CN1631949A - Method for preparing hollow magnetic composite particulate for magnetic rheologic liquid by using polystyrene microsphere - Google Patents
Method for preparing hollow magnetic composite particulate for magnetic rheologic liquid by using polystyrene microsphere Download PDFInfo
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- CN1631949A CN1631949A CN 200410084318 CN200410084318A CN1631949A CN 1631949 A CN1631949 A CN 1631949A CN 200410084318 CN200410084318 CN 200410084318 CN 200410084318 A CN200410084318 A CN 200410084318A CN 1631949 A CN1631949 A CN 1631949A
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- hollow
- magnetic
- magnetic composite
- iron salt
- composite particle
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Abstract
The invention belongs to compound material and function material technological field, concretely are a shallow magnetic compound micro particle for magnetic rheologic liquid and its preparing method. The micro ball is formed by covering a layer of Fe3O4 on the shallow polystyrene micro ball, and it is comprised of shallow polystyrene micro ball, trivalent ferric salt, bivalent ferric salt, dispersant and alkali which are mixed by proper ratio. Through supersonic dispersion, covering micro particle and after-procession, the product is made. The product made by the invention has small density, good magnetic performance, high shearing stress and outstanding depositing stability.
Description
Technical field
The invention belongs to matrix material and technical field of function materials, be specifically related to a kind of hollow magnetic particulate that is used for magnetic flow liquid and preparation method thereof.
Background technology
Tiny balloon is a kind of novel microparticle material that grows up in 20th century five, the sixties.Its distinguishing feature is that density is little, mechanical strength is big, good stability.Magnetic oxide Fe
3O
4Can be prepared into the particle that particle diameter is tens nanometers, good application prospects be arranged as the magnetic flow liquid material.But the magnetic particle in traditional magnetic flow liquid since density far above Media density, have easy reunion, the characteristics of free settling, had a strong impact on magnetic flow liquid use properties and apply.Fe
3O
4Particle is no exception, density is too big, and free settling has limited its application in this field.
Summary of the invention
The objective of the invention is to propose that a kind of density is little, magnetic property good, sedimentation stability is good and shear yield stress is high can be used for magnetic particle of magnetic flow liquid and preparation method thereof.
The magnetic particle that is used for magnetic flow liquid that the present invention proposes is to coat one deck Fe at hollow PS microsphere surface
3O
4And the Hollow Compound magnetic particle of forming, its material component proportioning by weight is as follows:
100 parts of hollow PS microballoons
Dispersion agent 0-50 part
Trivalent iron salt 50-400 part
Divalent iron salt 20-200 part
Alkali 20-200 part
Wherein, hollow PS microballoon is that particle diameter is the hollow polystyrene microsphere of 20nm-20 μ m.
Described dispersion agent is meant various organic and inorganic, compound tensio-active agents.
Described trivalent iron salt is meant the salt that contains ferric ion, as FeCl
3, Fe (NO
3)
3, Fe
2(SO
4)
3Deng, but be not limited only to this.
Described divalent iron salt is meant the salt that contains ferrous ion, as FeCl
2, FeSO
4, Fe (NO
3)
2Deng, but be not limited only to this.
Described alkali is meant that the pH value of its solution can be greater than 9 alkaline matter, as NaOH, and NH
3H
2O etc., but be not limited only to this.
Preparation method of the present invention is as follows:
(1) dispersion of hollow PS microballoon
With hollow PS microballoon ultra-sonic dispersion in dispersion medium, get sample a.
(2) Fe
3O
4Coat hollow PS microballoon
Ferric salt solution and divalent iron salt solution are placed reaction vessel, add sample a, and add alkali, the heated and stirred reaction adds dispersion agent then, is cooled to room temperature under stirring.
(3) aftertreatment:
The washing of sample, magnetic separates.
Among the above-mentioned preparation method, heated and stirred is reacted general sectional and is carried out, promptly add sample a after, heated 0.5-1.5 hour, be warming up to 50-65 ℃; Add alkaline solution, continue heat temperature raising to 90-100 ℃; Add dispersion agent then, be cooled to room temperature under stirring.
At present, have report (Wang Caifang, Xiong Weihao in hollow glass microbead surface coated with barium ferrite coating, cenosphere is the preparation and the research of the ferrite composite material of base, functional materials, 2004,35:536-538), but also do not have similarly of the present inventionly to coat Fe at hollow PS microsphere surface
3O
4, as the report of magnetorheological materials.
By the hollow magnetic composite particles that the present invention makes, density is little, and magnetic property is good, and the shear-stress height has good sedimentation stability.
Description of drawings
Fig. 1 is Fe
3O
4Particulate and PS tiny balloon have coated Fe
3O
4The sedimentation stability of composite particles in water relatively.
Fig. 2 is based on Fe
3O
4Particulate (content 8wt%) and PS tiny balloon have coated Fe
3O
4The apparent viscosity of the magnetic flow liquid (water is medium) of magnetic composite particle (composite particles content 8wt%) compares with the variation of magneticstrength.
