CN104403030A - Suspension polymerization preparation method of polystyrene-coated ferriferrous oxide composite particle - Google Patents
Suspension polymerization preparation method of polystyrene-coated ferriferrous oxide composite particle Download PDFInfo
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- CN104403030A CN104403030A CN201410620627.7A CN201410620627A CN104403030A CN 104403030 A CN104403030 A CN 104403030A CN 201410620627 A CN201410620627 A CN 201410620627A CN 104403030 A CN104403030 A CN 104403030A
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Abstract
The invention relates to a suspension polymerization preparation method of a polystyrene-coated ferriferrous oxide composite particle. The method comprises the following steps: placing a n-octane solution in a water bath, adding a mixed solution of ferrous sulfate and ferric chloride, then adding sodium oleate and ammonia water to carry out reactions to obtain oil-soluble ferriferrous oxide; mixing the obtained ferriferrous oxide, polystyrene, and benzoyl peroxide under supersonic waves to obtain a mixed solution, adding a dispersant and deionized water, carrying out reactions for 4 to 6 hours at a temperature of 90 DEG C, washing, separating, and drying so as to obtain the polystyrene-coated ferriferrous oxide magnetic composite particles. The preparation method has the advantages of simple operation and mild reaction conditions. The obtained magnetic composite particles are evenly dispersed, are stable, and thus have a good application prospect.
Description
Technical field
The invention belongs to the preparation field of magnetic composite, particularly a kind of suspension polymerization prepares the method for polystyrene coated ferroferric oxide magnetic composite particles.
Background technology
Ferriferrous oxide nano magneticsubstance, because of itself distinctive physics, chemical property, as small-size effect, surface and interface effect and macro quanta tunnel effect, shows the character different from conventional material.Be commonly used for recording materials, pigment, magnetic fluid material, catalyzer, magnetic macromolecular microsphere and electronic material etc., it also has good application prospect at biological technical field and medical field.Z 250 has good magnetic performance, and the matrix material after polystyrene is coated can be applied to the vitro detection of disease, has important medical use and is worth.Thus, coated the having great importance of oil soluble Z 250 p-poly-phenyl ethene under research and probe differential responses condition.
At present, the preparation main method of Z 250 has coprecipitation method and thermal decomposition method.Co deposited synthesis nano particle granular size heterogeneity out, dispersed bad, easily reunite, oxidizable etc.; Although the nano particle granular size that thermolysis process produces is more homogeneous, conditional request during synthesis is higher, and generally need high-temperature high-pressure reaction kettle, temperature will maintain about 180 DEG C.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that suspension polymerization prepares polystyrene coated ferroferric oxide magnetic composite particles, and the inventive method is simple to operate, reaction conditions is gentle, and experimental raw is cheap, good economy performance; The magnetic nano-particle that this invention prepares is uniformly dispersed, stable, have a good application prospect.
A kind of suspension polymerization of the present invention prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, comprising:
(1) octane solution is placed in 20-30 DEG C of water-bath, adds the mixing solutions of ferrous sulfate and iron trichloride, then add sodium oleate and ammoniacal liquor, reaction 1-2h, obtains oil soluble Z 250; Wherein the mol ratio of ferrous sulfate and sodium oleate is 1:1-2; The volume ratio of ammonia soln and mixing solutions is 1-2.5:10;
(2) by oil soluble Z 250, vinylbenzene (5% sodium hydroxide solution washing 2-5 time), benzoyl peroxide, ultrasonic mixing, obtain mixing solutions, then add in dispersion agent and deionized water, under 80-100 DEG C of condition, react 4-6h, washing, be separated, drying, obtains polystyrene coated ferroferric oxide magnetic composite particles; Wherein the mol ratio of Z 250 and vinylbenzene, benzoyl peroxide is 1:33.49:0.29-2.89; Dispersion agent and cinnamic mol ratio are 1:110.8.
In described step (1), the mass percentage concentration of octane solution is 98%.
