CN108328661A - One step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method - Google Patents
One step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method Download PDFInfo
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- CN108328661A CN108328661A CN201810427316.7A CN201810427316A CN108328661A CN 108328661 A CN108328661 A CN 108328661A CN 201810427316 A CN201810427316 A CN 201810427316A CN 108328661 A CN108328661 A CN 108328661A
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- Prior art keywords
- polyacrylic acid
- diethylene glycol
- ferric oxide
- sodium hydroxide
- oxide nano
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Links
- 229920002125 Sokalan® Polymers 0.000 title claims abstract description 37
- 239000004584 polyacrylic acid Substances 0.000 title claims abstract description 37
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical class O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 31
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 112
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 18
- 239000012498 ultrapure water Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 150000001805 chlorine compounds Chemical class 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 abstract description 22
- 239000002245 particle Substances 0.000 abstract description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 14
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000012930 cell culture fluid Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000002296 dynamic light scattering Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- -1 biology Sensor Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000012631 diagnostic technique Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940031182 nanoparticles iron oxide Drugs 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 239000001974 tryptic soy broth Substances 0.000 description 1
- 108010050327 trypticase-soy broth Proteins 0.000 description 1
Classifications
-
- 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a step high temperature method and prepares polyacrylic acid modified ferric oxide nano particl method, includes the following steps：Sodium hydroxide is dissolved in diethylene glycol (DEG), under nitrogen protection, 110 ~ 130 DEG C is heated to, after keeping the temperature 1 ~ 3h, is cooled to 65 ~ 75 DEG C, obtains sodium hydroxide/diethylene glycol solution；Iron trichloride hexahydrate, four water frerrous chlorides, polyacrylic acid and diethylene glycol (DEG) are mixed, under nitrogen protection, are heated to 210 ~ 230 DEG C; keep the temperature 0.5 ~ 1.5 h; reaction solution is obtained, sodium hydroxide/diethylene glycol solution into reaction solution reacts 5 ~ 15min; it is down to room temperature; under 3000 ~ 8000 rpm, supernatant is abandoned in centrifugation; after layer object is removed using ultra-pure water and alcohol blend cleaning for several times, polyacrylic acid modified ferric oxide nano particle is obtained.Ferric oxide nanometer particle particle diameter distribution produced by the present invention is uniform, grain size is smaller；It is of low cost with good water-soluble, colloidal stability and cell compatibility, it is storage-stable in aqueous solution.
Description
Technical field
The invention belongs to field of material technology, and in particular to a step high temperature method prepares polyacrylic acid modified ferric oxide nano
Grain method.
Background technology
Ferric oxide nanometer particle（Iron Oxide Nanoparticles）It is widely used in magnetic energy-storage medium, biology
Sensor, drug load and the fields such as therapeutic treatment.And in terms of drug is loaded with medical application, ferric oxide nanometer particle exists
In water the homogeneity of size, dispersibility and the stability in cell culture fluid be influence its field apply it is main because
Element.The researchers such as Nat Mater prepare ferric oxide nanometer particle using high temperature method, and particle size obtained is made than more uniform
Standby ferric oxide nanometer particle is because surface is hydrophobic molecule, it is difficult to soluble in water.In order to solve ferric oxide nanometer particle in water
In dissolubility and dispersion problem, Adv. Funct. Mater etc. use ligand exchange process, the oxygen that high temperature method is prepared
Change iron nano-particle coordinate it is modifies, in terms of obtained modified oxidized iron nano-particle can be used for medical diagnostic techniqu,
But during preparing modified oxidized iron nano-particle, often needs that the medium of nano particle will be kept to replace, be easy to make it
Generate agglomeration.
Invention content
Present invention aims at provide a step high temperature method to prepare polyacrylic acid modified ferric oxide nano particl method.
