CN103224831A - Electrorheological fluid and its preparation method - Google Patents
Electrorheological fluid and its preparation method Download PDFInfo
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- CN103224831A CN103224831A CN2013101282852A CN201310128285A CN103224831A CN 103224831 A CN103224831 A CN 103224831A CN 2013101282852 A CN2013101282852 A CN 2013101282852A CN 201310128285 A CN201310128285 A CN 201310128285A CN 103224831 A CN103224831 A CN 103224831A
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- ethylene glycol
- flower
- polyaniline
- iron
- electrorheological fluid
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- 239000012530 fluid Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229920000767 polyaniline Polymers 0.000 claims abstract description 64
- 239000000463 material Substances 0.000 claims abstract description 59
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 54
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002114 nanocomposite Substances 0.000 claims abstract description 49
- 239000002105 nanoparticle Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920002545 silicone oil Polymers 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 239000011246 composite particle Substances 0.000 claims abstract description 9
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 9
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 50
- DJNOZDZCBSYHGY-UHFFFAOYSA-N ethane-1,2-diol;iron Chemical compound [Fe].OCCO DJNOZDZCBSYHGY-UHFFFAOYSA-N 0.000 claims description 43
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 238000005253 cladding Methods 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000004160 Ammonium persulphate Substances 0.000 claims description 5
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 5
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000012692 Fe precursor Substances 0.000 abstract 2
- 229940031182 nanoparticles iron oxide Drugs 0.000 abstract 2
- 238000003756 stirring Methods 0.000 description 20
- 239000005457 ice water Substances 0.000 description 17
- 239000007788 liquid Substances 0.000 description 12
- 229910000859 α-Fe Inorganic materials 0.000 description 11
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 6
- 230000005684 electric field Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
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- 239000002243 precursor Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- 239000002322 conducting polymer Substances 0.000 description 2
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- 239000002086 nanomaterial Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000005408 paramagnetism Effects 0.000 description 2
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Images
Abstract
The invention relates to an electrorheological fluid material and its preparation method. The dispersed phase of the electrorheological fluid is a coated magnetic nano-composite particle compounded by flower-like ethylene glycol based iron or flower-like iron oxide nanoparticles and polyaniline nanoparticles growing thereon. The continuous phase is dimethyl silicone oil. The preparation process first employs a high temperature reflux method to prepare a flower-like ethylene glycol based iron precursor, which can directly undergo in-situ growth to obtain polyaniline so as to prepare the flower-like ethylene glycol based iron/polyaniline nanocomposite material; or the ethylene glycol based iron precursor can be calcined into iron oxide, which is then adopted as the substrate to undergo in-situ growth to obtain polyaniline nanoparticles, thereby preparing the monthly rose-like iron oxide/polyaniline nanocomposite material. The preparation process is simple, the raw materials are easily available, and the components and performance are easy to control. The ethylene glycol based iron or iron oxide nanoparticles in the composite particles has a flower structure, and after combination with polyaniline, the material performance is improved, so that the comprehensive performance, especially the electrorheological and magnetic properties of the material can be optimized.
Description
Technical field
The present invention relates to a kind of electro-rheologic fluid material and preparation method thereof, be specifically related to Nano composite granules electro-rheologic fluid material that a kind of flower-shaped ethylene glycol Fe nanometer particles or flower-shaped ferric oxide nano particles/polyaniline nano particle be composited and preparation method thereof.
