CN104843802B - The preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon - Google Patents
The preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon Download PDFInfo
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- CN104843802B CN104843802B CN201510254792.XA CN201510254792A CN104843802B CN 104843802 B CN104843802 B CN 104843802B CN 201510254792 A CN201510254792 A CN 201510254792A CN 104843802 B CN104843802 B CN 104843802B
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Abstract
The invention belongs to the preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon, adopt the synthesis of seed growth Two-step control, namely utilize nano particle that solution A produces as seed, utilize solution B as the mother liquor of subsequent growth, realized the regulation and control of super-paramagnetic ferriferrous oxide Microsphere Size by both control ratio and temperature. The size of the micrometer sized superparamagnetic Z 250 microballoon of preparation is between 500nm to 2500nm, and favorable dispersity, uniform particle diameter, and the ferroferric oxide particle prepared has superparamagnetic performance.
Description
Technical field
The present invention relates to field of nano material preparation, it is specifically related to the preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon.
Background technology
Z 250 (Fe3O4) it is a kind of important spinel type ferrite, it it is novel high functional inorganic materials geared to the 21st century, owing to it has the unrivaled property of general block materials and novelty teabag in optical, electrical, medical, magnetic Jie etc., so in fields such as national defence, environmental engineering, Surface Engineering, chemical industry, electronics and semiconductor materials, there is application prospect widely. In in the past few decades, the various method preparing Z 250 receives much attention, up to the present, develop multiple synthetic method, such as chemical coprecipitation, oil/water emulsion method, thermal decomposition method, solvent-thermal process method, sonochemistry method, discharge decomposition method, arc electric discharge, combustion synthesis method etc. Although the preparation research of Z 250 has obtained very big progress, but preparation good dispersion, uniform particle diameter micrometer sized superparamagnetic Z 250 spherical particle are still very difficult.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon with good dispersion, uniform particle diameter.
For achieving the above object, the technical solution used in the present invention is, a preparation method for micrometer sized superparamagnetic Z 250 microballoon, comprises the following steps: 1. join in ethylene glycol by Iron(III) chloride hexahydrate, sodium formiate and 10-30wt% polyacrylic acid solution, stirs even mixed solution A; 2. Iron(III) chloride hexahydrate, sodium acetate are joined in ethylene glycol, stir even mixing solutions B; 3. mixed solution A is transferred to, in churned mechanically reactor, mechanical stirring speed is 150-300 rev/min, reactor is warming up to 230 ~ 250 DEG C and keeps, react and obtain black turbid solution in 2 ~ 3 hours; Reactor is cooled to 60-100 DEG C, and after reacting kettle inner pressure is down to normal pressure, mixing solutions B is injected in reactor, mechanical stirring speed is adjusted to 30-60 rev/min, stir 10 ~ 20 minutes, then reactor is warmed up to 180 ~ 200 DEG C and keeps, continue reaction and obtain mixture in 5 ~ 12 hours; 4. the mixture that 3. step is obtained by reacting is obtained black solid through Magneto separate, by black solid ethanol purge 2 ~ 6 times, then at 60-80 DEG C of baking oven inner drying, obtain micrometer sized superparamagnetic Z 250 microballoon.
Described step 1. in the mol ratio of Iron(III) chloride hexahydrate and sodium formiate be 1: 8 ~ 10, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 300 ~ 500, the volume ratio of ethylene glycol and 10-30wt% polyacrylic acid solution be 30 ~ 50: 1.
Described step 2. in the mol ratio of Iron(III) chloride hexahydrate and sodium acetate be 1: 6 ~ 8, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 30 ~ 150.
Described step 3. in the volume ratio of mixed solution A and mixing solutions B be 1: 1 ~ 15.
The useful effect that the present invention produces is, the raw material that the preparation method of the present invention uses is easy to get, technique is simple, adopt the synthesis of seed growth Two-step control, namely utilize nano particle that solution A produces as seed, utilize solution B as the mother liquor of subsequent growth, realized the regulation and control of super-paramagnetic ferriferrous oxide Microsphere Size by both control ratio and temperature. The size of the micrometer sized superparamagnetic Z 250 microballoon of preparation is between 500nm to 2500nm, and favorable dispersity, uniform particle diameter, and the ferroferric oxide particle prepared has superparamagnetic performance.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of ferroferric oxide nano granules seed prepared by embodiment 1;
Fig. 2 is the electron scanning micrograph of micrometer sized superparamagnetic Z 250 microballoon prepared by embodiment 1;
Fig. 3 is the electron scanning micrograph of micrometer sized superparamagnetic Z 250 microballoon prepared by embodiment 2;
Fig. 4 is the electron scanning micrograph of micrometer sized superparamagnetic Z 250 microballoon prepared by embodiment 3;
Fig. 5 is the electron scanning micrograph of micrometer sized superparamagnetic Z 250 microballoon prepared by embodiment 4;
Fig. 6 is that micrometer sized superparamagnetic Z 250 microballoon magnetic performance prepared by embodiment 1 characterizes the typical superparamagnetic curve obtained.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to this.