Based on above-mentioned purpose, the present invention takes following technical scheme：
One step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method, includes the following steps：
1）Sodium hydroxide is dissolved in diethylene glycol (DEG), under nitrogen protection, 110 ~ 130 DEG C is heated to, after keeping the temperature 1 ~ 3h, is cooled to 65
~ 75 DEG C, obtain sodium hydroxide/diethylene glycol solution；
2）Iron trichloride hexahydrate, four water frerrous chlorides, polyacrylic acid and diethylene glycol (DEG) are mixed, under nitrogen protection, it is heated to 210 ~
230 DEG C, 0.5 ~ 1.5 h is kept the temperature, reaction solution is obtained, step 1 is added into reaction solution）Sodium hydroxide/diethylene glycol solution, reaction 5 ~
15min is down to room temperature, and under 3000 ~ 8000 rpm, supernatant is abandoned in centrifugation, is removed layer object and is used ultra-pure water and alcohol blend
After cleaning for several times, polyacrylic acid modified ferric oxide nano particle is obtained；The molar ratio of the Iron trichloride hexahydrate and four water frerrous chlorides
For (1 ~ 3) ︰ 1, the monomer molar amount of polyacrylic acid and the mole ratio of Iron trichloride hexahydrate are 10 ︰ 1, and the monomer of polyacrylic acid rubs
It is that (1.5 ~ 2.5) ︰ 1, reaction solution and the volume ratio of sodium hydroxide/diethylene glycol solution are that you, which measure with the mole ratio of diethylene glycol (DEG),
（18~22）︰（15~18）.
Step 1）In, the amount ratio of sodium hydroxide and diethylene glycol (DEG) is 0.2g ︰ 20mL.
Step 2）It is cleaned 3 ~ 5 times using ultra-pure water and alcohol blend.
Step 2）It removes layer object first to be cleaned 2 ~ 5 times with ultra-pure water, then is cleaned using ultra-pure water and alcohol blend.
Compared with prior art, the invention has the advantages that：
1）The present invention is more easy to modify ferric oxide nanometer particle using polyacrylic acid, to obtain more stable iron oxide
Nano particle is " one pot " method without reaction medium is needed to change in entire reaction process, easy to operate, is avoided in conventional method
Agglomeration caused by the processes such as the centrifugal drying to unmodified ferric oxide nanometer particle；
2）Ferric oxide nanometer particle particle diameter distribution produced by the present invention is uniform, grain size is smaller；It is steady with good water solubility, colloid
Qualitative and cell compatibility, of low cost, storage-stable is not in aqueous solution, in three months agglomeration, grain size
It will not change, can be used for drug controlled release and medical field.
Description of the drawings
Fig. 1 is Sample Scan electromicroscopic photograph made from embodiment 1；
Fig. 2 is DLS results in sample made from embodiment 1 in water different time；
Fig. 3 is the hydrated diameter result that sample is surveyed in cell culture fluid made from embodiment 1.
Specific implementation mode
Embodiment 1
One step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method, includes the following steps：
1）0.2g sodium hydroxides are dissolved in 20mL diethylene glycol (DEG)s, under nitrogen protection, 120 DEG C is heated to, after keeping the temperature 1h, is cooled to
70 DEG C, obtain sodium hydroxide/diethylene glycol solution；
2）0.108g Iron trichloride hexahydrates, tetra- water frerrous chlorides of 0.08g, 0.28g polyacrylic acid and 17mL diethylene glycol (DEG)s are mixed, in nitrogen
Under gas shielded, 220 DEG C are heated to, 1 h is kept the temperature, obtains reaction solution, step 1 is added into reaction solution）Gained sodium hydroxide/diethylene glycol (DEG)
Solution reacts 10min, is down to room temperature（25℃）, under 3000 rpm, centrifugation abandons supernatant, it is first clear with ultra-pure water to remove layer object
It washes 3 times, then uses ultra-pure water and alcohol blend（Ultra-pure water and the mixing of alcohol arbitrary proportion）After cleaning 3 times, poly- third is obtained
Olefin(e) acid modified ferric oxide nano particle.
