change by regulating magnetic field intensity to make magnetic liquid possess regular photoelectric properties, therefore such Magnetic Fluids has great potential in the application in the fields such as micro-optic device and photonic crystal.
But the preparation of this class magnetic liquid need to overcome three difficult points: the one, and the stability of conducting polymer coated magnetic nano particle; The 2nd, the size magnitude control of conducting polymer integument; The 3rd, how stable dispersion is in base load liquid for the nano magnetic particle after parcel.The present invention, just based on overcoming above three difficult points, is prepared into polyaniline derivative parcel Fe
3o
4magnetic-particle magnetic liquid.
Summary of the invention
The object of this invention is to provide a kind of substep assembling and prepare the preparation method of polyaniline derivative parcel nano magnetic particle magnetic liquid, its magnetic-particle surface of magnetic liquid existing is at present all common organic long-chain molecules.Except the essential characteristic that some magnetic liquids possess, there is no other unique features.The present invention uses the magnetic liquid of substep assembling preparation by polyaniline derivative parcel nano magnetic particle, and its preparation method is:
(1) preparation process:
A, by the Fe (NO configuring
3)
39H
2o solution and FeSO
47H
2o solution is poured in there-necked flask, mixes the rear ammoniacal liquor that adds fast, rapid stirring, and then magnetic separates, then washs to PH=7.0 with deionized water, outwells supernatant and stays sediment, by the Fe (NO configuring
3)
39H
2o solution is poured in above-mentioned sediment and is seethed with excitement and stop for 30 minutes, and it is cooling that magnetic is separated to nature, outwells supernatant liquor, uses acetone and deionized water cyclic washing until neutrality is placed in vacuumize ware and is dried after sediment filtration, then pulverizes, and obtains nanometer Fe
3o
4particle.
B, get above-mentioned nanometer Fe
3o
4particle, acid adding is configured to Massart magnetic liquid, places slaking two time-of-weeks.
C, aniline, ortho-aminobenzoic acid are added to the Massart magnetic liquid that slaking is good, then add purify the to obtain Fe of polyaniline derivative parcel of the hydrochloric acid stirring reaction 6 hours that is dissolved with ammonium persulfate, product removal of impurities
3o
4/ polyaniline derivative composite particles.
D, by Fe
3o
4/ polyaniline derivative composite particles adds in the nonpolar group carrier fluid that is dissolved with DBSA mechanical agitation 6 hours, then within centrifugal 5 minutes, gets supernatant liquid, is polyaniline derivative parcel Fe
3o
4magnetic-particle magnetic liquid.
(2) mol ratio of nine described water ferric nitrates, ferrous sulfate heptahydrate, ammoniacal liquor, nitric acid, ortho-aminobenzoic acid, hydrochloric acid, aniline, ammonium persulfate, DBSA, absolute ethyl alcohol is followed successively by: 10 ~ 12.7:2:5:18.75:1:10:0.74:2:0.69:1.
Beneficial effect of the present invention: the present invention is by first preparing Massart magnetic liquid, home position polymerization reaction becomes after polyaniline derivative ortho-aminobenzoic acid, aniline polymerization to reach by chemical bond and be firmly wrapped in the effect on magnetic nanoparticle again, by mathematical computations aniline monomer quantity, accurately control consumption, prevent that aniline polymerization degree from exceeding the size magnitude that magnetic liquid can carry, thereby reach, control Fe
3o
4the effect of/polyaniline derivative composite particles particle diameter; Adopt DBSA to increase its close nonpolar group carrier fluid as surfactant and dopant.Thereby acquisition magnetic liquid.
Embodiment
embodiment 1:
A, by the 250ml Fe (NO configuring
3)
39H
2o (31.32g) solution and 250ml FeSO
47H
2o (12.24g) solution is poured in there-necked flask and is added fast 50ml concentrated ammonia liquor (25-28%) after dissolving, rapid stirring, then magnetic separates, then washs to PH=7.0 with deionized water, outwell supernatant and stay sediment, by the 500ml Fe (NO configuring
3)
39H
2o (57.91g) solution is poured in the above-mentioned sediment having washed and is seethed with excitement and stop for 30 minutes, and it is cooling that magnetic is separated to nature, outwells supernatant liquor, with acetone and deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverize, obtain nanometer Fe
3o
4particle.