In described step (1), in mixing solutions, the mol ratio of ferrous sulfate and iron trichloride is 1:2.
In described step (1), in mixing solutions, the concentration of ferrous sulfate is 0.998-0.299M, and iron trichloride concentration is 0.199-0.600M.
In described step (1), bath temperature is 25 DEG C, and the reaction times is 2h.
In described step (2), in mixing solutions, the concentration of Z 250 is 0.011-0.032M; The mol ratio of Z 250 and vinylbenzene, benzoyl peroxide is 1:33.49:2.89.
In described step (2), the mass percentage concentration of dispersion agent is 1.5%; The volume ratio of dispersion agent and deionized water is 1:1-4.
In described step (2), dispersion agent is polyvinyl alcohol.
In described step (2), temperature of reaction is 90 DEG C.
In described step (2), washing is for using washing with alcohol 3-5 time, is separated into magnetic resolution; Drying temperature is 50-65 DEG C, and time of drying is 1-5h.
Preparation method's principle: water-fast styrene monomer and oil soluble Z 250 be suspended in water with small droplets shape and be polymerized, the Z 250 that the sodium oleate of water-oil interface method synthesis is modified and cinnamic vinyl polymerization generate product.Basal component has monomer, initiator, water and dispersion agent, and oil-soluble monomer can be dispersed in water formation stable suspension by dispersion agent.
beneficial effect
(1) the present invention's Z 250 size tunable, good dispersity, product purity of adopting water-oil interface method to synthesize is high, polystyrene to Z 250 coated simple to operate, productive rate is high, cost is low, efficiency is high;
(2) the present invention is simple to operate, reaction conditions is gentle, and experimental raw is cheap, good economy performance;
(3) the magnetic coupling granular size that the present invention obtains is 268nm-2.6 μm, is uniformly dispersed, stable, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of embodiment 1;
Fig. 2 is the X-ray diffractogram of embodiment 1 products therefrom;
Fig. 3 is the TEM figure of embodiment 1 products therefrom;
Fig. 4 is the TEM figure of embodiment 2 products therefrom;
Fig. 5 is the TEM figure of comparative example 1 products therefrom.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
1, getting 30ml octane solution joins in there-necked flask, is placed in 25 DEG C of water-baths;
2, take 0.444g (0.01mol) ferrous sulfate and 0.864g (0.02mol) iron trichloride is mixedly configured into 20ml solution, slowly add in there-necked flask with syringe under stirring fully;
3, take 4.0g sodium oleate and be mixed with 20mL solution, get 1ml sodium oleate solution, slowly add in there-necked flask with syringe under stirring fully;
4, get the ammoniacal liquor that 1.8mL massfraction is 27%, slowly add in there-necked flask with syringe, in a water bath ageing reaction 2h, obtain oil soluble Z 250 with after washing with alcohol for several times rear 10000rpm centrifugation.
5, get 1g above-mentioned oil soluble Z 250,1h is stand-by for the ultrasonic mixing of 16.91ml vinylbenzene (5% sodium hydroxide solution washs three times) 0.9g benzoyl peroxide.
6, getting 20ml polyvinyl alcohol adds in there-necked flask, is transferred in there-necked flask, is finally transferred to there-necked flask with after 100ml deionized water rinsing by above-mentioned Z 250, vinylbenzene and benzoyl peroxide mixing solutions.
7, startup is stirred and is rapidly heated to 90 DEG C, controls constant rotational speed reaction 4h, by product absolute ethanol washing several, is drying to obtain magnetic coupling particle after Magneto separate under 60 DEG C of conditions.Clap TEM figure and show, product median size is about 4.60 ± 0.62 μm, and dispersion is relatively more even, and does not almost have agglomeration.
