CN100436572C - Production of organic sol variable current fluid of nanometer titanium oxide - Google Patents
Production of organic sol variable current fluid of nanometer titanium oxide Download PDFInfo
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- CN100436572C CN100436572C CNB2005100961052A CN200510096105A CN100436572C CN 100436572 C CN100436572 C CN 100436572C CN B2005100961052 A CNB2005100961052 A CN B2005100961052A CN 200510096105 A CN200510096105 A CN 200510096105A CN 100436572 C CN100436572 C CN 100436572C
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Abstract
Production of nano-titanium oxide organic sol electrorheo-liquid is carried out by taking titanate tetrabutyl ester as hydrolytic precursor, controlling reactive condition, preparing transparent titanium oxide hydrosol, extracting by sol and organic solvent, separating and evaporating to obtain the final product. It's cheap, convenient and has no environmental pollution.
Description
Technical field
The present invention relates to a kind of preparation method of electrorheological fluid, particularly a kind of preparation method of organic sol variable current fluid of nanometer titanium oxide.
Background technology
Electrorheological fluid generally is that the molecule by high-k is dispersed in the suspension system that forms in the insulating liquid of low-k.But since its moment under effect of electric field realize quick, reversible, the adjustable transformation between liquid-solid, electrorheological fluid becomes very potential SMART FLUID in a kind of important artificial intelligence material and the efficient electromechanical integration, and it is considered to make the material that revolution takes place such as many departments such as the vehicles, hydraulic efficiency installation, machinery manufacturing industry, sensor technology.In order to reach practical requirement, electrorheological fluid at first should have high as far as possible yielding stress, and secondly it also should have a lot of character that are fit to actually operatings, and is low as leakage current density, temperature stability good, null field viscosity is low, antisolvent precipitation excellent in stability etc.Electrorheological fluid can be divided into biphase current and become liquid and single-phase electricity rheology liquid.The former is dispersed in the insulating liquid by solid particulate and forms, and the latter is meant the liquid crystalline polymers electrorheological fluid.Biphase current becomes material and comprises inorganic materials, organic and polymer materials and organic/inorganic composite material.Though the inorganic materials high yield stress, because particulate density is big, hardness is big, makes the particulate suspension stability poor, big to the wearing and tearing of device.Organic polymer material preparation condition complexity, toxicity are big, and because agglomeration of particles is strong, cause dispersed relatively poor, shear-stress is low.Though organic/inorganic composite material makes the over-all properties of electrorheological fluid, as: shear-stress, leakage current density have greatly improved, problems such as the particulate suspension stability is poor, grain pattern destructible that it still exists.Investigators developed nanometer electric current material afterwards, and the stability of suspension and static mechanical value are improved greatly, became liquid but still belong to biphase current, and preparation particulate link can produce the particulate reunion and grow up, and powder is to the problems such as pollution of environment.There is not biphase consistency suspension stability problem in liquid crystalline polymers owing to be a phase, has overcome biphase current and has become some shortcomings of liquid, but had problems such as the ER effect is weak, the time of response is slow, zero electric field viscosity height.Therefore open up new preparation method, the er material of looking for high comprehensive performance becomes the focus in this field.Our design utilizes the extraction of water-sol organosol directly to produce SDBS modified Nano titanium oxide organic sol variable current fluid, it has good mechanics value, very low leakage current density, especially the antisolvent precipitation performance is good, do not precipitate, and in preparation process, saved the loaded down with trivial details operations such as preparation of suction filtration, drying, grinding and the electrorheological fluid of powder, and avoided the environmental pollution of powder, be a kind of environment-friendly type electrorheological fluid preparation method who has practical value.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of modified Nano titanium oxide organic sol variable current fluid of antisolvent precipitation performance excellence.This preparation method is because of need not this step of powder preparing, directly produce target current and become the liquid sample, thereby having saved loaded down with trivial details powder preparing operation, eliminated in the powder preparing process the pollution of environment, is a kind of environment-friendly type electrorheological fluid preparation method who has practical value.