Embodiment
Following examples are only for further specifying the present invention, are not violating under the purport of the present invention, and the present invention should be not limited to the content that following experimental example is specifically expressed.
Embodiment 1
Raw materials used proportioning is as follows:
Hollow PS microballoon (median size 2.5 μ m) 100 parts (weight)
5 parts of sodium lauryl sulphate (weight)
100 parts of iron trichlorides (weight)
50 parts of ferrous sulfates (weight)
50 parts in sodium hydroxide (weight)
The preparation of magnetic composite particle:
In above-mentioned component share ratio, hollow PS microballoon was disperseed 3 hours in deionized water for ultrasonic, get sample a.Iron trichloride and ferrous sulfate wiring solution-forming are added in the reaction vessel, add sample a, stirring heating 0.5-1 hour, be warming up to 60 ℃; NaOH is dissolved in the deionized water wiring solution-forming, joins that stirring reaction continued to be warming up to 90 ℃ after 1 hour in the reaction vessel, stop heating, add sodium lauryl sulphate, stir cooling down.To neutral, magnetic separates with deionized water wash.
The performance of magnetic composite particle:
(1) adopting the density gradient tube method to record this Hollow Compound particulate apparent density is 1.3g/cm
3, be about Fe
3O
4/ 4th of a density of particle.
(2) the hollow magnetic particle of the present invention's preparation has good sedimentation stability.Do not adding any additives, be under the situation of carrier fluid with water, when magnetic composite particle content during greater than 8wt% long-time the placement do not have sedimentation.Fig. 1 is the prepared composite particles content of the present invention when being 3wt%, with content be that 8wt%, particle diameter are the Fe about 50nm
3O
4The particles settling performance curve.The settling property of magnetic-particle represents with rate of descent V, V=a/ (a+b) * 100% wherein, and a is the volume of supernatant liquid, b is the volume of the muddy liquid of lower floor.The hollow magnetic particles settling stability of the present invention's preparation improves greatly.
(3) with Fe
3O
4Coat PS tiny balloon magnetic composite particle and Fe
3O
4Particulate is that medium is made magnetic flow liquid with water, adopt the NDJ-79 type rotational viscosimeter (dynamo-electric factory of Tongji University) of reequiping to study its magnetorheological performance, the result as shown in Figure 2, the magnetorheological performance of two kinds of magnetic flow liquids is comparatively approaching, null field viscosity is all lower, and along with the rising of magneticstrength, the apparent viscosity of magnetic flow liquid also sharply raises thereupon.
Embodiment 2
The proportioning of raw materials used weight share is as follows:
100 parts of hollow PS microballoons (median size 50nm)
0 part of sodium lauryl sulphate
Fe (NO
3)
350 parts
FeSO
420 parts
20 parts in sodium hydroxide
The preparation of magnetic composite particle:
In above-mentioned component share ratio, hollow PS microballoon was disperseed 2 hours in deionized water for ultrasonic, get sample a.With Fe (NO
3)
3And FeSO
4Wiring solution-forming adds in the reaction vessel, adds sample a, and stirring heating was warming up to 65 ℃ about 1 hour; NaOH is dissolved in the deionized water wiring solution-forming, joins that stirring reaction continued to be warming up to 95 ℃ after 1.5 hours in the reaction vessel, stop heating, stir cooling down.To neutral, magnetic separates with deionized water wash.The magnetic particle that obtains, its performance is similar as depicted in figs. 1 and 2.
The proportioning of raw materials used weight share is as follows:
Hollow PS microballoon (median size 20 μ m) 100 parts (weight)
50 parts of sodium lauryl sulphate (weight)
Fe
2(SO
4)
3400 parts (weight)
NH
3 H
2200 parts of O (weight)
The preparation of magnetic composite particle:
Hollow PS microballoon was disperseed 5 hours in deionized water for ultrasonic, get sample a.With Fe
2(SO
4)
3And FeCl
2Wiring solution-forming adds in the reaction vessel, adds sample a, stirring heating 1-1.5 hour, is warming up to 55 ℃; With NH
3H
2O is dissolved in the deionized water wiring solution-forming, joins that stirring reaction continued to be warming up to 100 ℃ after 1 hour in the reaction vessel, stops heating, adds sodium lauryl sulphate, stirs cooling down.To neutral, magnetic separates with deionized water wash.The magnetic particle that obtains, its performance is similar as depicted in figs. 1 and 2.
In the foregoing description, the parameter of each component raw material and consumption and preparation process only is the representative of choosing in order to describe the present invention.In fact a large amount of experiments show, in summary of the invention part institute restricted portion, all can obtain the magnetic composite particle with the similar performance of the foregoing description.