Embodiment 2
1, getting 30ml octane solution joins in there-necked flask, is placed in 25 DEG C of water-baths;
2, take 0.444g (0.01mol) ferrous sulfate and 0.864g (0.02mol) iron trichloride is mixedly configured into 20ml solution, slowly add in there-necked flask with syringe under stirring fully;
3, take 4.0g sodium oleate and be mixed with 20mL solution, get 1ml sodium oleate solution, slowly add in there-necked flask with syringe under stirring fully;
4, get the ammoniacal liquor that 1.8mL massfraction is 27%, slowly add in there-necked flask with syringe, in a water bath ageing reaction 2h, obtain oil soluble Z 250 with after washing with alcohol for several times rear 10000rpm centrifugation.
5, get 1g above-mentioned oil soluble Z 250,1h is stand-by for the ultrasonic mixing of 16.91ml vinylbenzene (5% sodium hydroxide solution washs three times) 2.0g benzoyl peroxide.
6, getting 20ml polyvinyl alcohol adds in there-necked flask, is transferred in there-necked flask, is finally transferred to there-necked flask with after 100ml deionized water rinsing by above-mentioned Z 250, vinylbenzene and benzoyl peroxide mixing solutions.
7, startup is stirred and is rapidly heated to 90 DEG C, controls constant rotational speed reaction 4h, by product absolute ethanol washing several, is drying to obtain magnetic coupling particle after Magneto separate under 60 DEG C of conditions.Clap TEM figure and show, product median size is about 500 ± 0.62nm, and dispersion is relatively more even, and does not almost have agglomeration.
Comparative example 1
1, getting 30ml octane solution joins in there-necked flask, is placed in 25 DEG C of water-baths;
2, take 0.444g (0.01mol) ferrous sulfate and 0.864g (0.02mol) iron trichloride is mixedly configured into 20ml solution, slowly add in there-necked flask with syringe under stirring fully;
3, take 4.0g sodium oleate and be mixed with 20mL solution, get 1ml sodium oleate solution, slowly add in there-necked flask with syringe under stirring fully;
4, get the ammoniacal liquor that 1.8mL massfraction is 27%, slowly add in there-necked flask with syringe, in a water bath ageing reaction 2h, obtain oil soluble Z 250 with after washing with alcohol for several times rear 10000rpm centrifugation.
5, get 1g above-mentioned oil soluble Z 250,1h is stand-by for the ultrasonic mixing of 16.91ml vinylbenzene (5% sodium hydroxide solution washs three times) 3.0g benzoyl peroxide.
6, getting 20ml polyvinyl alcohol adds in there-necked flask, is transferred in there-necked flask, is finally transferred to there-necked flask with after 100ml deionized water rinsing by above-mentioned Z 250, vinylbenzene and benzoyl peroxide mixing solutions.
7, startup is stirred and is rapidly heated to 90 DEG C, controls constant rotational speed reaction 4h, by product absolute ethanol washing several, is drying to obtain magnetic coupling particle after Magneto separate under 60 DEG C of conditions.Clap TEM figure and show, product median size is about 80.40 ± 0.62nm, disperses uneven, almost all reunites.
Claims (10)
1. suspension polymerization prepares a method for polystyrene coated ferroferric oxide magnetic composite particles, comprising:
(1) octane solution is placed in 20-30 DEG C of water-bath, adds the mixing solutions of ferrous sulfate and iron trichloride, then add sodium oleate and ammoniacal liquor, reaction 1-2h, obtains oil soluble Z 250; Wherein the mol ratio of ferrous sulfate and sodium oleate is 1:1-2; The volume ratio of ammonia soln and mixing solutions is 1-2.5:10;
(2) by oil soluble Z 250, vinylbenzene, benzoyl peroxide, ultrasonic mixing, obtains mixing solutions, then add in dispersion agent and deionized water, under 80-100 DEG C of condition, react 4-6h, washing, be separated, dry, obtain polystyrene coated ferroferric oxide magnetic composite particles; Wherein the mol ratio of Z 250 and vinylbenzene, benzoyl peroxide is 1:33.49:0.29-2.89; Dispersion agent and cinnamic mol ratio are 1:110.8.
2. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (1), the mass percentage concentration of octane solution is 98%.
3. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (1), in mixing solutions, the mol ratio of ferrous sulfate and iron trichloride is 1:2.
4. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (1), in mixing solutions, the concentration of ferrous sulfate is 0.998-0.299M, and iron trichloride concentration is 0.199-0.600M.
5. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (1), bath temperature is 25 DEG C, and the reaction times is 2h.
6. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (2), in mixing solutions, the concentration of Z 250 is 0.011-0.032M; The mol ratio of Z 250 and vinylbenzene, benzoyl peroxide is 1:33.49:2.89; Vinylbenzene 5% sodium hydroxide solution washing 2-5 time.
7. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (2), the mass percentage concentration of dispersion agent is 1.5%; The volume ratio of dispersion agent and deionized water is 1:1-4.
8. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (2), dispersion agent is polyvinyl alcohol.
9. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (2), temperature of reaction is 90 DEG C.
10. a kind of suspension polymerization according to claim 1 prepares the method for polystyrene coated ferroferric oxide magnetic composite particles, it is characterized in that: in described step (2), washing is for using washing with alcohol 3-5 time, is separated into magnetic resolution; Drying temperature is 50-65 DEG C, and time of drying is 1-5h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266775A (en) * | 2020-10-23 | 2021-01-26 | 西南石油大学 | Preparation of in-situ nano emulsifier and oil reservoir application method |
| CN112358630A (en) * | 2020-10-27 | 2021-02-12 | 中车青岛四方机车车辆股份有限公司 | Polystyrene-coated metal oxide nano particle and preparation method and application thereof |
| CN114015087A (en) * | 2021-11-16 | 2022-02-08 | 安徽和佳医疗用品科技有限公司 | High-elasticity rubber and plastic gloves containing magnetic microcapsules and preparation method thereof |
| CN115873589A (en) * | 2023-02-28 | 2023-03-31 | 成都理工大学 | Intelligent oil phase release self-suspension tracer proppant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556123A (en) * | 2003-12-30 | 2004-12-22 | 上海交通大学 | Preparation method of high magnetism content magnetic polymer particle |
| CN101544730A (en) * | 2009-04-10 | 2009-09-30 | 华东理工大学 | Method for preparing nanometer spherical polyelectrolyte brush with magnetic kernel |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556123A (en) * | 2003-12-30 | 2004-12-22 | 上海交通大学 | Preparation method of high magnetism content magnetic polymer particle |
| CN101544730A (en) * | 2009-04-10 | 2009-09-30 | 华东理工大学 | Method for preparing nanometer spherical polyelectrolyte brush with magnetic kernel |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266775A (en) * | 2020-10-23 | 2021-01-26 | 西南石油大学 | Preparation of in-situ nano emulsifier and oil reservoir application method |
| US11618847B2 (en) | 2020-10-23 | 2023-04-04 | Southwest Petroleum University | Methods for preparing and applying a nano emulsifier |
| CN112358630A (en) * | 2020-10-27 | 2021-02-12 | 中车青岛四方机车车辆股份有限公司 | Polystyrene-coated metal oxide nano particle and preparation method and application thereof |
| CN112358630B (en) * | 2020-10-27 | 2023-07-14 | 中车青岛四方机车车辆股份有限公司 | Polystyrene coated metal oxide nanoparticle and preparation method and application thereof |
| CN114015087A (en) * | 2021-11-16 | 2022-02-08 | 安徽和佳医疗用品科技有限公司 | High-elasticity rubber and plastic gloves containing magnetic microcapsules and preparation method thereof |
| CN115873589A (en) * | 2023-02-28 | 2023-03-31 | 成都理工大学 | Intelligent oil phase release self-suspension tracer proppant and preparation method thereof |
| CN115873589B (en) * | 2023-02-28 | 2023-05-09 | 成都理工大学 | Intelligent oil phase release self-suspension tracer type propping agent and preparation method thereof |
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