Background technology
Electrorheological fluid (Electrorheological Fluids is called for short ERF) is a kind of important intelligent material, and it normally is scattered in the transformer oil of low-k and the suspension system that forms by the solid particulate of high-k, low conductivity.It has the quality of controlled change, and its yielding stress, Young's modulus change with the variation of extra electric field.Electrorheological fluid has great application prospect in fields such as vibration damping, mechanical transmission, automatic control, electromechanical integration, little drivings.But owing in use exist some shortcomings, as the particulate sedimentation, yielding stress is not high, and temperature effective is too poor to cause problems such as operation temperature area is narrow, has limited its widespread use.The electrorheological particle is a kind of polarizable particles, according to the dielectric depolarization model, solid particulate with high-k produces the intensive polarization after adding electric field, move, form fibrous chain, and then be arranged in the column chain, thereby under shearing action, have the performance of shearing resistance, be similar to solid character.Coating of particles can produce tremendous influence to the performance of electrorheological.The application of the maximum of micron particle electrorheological fluid hinders and comes from its relatively poor resistance to settling energy; And the nano particle electrorheological fluid is because its higher mechanics value and good resistance to settling can receive increasing concern.Therefore, the nanostructure of modifying on micrometer structure can access a kind of micrometer/nanometer clad structure material, can have the two-fold advantage of micron and nano particle simultaneously concurrently, the mechanics and the cutting performance of the electrorheological fluid of preparation also are greatly improved than micron particle electrorheological fluid.
Ferric oxide is a kind of important conductor oxidate material, its preparation is simple, and character with a lot of excellences, such as good weathering resistance and photostabilization, ultraviolet radiation absorption that magnetic performance is good and good and shielding character, thereby at coating, automobile finish, leather industry, electronic product, ink material, plastic prod, magnetic recording material, field such as catalyzer and biomedical engineering has extremely widely uses, so the controlled preparation and the physico-Chemical Properties thereof of ferric oxide nano structured material have very important scientific meaning, have obtained domestic and international numerous researchists' extensive concern.
Polyaniline (PANI) has excellent physical chemistry, unique mechanism of doping effect and good environmental stability, and advantage such as raw material is cheap and easy to get, synthesis technique is easy, become maximum class conducting polymer composite of numerous scientists study and the most possible conducting polymer of realizing industrial applications.
The surface modification technology of nanoparticle is an emerge science, and the finishing of nanoparticle has in recent years formed a research field, all has many problem values to inquire into from the method for modifying to the influence of modifying surface properties.The significance of studying in this field is have the more freedom degree that nanoparticle surface is carried out modification, not only can deeply be familiar with the basic physical influence of nanoparticle, and has enlarged the range of application of nanoparticle.By modification, can reach the purpose of four aspects: 1. improve or change the dispersiveness of nanoparticle, prevent the reunion of nanoparticle to nanoparticle surface; 2. improve the consistency between nanoparticle and other materials; 3. improve the nanoparticle surface activity; 4. make particle surface produce new physics, chemistry, mechanical property and new function.Modify and chemically modified according to having or not chemical reaction can be divided into surface physics between surface treatment agent and nanoparticle.
(J.APPL.POLYM.SCI.2012 DOI:10.1002/APP.37799) adopts the in-situ chemical oxidative polymerization method to prepare PANI-α-Fe to document
2O
3Nano composite material, and with methods such as XRD, FTIR, TGA and TEM it is characterized.Along with α-Fe
2O
3Adding, PANI-α-Fe
2O
3Electric conductivity reduce, this is because α-Fe
2O
3The conductive path that blocks PANI.The magnetization result shows α-Fe
2O
3Nanoparticle and PANI show ferromegnetism and paramagnetism respectively, yet, PANI-α-Fe
2O
3Nano composite granules then shows as superparamagnetism.Dynamically current potential studies show that, in moisture 3.5% NaCl solution, ties the control current transmission by forming P-N, has quite significant corrosion protection performance.
Goal of the invention and content
The flower-like nanometer composite particles electro-rheologic fluid material that the purpose of this invention is to provide a kind of novelty, its disperse phase is for being the long magnetic nanometer composite material thereon of matrix, polyaniline nano particle with flower-shaped ethylene glycol iron or ferric oxide, and external phase is dimethyl silicone oil.