Embodiment 1
The preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon, comprise the following steps: 1. Iron(III) chloride hexahydrate, sodium formiate and 20wt% polyacrylic acid solution are joined in ethylene glycol, stir even mixed solution A, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium formiate be 1: 9, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 500, the volume ratio of ethylene glycol and 20wt% polyacrylic acid solution be 40: 1; 2. Iron(III) chloride hexahydrate, sodium acetate are joined in ethylene glycol, stir even mixing solutions B, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium acetate be 1: 7, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 150; 3. mixed solution A is transferred to, in churned mechanically autoclave, mechanical stirring speed is 200 revs/min, autoclave is warming up to 240 DEG C and keeps, reacts and obtain black turbid solution in 2.5 hours; Autoclave is cooled to 80 DEG C, and will after pressure is down to normal pressure in autoclave, mixing solutions B is injected in reactor, mechanical stirring speed is adjusted to 45 revs/min, stir 15 minutes, then autoclave is warmed up to 200 DEG C and keeps, continue reaction and obtain mixture in 5 hours; Wherein the volume ratio of mixed solution A and mixing solutions B is 1: 1; 4. the mixture that 3. step is obtained by reacting is obtained black solid through Magneto separate, by black solid washes of absolute alcohol 4 times, then at 70 DEG C of baking oven inner dryings, obtain the Z 250 microballoon of mean sizes at 500nm, its electron scanning micrograph is such as Fig. 2 (SEM, JEOLJSM-6360LV, acceleration voltage is 10kV) shown in, as can be seen from Figure 2 synthetic product is very even. As shown in Figure 6, saturation magnetization reaches 88emu/g to its magnetic characterization, and coercive force be the Z 250 microballoon that zero confirmation has been synthesized is superparamagnetic.
In the present embodiment step 3. in black turbid solution obtain ferroferric oxide nano granules through Magneto separate, by this ferroferric oxide nano granules through washes of absolute alcohol 3 times, after 70 DEG C of baking oven inner dryings, obtaining mean sizes is 150nm ferroferric oxide nano granules seed, its electron scanning micrograph is such as Fig. 1 (SEM, JEOLJSM-6360LV, acceleration voltage is 10kV) shown in.
Embodiment 2
The preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon, comprise the following steps: 1. Iron(III) chloride hexahydrate, sodium formiate and 10wt% polyacrylic acid solution are joined in ethylene glycol, stir even mixed solution A, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium formiate be 1: 8, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 400, the volume ratio of ethylene glycol and 10wt% polyacrylic acid solution be 30: 1; 2. Iron(III) chloride hexahydrate, sodium acetate are joined in ethylene glycol, stir even mixing solutions B, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium acetate be 1: 6, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 100; 3. mixed solution A is transferred to, in churned mechanically autoclave, mechanical stirring speed is 150 revs/min, autoclave is warming up to 230 DEG C and keeps, reacts and obtain black turbid solution in 2 hours; Autoclave is cooled to 60 DEG C, and by after in autoclave, pressure is down to normal pressure, mixing solutions B is injected in autoclave, mechanical stirring speed is adjusted to 30 revs/min, stir 10 minutes, then autoclave is warmed up to 200 DEG C and keeps, continue reaction and obtain mixture in 10 hours; Wherein the volume ratio of mixed solution A and mixing solutions B is 1: 3; 4. the mixture that 3. step is obtained by reacting is obtained black solid through Magneto separate, by black solid washes of absolute alcohol 2 times, then at 60 DEG C of baking oven inner dryings, obtain the super-paramagnetic ferriferrous oxide microballoon that mean sizes is 900nm, its electron scanning micrograph is such as Fig. 3 (SEM, JEOLJSM-6360LV, acceleration voltage is 10kV) shown in, as can be seen from Figure 3 synthetic product is very even.
Embodiment 3
The preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon, comprise the following steps: 1. Iron(III) chloride hexahydrate, sodium formiate and 30wt% polyacrylic acid solution are joined in ethylene glycol, stir even mixed solution A, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium formiate be 1: 10, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 300, the volume ratio of ethylene glycol and 30wt% polyacrylic acid solution be 50: 1; 2. Iron(III) chloride hexahydrate, sodium acetate are joined in ethylene glycol, stir even mixing solutions B, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium acetate be 1: 8, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 50; 3. mixed solution A is transferred to, in churned mechanically autoclave, mechanical stirring speed is 300 revs/min, autoclave is warming up to 250 DEG C and keeps, reacts and obtain black turbid solution in 3 hours; Reactor is cooled to 100 DEG C, and after pressure is down to normal pressure in autoclave, mixing solutions B will be injected into high pressure
In reactor, mechanical stirring speed is adjusted to 60 revs/min, stirs 20 minutes, then autoclave is warmed up to 190 DEG C and keeps, and continues reaction and obtains mixture in 12 hours; Wherein the volume ratio of mixed solution A and mixing solutions B is 1: 7; 4. the mixture that 3. step is obtained by reacting is obtained black solid through Magneto separate, by black solid washes of absolute alcohol 6 times, then at 80 DEG C of baking oven inner dryings, obtain the super-paramagnetic ferriferrous oxide microballoon that mean sizes is 1500nm, its electron scanning micrograph is such as Fig. 4 (SEM, JEOLJSM-6360LV, acceleration voltage is 10kV) shown in, as can be seen from Figure 4 synthetic product is very even.