B, get above-mentioned nanometer Fe
3o
4particle 5g, adds 94.47ml nitric acid (0.91 mol.L
-1) be configured to the Massart magnetic liquid of 1% volume fraction, place slaking two time-of-weeks.
C, 1.5ml aniline, 3g ortho-aminobenzoic acid are added to the Massart magnetic liquid that slaking is good, then add 200ml hydrochloric acid (0.1 mol.L that is dissolved with 10g ammonium persulfate
-1) in stirring reaction 6 hours, purify the to obtain Fe3O4/ polyaniline derivative composite particles of polyaniline derivative parcel of product removal of impurities.
D, composite particles is added in the 30ml ethyl acetate that is dissolved with 6ml DBSA to mechanical agitation 6 hours, then within centrifugal 5 minutes, get upper strata liquid and be polyaniline derivative parcel Fe
3o
4magnetic-particle magnetic liquid.
embodiment 2:
A, by the 250ml Fe (NO configuring
3)
39H
2o (31.32g) solution and 250ml FeSO
47H
2o (12.24g) solution is poured in there-necked flask and is added fast 50ml concentrated ammonia liquor (25-28%) after dissolving, rapid stirring, then magnetic separates, then washs to PH=7.0 with deionized water, outwell supernatant and stay sediment, by the 500ml Fe (NO configuring
3)
39H
2o (82.02g) solution is poured in the above-mentioned sediment having washed and is seethed with excitement and stop for 30 minutes, and it is cooling that magnetic is separated to nature, outwells supernatant liquor, with acetone and deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverize, obtain nanometer Fe
3o
4particle.
B, get above-mentioned nanometer Fe
3o
4particle 5g, adds 94.47ml nitric acid (0.91 mol.L
-1) be configured to the Massart magnetic liquid of 1% volume fraction, place slaking two time-of-weeks.
C, 1.5ml aniline, 3g ortho-aminobenzoic acid are added to the Massart magnetic liquid that slaking is good, then add 200ml hydrochloric acid (0.1 mol.L that is dissolved with 10g ammonium persulfate
-1) in stirring reaction 6 hours, purify the to obtain Fe3O4/ polyaniline derivative composite particles of polyaniline derivative parcel of product removal of impurities.
D, composite particles is added in the 30ml ethyl acetate that is dissolved with 6ml DBSA to mechanical agitation 6 hours, then within centrifugal 5 minutes, get upper strata liquid and be polyaniline derivative parcel Fe
3o
4magnetic-particle magnetic liquid.
embodiment 3:
A, by the 250ml Fe (NO configuring
3)
39H
2o (31.32g) solution and 250ml FeSO
47H
2o (12.24g) solution is poured in there-necked flask and is added fast 50ml concentrated ammonia liquor (25-28%) after dissolving, rapid stirring, then magnetic separates, then washs to PH=7.0 with deionized water, outwell supernatant and stay sediment, by the 500ml Fe (NO configuring
3)
39H
2o (57.91g) solution is poured in the above-mentioned sediment having washed and is seethed with excitement and stop for 30 minutes, and it is cooling that magnetic is separated to nature, outwells supernatant liquor, with acetone and deionized water cyclic washing until neutrality, natural drying in vacuumize ware, pulverize, obtain nanometer Fe
3o
4particle.
B, get above-mentioned nanometer Fe
3o
4particle 5g, adds 94.47ml nitric acid (0.91 mol.L
-1) be configured to the Massart magnetic liquid of 1% volume fraction, place slaking two time-of-weeks.
C, 1.5ml aniline, 3g ortho-aminobenzoic acid are added to the Massart magnetic liquid that slaking is good, then add 200ml hydrochloric acid (0.1 mol.L that is dissolved with 10g ammonium persulfate
-1) in stirring reaction 6 hours, purify the to obtain Fe3O4/ polyaniline derivative composite particles of polyaniline derivative parcel of product removal of impurities.
D, composite particles is added in the 35ml ethyl acetate that is dissolved with 6ml DBSA to mechanical agitation 6 hours, then within centrifugal 5 minutes, get upper strata liquid and be polyaniline derivative parcel Fe
3o
4magnetic-particle magnetic liquid.