Technical scheme provided by the invention is: a kind of preparation method of organic sol variable current fluid of nanometer titanium oxide, the disperse phase that it is characterized in that this electrorheological fluid is a Sodium dodecylbenzene sulfonate surface modification TiOx nano particle, external phase is dimethyl silicone oil, preparing this electrorheological fluid selects for use tetrabutyl titanate to make the hydrolysis presoma, the control reaction conditions, produce the transparent nano titanium oxide water-sol earlier, directly produce organic sol variable current fluid of nanometer titanium oxide through the operation of gelling, organic solvent extraction, separation and evaporation.
The modified Nano titanium oxide organic sol variable current fluid that the present invention makes has extremely excellent resistance to settling, good mechanical performance.And the loaded down with trivial details operations such as preparation of suction filtration, drying, grinding and the electrorheological fluid of powder in preparation process, have been saved, avoided the environmental pollution of powder, reaction is carried out at normal temperatures, and preparation condition is simple, for being a kind of brand-new and environment-friendly type electrorheological fluid preparation method that have practical value.
The concrete technological specification of preparation each flow process of organic sol variable current fluid of nanometer titanium oxide is as follows:
1, select for use tetrabutyl titanate to make the hydrolysis presoma, Sodium dodecylbenzene sulfonate is done jelling agent and organic surface modifying agent, and 6M hydrochloric acid is done hydrolysis inhibitor.
2, measure the 50ml deionized water, add the 6mol/L hydrochloric acid of 3.5ml～5ml, be made into acidic solution, pH is 0.5～1.5,7.5g (making concentration in 0.2mol/L～0.6mol/L) tetrabutyl titanate is slowly splashed into above-mentioned acidic solution, and normal-temperature reaction got light blue transparent water colloidal sol in 5 hours.
3, the 6mol/L hydrochloric acid with 0.64g～1.2g (mass percent concentration is 0.8%～1.5%) Sodium dodecylbenzene sulfonate and 2ml adds in the 30ml deionized water, after the dissolving fully, splashes into above-mentioned transparent water colloidal sol, stirs and gets white emulsion after 3 hours.
4, make its back (organic extractant is 1～3 with water-sol volume ratio) that is uniformly dispersed with stirring in 5ml (making the silicone oil mass percent concentration in 3%～10%) the dimethyl silicone oil adding 150ml sherwood oil, it is added white emulsion in 3, and vigorous stirring made in the petroleum ether solution that nano-titanium oxide replaces dimethyl silicone oil in 5 hours.
5, pour gained liquid in 4 in separating funnel standing demix, the upper strata is the oyster white organosol, lower floor is the aqueous solution, isolate lower layer of water colloidal sol, with the upper strata organosol rotary evaporation that reduces pressure at normal temperatures, to evaporate then residuum in vacuum drying oven 80 ℃ dry 3 hours down, obtain organic sol variable current fluid of nanometer titanium oxide, grain graininess is 7nm～100nm.
Description of drawings
The shear-stress of Fig. 1 organic sol variable current fluid of nanometer titanium oxide and the relation of shearing rate.
The oil-water mixture layering situation photo that Fig. 2 embodiment one, embodiment two, embodiment five produce.
Embodiment
Used chemical feedstocks is except that butyl (tetra) titanate is chemical pure, and all the other are analytical pure entirely, and deionized water is the laboratory self-control.
Below in conjunction with embodiment and description of drawings the present invention is described in further detail:
Embodiment one
Select for use tetrabutyl titanate to make the hydrolysis presoma, Sodium dodecylbenzene sulfonate is done jelling agent and organic surface modifying agent, and 6M hydrochloric acid is done hydrolysis inhibitor.Measure the 50ml deionized water, add the 6mol/L hydrochloric acid of 3.5ml～5ml, be made into acidic solution.The 7.5g tetrabutyl titanate is splashed into above-mentioned acidic solution slowly, and normal-temperature reaction got light blue transparent water colloidal sol in 5 hours.6mol/L hydrochloric acid with 0.64g～1.2g Sodium dodecylbenzene sulfonate and 2ml adds in the 30ml deionized water in addition, after the dissolving, splashes in the above-mentioned transparent water colloidal sol fully, stirs and gets white emulsion after 3 hours.Again with after stirring is uniformly dispersed it in the 5ml dimethyl silicone oil adding 150ml sherwood oil, the petroleum ether solution of dimethyl silicone oil is added in the above-mentioned white emulsion, vigorous stirring is poured liquid in separating funnel standing demix after making the nano-titanium oxide displacement in 5 hours in sherwood oil, the upper strata is the oyster white organosol, lower floor is the aqueous solution, isolate lower aqueous solution, with the upper strata organosol rotary evaporation that reduces pressure at normal temperatures, to evaporate then residuum in vacuum drying oven 80 ℃ dry 3 hours down, obtain organic sol variable current fluid of nanometer titanium oxide.The relation of its shear-stress and shearing rate as shown in Figure 1, its oil-water mixture layering situation is as shown in Figure 2.