The present invention also aims to provide a kind of method for preparing nanometer ethylene glycol iron or ferric oxide/polyaniline composite material, this method gained nano composite material is the cladding nanometer composite particles that is composited by flower-shaped ethylene glycol iron or ferric oxide nano particles and the load polyaniline nano particle on it, adopts high temperature reflux method and in-situ polymerization growth method to combine and prepares.Preparation technology is simple, and raw material is easy to get, and component and performance are easy to control, ethylene glycol iron or ferric oxide nanometer particle in the composite particles have flower-like structure, with improved the performance of material after polyaniline combines, thereby the over-all properties of this material, especially electrorheological and magnetic property are optimized.
Purpose of the present invention can be achieved through the following technical solutions:
Electrorheological fluid of the present invention, its disperse phase are the cladded type magnetic Nano composite granules that is composited by flower-shaped ethylene glycol Fe nanometer particles or flower-shaped ferric oxide nano particles and growth polyaniline nano particle thereon, and external phase is dimethyl silicone oil.
The preparation technology of above-mentioned electrorheological fluid may further comprise the steps:
(1) presoma ethylene glycol iron 0.2～0.25g is distributed in 80～100mL deionized water, adds 0.5～1mL monomer aniline, 1.0～1.5g ammonium persulfate initiator, initiated polymerization;
(2) reaction 1 hour after, use ethanol and water washing respectively after, the oven dry, just obtain flower-shaped ethylene glycol Fe nanometer particles/polyaniline nano particle cladding nanometer composite particles;
(3) this sample and dimethyl silicone oil are mixed with electrorheological fluid by a certain percentage.
The preparation process of above-mentioned electrorheological fluid can also comprise following several steps:
(1) with after the presoma ethylene glycol iron washing and drying, calcining is 2 hours in 500 ℃ of air atmospheres, makes ferric oxide;
(2) get ferric oxide 0.2～0.25g and be distributed in 80～100mL deionized water, add 0.5～1mL monomer aniline, 1.0～1.5g ammonium persulphate, initiated polymerization;
(3) reaction 1 hour after, use ethanol and water washing respectively after, the oven dry, just obtain flower-shaped ferric oxide nano particles/polyaniline nano particle cladding nanometer composite particles;
(4) this sample and methyl-silicone oil are mixed with electrorheological fluid by a certain percentage.
Wherein, described presoma ethylene glycol iron adopts following method preparation:
(1) under powerful agitation condition, with 1.0～1.5g iron trichloride, 2.5～3.0g urea, 7.0～7.5g Tetrabutyl amonium bromide are dissolved in the 180mL ethylene glycol;
(2) progressively be warming up to 190～210 ℃ under the reflux conditions;
(3) reacted 30 minutes under said temperature, stop heating, naturally cool to room temperature, after the removal supernatant liquor, products therefrom obtains ethylene glycol iron after washing through alcohol.
Specifically:
(1) weighing 1.0-1.5g FeCl in a 250mL there-necked flask
36H
2O, 2.5-3.0g urea, 7.0-7.5g Tetrabutyl amonium bromide and 150-180mL ethylene glycol at room temperature stirred 30 minutes, began heating under refluxing then and progressively were warming up to 190-210 ℃, reacted to stop heating after 30 minutes, remove supernatant liquor behind the naturally cooling, centrifugal, absolute ethanol washing three times is with the ethylene glycol iron oven dry that obtains after the washing, through 500 ℃ of calcinings of 2 hours, obtain ferric oxide (α-Fe again
2O
3).
(2) get 0.2-0.25g oxidation of precursor iron and add in the 80mL deionized water, add 0.5-1.0mL aniline again and mix, be designated as A liquid, 1.0-1.5g APS is dissolved in the 20mL deionized water as initiator, be designated as B liquid.Cooling added in the A liquid B liquid and vigorous stirring after 30 minutes in ice-water bath respectively, react after 1 hour, with washing with alcohol three times, dried with behind the deionized water centrifuge washing three times again, and grinding can get ferric oxide/polyaniline nano composite particles.
(3) with this sample and dimethyl silicone oil by a certain percentage (10-20wt%) be mixed with electrorheological fluid.