Claims (1)
1. a magnetic liquid for polyaniline derivative parcel nano magnetic particle is prepared in substep assembling, it is characterized in that:
(1) preparation process:
A, by the Fe (NO configuring
3)
39H
2o solution and FeSO
47H
2o solution is poured in there-necked flask, mixes the rear ammoniacal liquor that adds fast, rapid stirring, and then magnetic separates, then washs to PH=7.0 with deionized water, outwells supernatant and stays sediment, by the Fe (NO configuring
3)
39H
2o solution is poured in above-mentioned sediment and is seethed with excitement and stop for 30 minutes, and it is cooling that magnetic is separated to nature, outwells supernatant liquor, uses acetone and deionized water cyclic washing until neutrality is placed in vacuumize ware and is dried after sediment filtration, then pulverizes, and obtains nanometer Fe
3o
4particle;
B, get above-mentioned nanometer Fe
3o
4particle, acid adding is configured to Massart magnetic liquid, places slaking two time-of-weeks;
C, aniline, ortho-aminobenzoic acid are added to the Massart magnetic liquid that slaking is good, then add purify the to obtain Fe of polyaniline derivative parcel of the hydrochloric acid stirring reaction 6 hours that is dissolved with ammonium persulfate, product removal of impurities
3o
4/ polyaniline derivative composite particles;
D, by Fe
3o
4/ polyaniline derivative composite particles adds in the nonpolar group carrier fluid that is dissolved with DBSA mechanical agitation 6 hours, then within centrifugal 5 minutes, gets supernatant liquid, is polyaniline derivative parcel Fe
3o
4magnetic-particle magnetic liquid;
(2) mol ratio of nine described water ferric nitrates, ferrous sulfate heptahydrate, ammoniacal liquor, nitric acid, ortho-aminobenzoic acid, hydrochloric acid, aniline, ammonium persulfate, DBSA, absolute ethyl alcohol is followed successively by: 10 ~ 12.7:2:5:18.75:1:10:0.74:2:0.69:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410016751.2A CN103745794B (en) | 2014-01-15 | 2014-01-15 | The magnetic liquid of polyaniline derivative parcel nano magnetic particle is prepared in a kind of substep assembling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410016751.2A CN103745794B (en) | 2014-01-15 | 2014-01-15 | The magnetic liquid of polyaniline derivative parcel nano magnetic particle is prepared in a kind of substep assembling |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103745794A true CN103745794A (en) | 2014-04-23 |
| CN103745794B CN103745794B (en) | 2016-05-25 |
Family
ID=50502807
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410016751.2A Expired - Fee Related CN103745794B (en) | 2014-01-15 | 2014-01-15 | The magnetic liquid of polyaniline derivative parcel nano magnetic particle is prepared in a kind of substep assembling |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103745794B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111063500A (en) * | 2020-01-10 | 2020-04-24 | 中山大学 | Modified magnetic nano-particles, non-polar solvent-based magnetic liquid, preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012009128A2 (en) * | 2010-06-28 | 2012-01-19 | Baker Hughes Incorporated | Nanofluids and methods of use for drilling and completion fluids |
| CN102360676A (en) * | 2011-09-29 | 2012-02-22 | 南昌航空大学 | Method for preparing magneto conducting magnetic fluid |
-
2014
- 2014-01-15 CN CN201410016751.2A patent/CN103745794B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012009128A2 (en) * | 2010-06-28 | 2012-01-19 | Baker Hughes Incorporated | Nanofluids and methods of use for drilling and completion fluids |
| CN102360676A (en) * | 2011-09-29 | 2012-02-22 | 南昌航空大学 | Method for preparing magneto conducting magnetic fluid |
Non-Patent Citations (2)
| Title |
|---|
| DANMING CHAO: "Anthranilic Acid Assisted Preparation of Fe3O4–Poly(aniline-co-o-anthranilic acid) Nanoparticles", 《JOURNAL OF APPLIED POLYMER SCIENCE》, vol. 102, 31 December 2006 (2006-12-31), pages 1666 - 1671 * |
| 王安蓉: "水基Fe3O4 离子型磁性液体的制备与磁性", 《西南师范大学学报(自然科学版)》, vol. 31, no. 5, 31 October 2006 (2006-10-31) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111063500A (en) * | 2020-01-10 | 2020-04-24 | 中山大学 | Modified magnetic nano-particles, non-polar solvent-based magnetic liquid, preparation method and application |
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| Publication number | Publication date |
|---|---|
| CN103745794B (en) | 2016-05-25 |
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