Embodiment 4
The preparation method of a kind of micrometer sized superparamagnetic Z 250 microballoon, comprise the following steps: 1. Iron(III) chloride hexahydrate, sodium formiate and 25wt% polyacrylic acid solution are joined in ethylene glycol, stir even mixed solution A, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium formiate be 1: 8, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 300, the volume ratio of ethylene glycol and 25wt% polyacrylic acid solution be 31: 1; 2. Iron(III) chloride hexahydrate, sodium acetate are joined in ethylene glycol, stir even mixing solutions B, wherein the mol ratio of Iron(III) chloride hexahydrate and sodium acetate be 1: 6, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 30; 3. mixed solution A is transferred to, in churned mechanically autoclave, mechanical stirring speed is 250 revs/min, autoclave is warming up to 230 DEG C and keeps, reacts and obtain black turbid solution in 3 hours; Autoclave is cooled to 90 DEG C, and will after pressure is down to normal pressure in autoclave, mixing solutions B is injected in reactor, mechanical stirring speed is adjusted to 50 revs/min, stir 10 minutes, then autoclave is warmed up to 180 DEG C and keeps, continue reaction and obtain mixture in 12 hours; Wherein the volume ratio of mixed solution A and mixing solutions B is 1: 15; 4. the mixture that 3. step is obtained by reacting is obtained black solid through Magneto separate, by black solid washes of absolute alcohol 5 times, then at 75 DEG C of baking oven inner dryings, obtain the super-paramagnetic ferriferrous oxide microballoon that mean sizes is 2500nm, its electron scanning micrograph is such as Fig. 5 (SEM, JEOLJSM-6360LV, acceleration voltage is 10kV) shown in, as can be seen from Figure 5 synthetic product is very even.
Claims (3)
1. the preparation method of a micrometer sized superparamagnetic Z 250 microballoon, it is characterised in that, comprise the following steps: 1. Iron(III) chloride hexahydrate, sodium formiate and 10-30wt% polyacrylic acid solution are joined in ethylene glycol, stir even mixed solution A; 2. Iron(III) chloride hexahydrate, sodium acetate are joined in ethylene glycol, stir even mixing solutions B; 3. mixed solution A is transferred to in churned mechanically reactor, reactor is warming up to 230 ~ 250 DEG C and keeps, react and obtain black turbid solution in 2 ~ 3 hours, reactor is cooled to 60-100 DEG C, and after reacting kettle inner pressure is down to normal pressure, mixing solutions B is injected in reactor, stir 10 ~ 20 minutes, then reactor is warmed up to 180 ~ 200 DEG C and keeps, continue reaction and obtain mixture in 5 ~ 12 hours; 4. the mixture that 3. step is obtained by reacting is obtained black solid through Magneto separate, by black solid ethanol purge 2 ~ 6 times, then at 60-80 DEG C of baking oven inner drying, obtain micrometer sized superparamagnetic Z 250 microballoon; Described step 3. in the volume ratio of mixed solution A and mixing solutions B be 1: 1 ~ 15.
2. the preparation method of micrometer sized superparamagnetic Z 250 microballoon as claimed in claim 1, it is characterized in that, described step 1. in the mol ratio of Iron(III) chloride hexahydrate and sodium formiate be 1: 8 ~ 10, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 300 ~ 500, the volume ratio of ethylene glycol and 10-30wt% polyacrylic acid solution be 30 ~ 50: 1.
3. the preparation method of micrometer sized superparamagnetic Z 250 microballoon as claimed in claim 1, it is characterized in that, described step 2. in the mol ratio of Iron(III) chloride hexahydrate and sodium acetate be 1: 6 ~ 8, the mol ratio of Iron(III) chloride hexahydrate and ethylene glycol be 1: 30 ~ 150.
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| CN105967241B (en) * | 2016-05-06 | 2018-01-16 | 华侨大学 | One kind prepares Fe3O4The method of nanoscale magnetic bead |
| CN112142115A (en) * | 2019-06-27 | 2020-12-29 | 南京中科拜尔医学技术有限公司 | Preparation method of superparamagnetic micron-sized magnetic beads |
| CN111072070B (en) * | 2019-12-24 | 2022-08-12 | 周口师范学院 | Preparation method of high-saturation magnetization superparamagnetic porous ferrite microspheres |
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| CN101805026A (en) * | 2010-03-12 | 2010-08-18 | 南京大学 | Method for preparing spherical super-paramagnetic ferroferric oxide nano-clusters |
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