The preparation technology that the present invention adopts high temperature reflux method and in-situ polymerization growth method to combine.With iron trichloride (FeCl
36H
2O), urea (UR), Tetrabutyl amonium bromide (TBAB), ethylene glycol (EG), aniline (AN), ammonium persulphate (APS) etc. are raw material, cetyl trimethylammonium bromide (CTAB) is made tensio-active agent, preparation ethylene glycol iron or α-Fe
2O
3/ PANI Nano composite granules.The principle of preparation is to adopt the high temperature reflux method to prepare ethylene glycol iron presoma earlier, and flower-shaped ethylene glycol iron presoma both can grow polyaniline by direct in-situ, prepared flower-shaped ethylene glycol iron/polyaniline nano-composite material; Flower-shaped ethylene glycol iron presoma can be converted into ferric oxide through calcining again, and again as substrate, CTAB is a tensio-active agent, and growth in situ goes out polyaniline on the ferric oxide flower-like structure, prepares the flower-shaped ferric oxide/polyaniline nano-composite material of Chinese rose.
The present invention compared with prior art has following significant technological merit:
1, preparation method of the present invention adopts the preparation technology that high temperature reflux method and situ aggregation method combine, by α-Fe
2O
3Nanoparticle and polyaniline nano particle are compounded to form the cladding nanometer composite particles, and the Nano composite granules particle diameter of preparation is less, at flower-shaped α-Fe
2The last original position of O3 coats growth polyaniline nano particle, and this structure has special surface topography, and product has the performance different with flower-shaped precursor particle, presents paramagnetism, and has weak magnetic.
2, the electrorheological fluid by the preparation of this material and methyl-silicone oil had both had high mechanics value, and wide operation temperature area and resistance to settling have preferably reduced the cost of electrorheological fluid again, and reaction process is easy to control, and is nontoxic, and equipment is not had particular requirement.Having given full play to the speciality of inorganic/inorganic nano composite material, is a kind of er material of high comprehensive performance.Preparation technology is simple, and raw material is easy to get, and component and performance are easy to control, and product is nontoxic, is easy to suitability for industrialized production and widespread use.
Description of drawings
The stereoscan photograph of Fig. 1 precursor ethylene glycol iron.
The stereoscan photograph of Fig. 2 ferric oxide.
The uv-vis spectra of Fig. 3 ferric oxide.
The stereoscan photograph of Fig. 4 ethylene glycol iron/polyaniline nano-composite material.
The transmission electron microscope photo of Fig. 5 ethylene glycol iron/polyaniline nano-composite material.
The uv-vis spectra of Fig. 6 ethylene glycol iron/polyaniline nano-composite material.
The electrorheological test collection of illustrative plates of Fig. 7 ethylene glycol iron/polyaniline nano-composite material.
The stereoscan photograph of Fig. 8 ethylene glycol iron/polyaniline nano-composite material.
The stereoscan photograph of Fig. 9 ethylene glycol iron/polyaniline nano-composite material.
The stereoscan photograph of Figure 10 ethylene glycol iron/polyaniline nano-composite material.
The stereoscan photograph of Figure 11 ferric oxide/polyaniline nano-composite material.
The uv-vis spectra of Figure 12 ferric oxide/polyaniline nano-composite material.
The magnetic property collection of illustrative plates of Figure 13 ferric oxide/polyaniline nano-composite material.
The stereoscan photograph of Figure 14 ferric oxide/polyaniline nano-composite material.
The uv-vis spectra of Figure 15 ferric oxide/polyaniline nano-composite material.
The pure Fe of Figure 16
2O
3And the XRD figure of ferric oxide/polyaniline nano-composite material spectrum.
The stereoscan photograph of Figure 17 ferric oxide/polyaniline nano-composite material.
The stereoscan photograph of Figure 18 ferric oxide/polyaniline nano-composite material.
The electrorheological test collection of illustrative plates of Figure 19 ferric oxide/polyaniline nano-composite material.