Embodiment 2
One step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method, includes the following steps：
1）0.2g sodium hydroxides are dissolved in 20mL diethylene glycol (DEG)s, under nitrogen protection, 120 DEG C is heated to, after keeping the temperature 1h, is cooled to
65 DEG C, obtain sodium hydroxide/diethylene glycol solution；
2）Iron trichloride hexahydrate, four water frerrous chlorides, polyacrylic acid and diethylene glycol (DEG) (dosage 18ml) are mixed, in nitrogen protection
Under, 210 DEG C are heated to, 1.5 h is kept the temperature, obtains reaction solution, step 1 is added into reaction solution）Sodium hydroxide/diethylene glycol solution, instead
15min is answered, room temperature is down to（25℃）, under 8000 rpm, centrifugation abandons supernatant, removes layer object and first cleaned 5 times with ultra-pure water,
Ultra-pure water and alcohol blend are used again（Ultra-pure water and the mixing of alcohol arbitrary proportion）After cleaning 5 times, obtains polyacrylic acid and repair
Adorn ferric oxide nanometer particle；The molar ratio of the Iron trichloride hexahydrate and four water frerrous chlorides is 2 ︰ 1, the monomer molar of polyacrylic acid
Amount and the mole ratio of Iron trichloride hexahydrate are 10 ︰ 1, and the monomer molar amount of polyacrylic acid and the mole ratio of diethylene glycol (DEG) are 1.5 ︰ 1.
Embodiment 3
One step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method, includes the following steps：
1）0.2g sodium hydroxides are dissolved in 20mL diethylene glycol (DEG)s, under nitrogen protection, 120 DEG C is heated to, after keeping the temperature 1h, is cooled to
75 DEG C, obtain sodium hydroxide/diethylene glycol solution；
2）By Iron trichloride hexahydrate, four water frerrous chlorides, polyacrylic acid and diethylene glycol (DEG)（Dosage is 16ml）Mixing, in nitrogen protection
Under, 230 DEG C are heated to, 0.5 h is kept the temperature, obtains reaction solution, step 1 is added into reaction solution）Sodium hydroxide/diethylene glycol solution, instead
5min is answered, room temperature is down to（25℃）, under 5000 rpm, centrifugation abandons supernatant, removes layer object and first cleaned 2 times with ultra-pure water, then
Using ultra-pure water and alcohol blend（Ultra-pure water and the mixing of alcohol arbitrary proportion）After cleaning 3 times, polyacrylic acid modification is obtained
Ferric oxide nanometer particle；The molar ratio of the Iron trichloride hexahydrate and four water frerrous chlorides is 3 ︰ 1, the monomer molar amount of polyacrylic acid
Mole ratio with Iron trichloride hexahydrate is 10 ︰ 1, and the monomer molar amount of polyacrylic acid and the mole ratio of diethylene glycol (DEG) are 2.5 ︰ 1.
4 performance test of embodiment
4.1 microstructure analysis
By the scanned electron-microscope scanning of polyacrylic acid modified ferric oxide nano particulate samples made from embodiment 1, scanning electron microscope photograph is obtained
Piece, as shown in Figure 1.Wherein, Figure 1A is the photo under high power, photos of the Figure 1B under low power.
As shown in Figure 1, ferric oxide nanometer particle particle diameter distribution is uniform, and grain size is smaller.
4.2 stability test in water
Polyacrylic acid modified ferric oxide nano particulate samples made from embodiment 1 are deposited in water, in different time, are used
Dynamic light scattering（DLS）The grain size of nano particle is measured, the results are shown in Figure 2.
As shown in Figure 2, nano particle produced by the present invention can steadily store in aqueous solution, will not in three months
There is agglomeration, grain size will not change, and have preferable stability.