Claims (7)
1, a kind of hollow magnetic composite particle that is used for magnetic flow liquid is characterized in that coating one deck Fe by hollow PS microsphere surface
3O
4And the Hollow Compound magnetic particle of forming, its material component proportioning by weight is as follows:
100 parts of hollow PS microballoons
Dispersion agent 0-50 part
Trivalent iron salt 50-400 part
Divalent iron salt 20-200 part
Alkali 20-200 part
Wherein, hollow PS microballoon is that particle diameter is the hollow polystyrene microsphere of 20nm-20 μ m.
2. magnetic composite particle according to claim 1 is characterized in that described dispersion agent is organic and inorganic or compound tensio-active agent.
3. magnetic composite particle according to claim 1 is characterized in that described trivalent iron salt is FeCl
3, Fe (NO
3)
3Or Fe
2(SO
4)
3
4. magnetic composite particle according to claim 1 is characterized in that described divalent iron salt is FeCl
2, FeSO
4Or Fe (NO
3)
2
5. magnetic composite particle according to claim 1, the alkali described in it is characterized in that for the pH value of its solution greater than 9 alkaline matter.
6. the preparation method of a magnetic composite microsphere as claimed in claim 1 is characterized in that step is:
(1) hollow PS particulate disperses: with hollow PS microballoon ultra-sonic dispersion in dispersion medium, get sample a;
(2) Fe
3O
4Coat hollow PS microballoon: ferric salt solution and divalent iron salt solution are added in the reaction vessel, add sample a, and add alkaline solution, the heated and stirred reaction adds dispersion agent, is cooled to room temperature under stirring;
(3) aftertreatment: washing, magnetic separates.
7, preparation method according to claim 6 is characterized in that the heated and stirred reaction segmentation in the step (2) is carried out: after adding sample a, heat 0.5-1.5 hour, be warming up to 50-65 ℃ add alkaline solution after the continuation heat temperature raising to 90-100 ℃; Add dispersion agent again, be cooled to room temperature under stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100843189A CN1303136C (en) | 2004-11-18 | 2004-11-18 | Method for preparing hollow magnetic composite particulate for magnetic rheologic liquid by using polystyrene microsphere |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100843189A CN1303136C (en) | 2004-11-18 | 2004-11-18 | Method for preparing hollow magnetic composite particulate for magnetic rheologic liquid by using polystyrene microsphere |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1631949A true CN1631949A (en) | 2005-06-29 |
| CN1303136C CN1303136C (en) | 2007-03-07 |
Family
ID=34847321
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100843189A Expired - Fee Related CN1303136C (en) | 2004-11-18 | 2004-11-18 | Method for preparing hollow magnetic composite particulate for magnetic rheologic liquid by using polystyrene microsphere |
Country Status (1)
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|---|---|
| CN (1) | CN1303136C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657614A (en) * | 2013-12-26 | 2014-03-26 | 南京大学 | Polystyrene based magnetic nano ferroferric oxide arsenic removal composite and preparation method thereof |
| CN103730226A (en) * | 2014-01-06 | 2014-04-16 | 四川大学 | Hollow magnetic polymer composite microsphere, and preparation method and application thereof |
| CN105176495A (en) * | 2014-06-20 | 2015-12-23 | 南京理工大学 | Polystyrene oil absorption material and preparation method thereof |
| CN106589647A (en) * | 2016-12-20 | 2017-04-26 | 佛山市高明区塑料行业协会 | Novel modified polystyrene plastic with magnetic property |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1096487C (en) * | 1999-07-12 | 2002-12-18 | 武汉工业大学 | nm-class composite polyphenylamine-Fe2O3 material and its preparing process |
| CN1302831A (en) * | 2001-01-09 | 2001-07-11 | 上海博纳科技发展有限公司 | Magnetic high-molecular microsphere and its preparing process |
| CN1269769C (en) * | 2003-04-21 | 2006-08-16 | 中国科学院理化技术研究所 | Method for preparing composite submicron magnetic particles by coating organic microspheres with nano magnetic iron oxide particles |
| CN1493608A (en) * | 2003-09-02 | 2004-05-05 | 华东理工大学 | Nano-ferroferric oxide/polystyrene magnetic composite material and its preparation method |
-
2004
- 2004-11-18 CN CNB2004100843189A patent/CN1303136C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657614A (en) * | 2013-12-26 | 2014-03-26 | 南京大学 | Polystyrene based magnetic nano ferroferric oxide arsenic removal composite and preparation method thereof |
| CN103730226A (en) * | 2014-01-06 | 2014-04-16 | 四川大学 | Hollow magnetic polymer composite microsphere, and preparation method and application thereof |
| CN103730226B (en) * | 2014-01-06 | 2016-10-05 | 四川大学 | A kind of hollow magnetic polymer complex microsphere and preparation method and application |
| CN105176495A (en) * | 2014-06-20 | 2015-12-23 | 南京理工大学 | Polystyrene oil absorption material and preparation method thereof |
| CN106589647A (en) * | 2016-12-20 | 2017-04-26 | 佛山市高明区塑料行业协会 | Novel modified polystyrene plastic with magnetic property |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1303136C (en) | 2007-03-07 |
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Granted publication date: 20070307 Termination date: 20091218 |