Embodiment
Embodiment one (preparation 1. of presoma ethylene glycol iron):
Weighing 1.2g FeCl in a clean 250mL there-necked flask
36H
2The O particle, 2.7g urea powder, 7.2gTBAB particle and 180mL ethylene glycol, stir and begin heating after 30 minutes, and open condensation reflux unit, reached before 195 ℃ in temperature, can observe solution colour and become yellow by redness earlier, become yellow-green colour then, become dark green at last.Keep this temperature to continue reaction and stop heating after 30 minutes, behind the naturally cooling, remove supernatant liquor, centrifugal, products therefrom is used the ethanol centrifuge washing three times again, obtains presoma ethylene glycol iron.
The stereoscan photograph of this presoma ethylene glycol iron as shown in Figure 1.The size of the flower-shaped presoma that makes is assembled into spherical flower-like structure by nanometer sheet between 3-5 μ m, and has the hollow form structure, the size homogeneous.
Embodiment two (preparation 2. of presoma ethylene glycol iron):
Weighing 1.2g FeCl in a clean 250ml there-necked flask
36H
2The O particle, 2.7g urea powder, 7.2gTBAB particle and 180mL ethylene glycol, stir and begin heating after 30 minutes, and open condensation reflux unit, reached before 195 ℃ in temperature, can observe solution colour and become yellow by redness earlier, become yellow-green colour then, become dark green at last.Keep this temperature to continue reaction and stop heating after 30 minutes, behind the naturally cooling, remove supernatant liquor, centrifugal, with ethanol centrifuge washing three times, deionized water is given a baby a bath on the third day after its birth time again, is distributed in the deionized water stand-by.
Embodiment three (ferric oxide preparation 3.):
Weighing 1.2g FeCl in a clean 250mL there-necked flask
36H
2The O particle, 2.7g urea powder, 7.2gTBAB particle and 180mL ethylene glycol, stir and begin heating after 30 minutes, and open condensation reflux unit, reached before 195 ℃ in temperature, can observe solution colour and become yellow by redness earlier, become yellow-green colour then, become dark green at last.Keep this temperature to continue reaction and stop heating after 30 minutes, behind the naturally cooling, remove supernatant liquor, centrifugal, use ethanol centrifuge washing three times, after the drying, calcining is 2 hours in 500 ℃ of air atmospheres, ethylene glycol iron is converted into ferric oxide through calcining, and its floriform appearance is kept, and is dispersed in the deionized water stand-by after the calcining particle cooling.
The stereoscan photograph of this ferric oxide as shown in Figure 2, uv-vis spectra as shown in Figure 3, XRD figure is composed shown in accompanying drawing 16a curve.The XRD figure spectrum shows that the crystal formation of gained ferric oxide meets α-Fe
2O
3
Embodiment four:
Get the high tube of clean 250ml beaker and add 0.2-0.25g ethylene glycol iron presoma 1., 0.5mL aniline and 80mL ethanol, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS and 20mL deionized water, be designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and centrifugal back is cleaned four times with ethanol, washes then three times, oven dry obtains ethylene glycol iron/polyaniline nano-composite material.This sample and dimethyl silicone oil are mixed with electrorheological fluid by a certain percentage.
The stereoscan photograph of this ethylene glycol iron/polyaniline nano-composite material as shown in Figure 4, the transmission photo as shown in Figure 5, uv-vis spectra as shown in Figure 6, electrorheological is tested as shown in Figure 7, shows that products therefrom has higher electric rheological effect.During added electric field, fluid does not present the Newtonian fuid behavior; After applying DC electric field, the fluidic shear-stress significantly improves, and presents tangible electrorheological behavior.
Embodiment five:
Get the high tube of clean 250ml beaker and add 0.2-0.25g ethylene glycol iron presoma 1., 1mL aniline and 80mL ethanol, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS and 20mL deionized water, be designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and is centrifugal, uses washing with alcohol four times, after the washed with de-ionized water three times, oven dry obtains ethylene glycol iron/polyaniline nano-composite material.