4.2 product particle dimensional stabilitys are tested
By taking embodiment 1 as an example, polyacrylic acid modified ferric oxide nano particulate samples made from embodiment 1 are dissolved in cell culture fluid
In（Trypticase soy broth）, using its hydrated diameter of dynamic light scattering measurement.The results are shown in Figure 3.
From the figure 3, it may be seen that using the hydrated diameter of dynamic light scattering measurement for 79.92nm, show that the polyacrylic acid of gained is repaiied
Decorations ferric oxide nanometer particle sample is not reunited after being dissolved in cell culture fluid, this further demonstrates that product of the present invention
Grain has good dimensional stability.
Claims (4)
1. a step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method, which is characterized in that include the following steps：
1）Sodium hydroxide is dissolved in diethylene glycol (DEG), under nitrogen protection, 110 ~ 130 DEG C is heated to, after keeping the temperature 1 ~ 3h, is cooled to 65
~ 75 DEG C, obtain sodium hydroxide/diethylene glycol solution；
2）Iron trichloride hexahydrate, four water frerrous chlorides, polyacrylic acid and diethylene glycol (DEG) are mixed, under nitrogen protection, it is heated to 210 ~
230 DEG C, 0.5 ~ 1.5 h is kept the temperature, reaction solution is obtained, step 1 is added into reaction solution）Sodium hydroxide/diethylene glycol solution, reaction 5 ~
15min is down to room temperature, and under 3000 ~ 8000 rpm, supernatant is abandoned in centrifugation, is removed layer object and is used ultra-pure water and alcohol blend
After cleaning for several times, polyacrylic acid modified ferric oxide nano particle is obtained；The molar ratio of the Iron trichloride hexahydrate and four water frerrous chlorides
For (1 ~ 3) ︰ 1, the monomer molar amount of polyacrylic acid and the mole ratio of Iron trichloride hexahydrate are 10 ︰ 1, and the monomer of polyacrylic acid rubs
It is that (1.5 ~ 2.5) ︰ 1, reaction solution and the volume ratio of sodium hydroxide/diethylene glycol solution are that you, which measure with the mole ratio of diethylene glycol (DEG),（18
~22）︰（15~18）.
2. step high temperature method as described in claim 1 prepares polyacrylic acid modified ferric oxide nano particl method, feature exists
In step 1）In, the amount ratio of sodium hydroxide and diethylene glycol (DEG) is 0.2g ︰ 20mL.
3. step high temperature method as claimed in claim 2 prepares polyacrylic acid modified ferric oxide nano particl method, feature exists
In step 2）It is cleaned 3 ~ 5 times using ultra-pure water and alcohol blend.
4. step high temperature method as claimed in claim 3 prepares polyacrylic acid modified ferric oxide nano particl method, feature exists
In step 2）It removes layer object first to be cleaned 2 ~ 5 times with ultra-pure water, then is cleaned using ultra-pure water and alcohol blend.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110853865A (en) * | 2019-11-20 | 2020-02-28 | 江南大学 | Preparation method and application of ferroferric oxide single-layer nano film |
| CN114854054A (en) * | 2022-04-02 | 2022-08-05 | 阜阳德润磁材科技有限公司 | Magnetic particle preparation process |
| CN115520907A (en) * | 2022-04-14 | 2022-12-27 | 西安超磁纳米生物科技有限公司 | Ultra-small ferrite nano-particles with active groups, and preparation and application thereof |
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| CN110853865A (en) * | 2019-11-20 | 2020-02-28 | 江南大学 | Preparation method and application of ferroferric oxide single-layer nano film |
| CN114854054A (en) * | 2022-04-02 | 2022-08-05 | 阜阳德润磁材科技有限公司 | Magnetic particle preparation process |
| CN115520907A (en) * | 2022-04-14 | 2022-12-27 | 西安超磁纳米生物科技有限公司 | Ultra-small ferrite nano-particles with active groups, and preparation and application thereof |
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