The stereoscan photograph of this ethylene glycol iron/polyaniline nano-composite material as shown in Figure 8.
Embodiment six:
Get the high tube of clean 250mL beaker and add 0.2-0.25g ethylene glycol iron presoma 2., 0.5mL aniline and 80mL deionized water, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS and 20mL deionized water, be designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and centrifugal after product cleans four times with ethanol again, washes then three times, oven dry obtains ethylene glycol iron/polyaniline nano-composite material.
The stereoscan photograph of this ethylene glycol iron/polyaniline nano-composite material as shown in Figure 9.
Embodiment seven:
Get the high tube of clean 250mL beaker and add 0.2-0.25g ethylene glycol iron presoma 2., 1mL aniline and 80mL deionized water, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS and 20mL deionized water, be designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and is centrifugal, uses washing with alcohol four times, after the washed with de-ionized water three times, oven dry obtains ethylene glycol iron/polyaniline nano-composite material.
The stereoscan photograph of this ethylene glycol iron/polyaniline nano-composite material as shown in Figure 10.
Embodiment eight:
Get the high tube of clean 250mL beaker and add 0.2-0.25g ferric oxide presoma 3., 0.5mL aniline and 80mL deionized water, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS and 20mL deionized water, be designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and centrifugal back is cleaned four times with ethanol, washes then three times, oven dry obtains ferric oxide/polyaniline nano-composite material.
The stereoscan photograph of this ferric oxide/polyaniline nano-composite material as shown in Figure 11, uv-vis spectra as shown in Figure 12, XRD figure is composed shown in accompanying drawing 16b curve, the magnetic property collection of illustrative plates as shown in Figure 13.
Embodiment nine:
Get the high tube of clean 250mL beaker and add 0.2-0.25g ferric oxide presoma 3., 1mL aniline and 80mL deionized water, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS and 20mL deionized water, be designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and centrifugal after product cleans four times with ethanol, washes then three times, oven dry obtains ferric oxide/polyaniline nano-composite material.
The stereoscan photograph of this ferric oxide/polyaniline nano-composite material as shown in Figure 14, uv-vis spectra as shown in Figure 15, XRD figure is composed shown in accompanying drawing 16c curve.From the XRD figure spectrum as can be seen, ferric oxide/polyaniline nano-composite material had both also had the diffraction peak of ferric oxide, had the peak of polyaniline again, illustrated that we have successfully prepared ferric oxide/polyaniline nano-composite material.
Embodiment ten:
Get the high tube of clean 250mL beaker and add 0.2-0.25g ferric oxide presoma 3., 0.5mL aniline and 80mL deionized water, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS, 0.3gCTAB and 20mL deionized water are designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and centrifugal back is cleaned four times with ethanol, washes then three times, oven dry obtains ferric oxide/polyaniline nano-composite material.
The stereoscan photograph of this ferric oxide/polyaniline nano-composite material as shown in Figure 17.
Embodiment 11:
Get the high tube of clean 250mL beaker and add 0.2-0.25g ferric oxide presoma 3., 0.3mL aniline and 80mL deionized water, vigorous stirring is designated as A solution; Get clean 50mL small beaker, add 1.22gAPS, 0.3gCTAB and 20mL deionized water are designated as B liquid.Two beakers are placed on respectively in the ice-water bath, cool off half an hour, pour B solution in A solution vigorous stirring again, the ice-water bath reaction was taken out after one hour, and centrifugal back is cleaned four times with ethanol, washes then three times, oven dry obtains ferric oxide/polyaniline nano-composite material.This sample and dimethyl silicone oil are mixed with electrorheological fluid by a certain percentage.
The stereoscan photograph of this ferric oxide/polyaniline nano-composite material as shown in Figure 18, the test of its electrorheological is as shown in Figure 19.
Claims (4)
1. electrorheological fluid, it is characterized in that, the disperse phase of this electrorheological fluid is the cladded type magnetic Nano composite granules that is composited by flower-shaped ethylene glycol Fe nanometer particles or flower-shaped ferric oxide nano particles and growth polyaniline nano particle thereon, and external phase is dimethyl silicone oil.
2. electrorheological fluid according to claim 1 is characterized in that, the preparation technology of described electrorheological fluid may further comprise the steps:
(1) presoma ethylene glycol iron 0.2～0.25g is distributed in 80～100mL deionized water, adds 0.5～1mL monomer aniline, 1.0～1.5g ammonium persulfate initiator, initiated polymerization;
(2) reaction 1 hour after, use ethanol and water washing respectively after, the oven dry, just obtain flower-shaped ethylene glycol Fe nanometer particles/polyaniline cladding nanometer composite particles;
(3) this sample and dimethyl silicone oil are mixed with electrorheological fluid by a certain percentage.
3. electro-rheologic fluid material as claimed in claim 1 is characterized in that, the preparation process of described electrorheological fluid comprises following several steps:
(1) with after the presoma ethylene glycol iron washing and drying, calcining is 2 hours in 500 ℃ of air atmospheres, makes ferric oxide;
(2) get ferric oxide 0.2～0.25g and be distributed in 80～100mL deionized water, add 0.5～1mL monomer aniline, 1.0～1.5g ammonium persulphate, initiated polymerization;
(3) reaction 1 hour after, use ethanol and water washing respectively after, the oven dry, just obtain flower-shaped ferric oxide nano particles/polyaniline cladding nanometer composite particles;
(4) this sample and methyl-silicone oil are mixed with electrorheological fluid by a certain percentage.
4. as claim 2 and 3 described electro-rheologic fluid materials, it is characterized in that described presoma ethylene glycol iron adopts following method preparation:
(1) under powerful agitation condition, with 1.0～1.5g iron trichloride, 2.5～3.0g urea, 7.0～7.5g Tetrabutyl amonium bromide are dissolved in the 180mL ethylene glycol;
(2) progressively be warming up to 190～210 ℃ under the reflux conditions;
(3) reacted 30 minutes under said temperature, stop heating, naturally cool to room temperature, after the removal supernatant liquor, products therefrom obtains ethylene glycol iron through after the washing with alcohol.
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| CN103468348A (en) * | 2013-09-29 | 2013-12-25 | 陕西师范大学 | Spherical aluminum powder/polyaniline nuclear-shell structure composite electrorheological fluid |
| CN103756756A (en) * | 2014-01-17 | 2014-04-30 | 青岛科技大学 | LDH/polyaniline nano composite material electrorheological fluid and preparation method thereof |
| CN104232251A (en) * | 2014-08-28 | 2014-12-24 | 陕西师范大学 | Polyaniline composite electrorheological fluid |
| CN106010736A (en) * | 2016-05-30 | 2016-10-12 | 青岛科技大学 | Anisotropic titanium oxide/polyaniline nanocomposite electrorheological fluid and preparation method thereof |
| CN110129112A (en) * | 2019-06-05 | 2019-08-16 | 青岛科技大学 | A kind of flower-shaped molybdenum disulfide/titanium dioxide nanometer composite particles ER fluid and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468348A (en) * | 2013-09-29 | 2013-12-25 | 陕西师范大学 | Spherical aluminum powder/polyaniline nuclear-shell structure composite electrorheological fluid |
| CN103468348B (en) * | 2013-09-29 | 2015-08-19 | 陕西师范大学 | Spherical aluminum powder/polyaniline nuclear-shell structure composite electrorheological fluid |
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| CN106010736A (en) * | 2016-05-30 | 2016-10-12 | 青岛科技大学 | Anisotropic titanium oxide/polyaniline nanocomposite electrorheological fluid and preparation method thereof |
| CN110129112A (en) * | 2019-06-05 | 2019-08-16 | 青岛科技大学 | A kind of flower-shaped molybdenum disulfide/titanium dioxide nanometer composite particles ER fluid and preparation method thereof |
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