Embodiment two
Select for use tetrabutyl titanate to make the hydrolysis presoma, Sodium dodecylbenzene sulfonate is done jelling agent and organic surface modifying agent, and 6M hydrochloric acid is done hydrolysis inhibitor.Measure the 50ml deionized water, add 6mol/L hydrochloric acid and the 1ml methane amide of 3.5ml～5ml, be made into acidic solution.The 7.5g tetrabutyl titanate is splashed into above-mentioned acidic solution slowly, and normal-temperature reaction got white emulsion in 5 hours.The 6mol/L hydrochloric acid of 0.64g～1.2g Sodium dodecylbenzene sulfonate and 2ml is added in the 30ml deionized water, after the dissolving fully, splash into above-mentioned white emulsion stirring and got white turbid liquid in 3 hours.After stirring is uniformly dispersed it in the 5ml dimethyl silicone oil adding 150ml sherwood oil, mixing solutions is added white turbid liquid, vigorous stirring after 5 hours is poured liquid into standing demix in the separating funnel, nano-titanium oxide fails to replace in the petroleum ether solution, the upper strata still is transparent petroleum ether solution, and lower floor is the oyster white water-sol.Its oil-water mixture layering situation as shown in Figure 2.
Embodiment three
Select for use tetrabutyl titanate to make the hydrolysis presoma, Sodium dodecylbenzene sulfonate is done jelling agent and organic surface modifying agent, and 6M hydrochloric acid is done hydrolysis inhibitor.Measure the 50ml deionized water, add 6mol/L hydrochloric acid and the 0.9g chromium nitrate of 3.5ml～5ml, be made into acidic solution.The 7.5g tetrabutyl titanate is splashed into above-mentioned acidic solution slowly, and normal-temperature reaction got green emulsion in 5 hours.The 6mol/L hydrochloric acid of 0.64g～1.2g Sodium dodecylbenzene sulfonate and 2ml is added in the 30ml deionized water, after the dissolving fully, splash into above-mentioned green emulsion stirring and got green turbid liquid in 3 hours.After stirring is uniformly dispersed it in the 5ml dimethyl silicone oil adding 150ml sherwood oil, mixing solutions is added green turbid liquid, vigorous stirring after 5 hours is poured liquid into standing demix in the separating funnel, there is not extract in the organic solution of upper strata, have only small quantities of particles in lower floor's light green aqueous solution, bottom has a large amount of white titanium oxide precipitations.
Embodiment four
Select for use tetrabutyl titanate to make the hydrolysis presoma, oleic acid is done jelling agent and organic surface modifying agent, and 6M hydrochloric acid is done hydrolysis inhibitor.Measure the 50ml deionized water, add the 6mol/L hydrochloric acid of 3.5ml～5ml, be made into acidic solution.The 7.5g tetrabutyl titanate is splashed into above-mentioned acidic solution slowly, and normal-temperature reaction got light blue transparent water colloidal sol in 5 hours.6mol/L hydrochloric acid with 0.5g～1g oleic acid and 2ml adds in the 30ml deionized water in addition, after the dissolving, splashes in the above-mentioned transparent water colloidal sol fully, stirs and gets white emulsion after 3 hours.Again with after stirring is uniformly dispersed it in the 5ml dimethyl silicone oil adding 150ml sherwood oil, the petroleum ether solution of dimethyl silicone oil is added in the above-mentioned white emulsion, vigorous stirring 24 as a child after, nano-titanium oxide fails to replace in the petroleum ether solution, the upper strata still is transparent petroleum ether solution, and lower floor is the oyster white water-sol.
Embodiment five
Select for use tetrabutyl titanate to make the hydrolysis presoma, cetyl trimethylammonium bromide is done jelling agent and organic surface modifying agent, and 6M hydrochloric acid is done hydrolysis inhibitor.Measure the 50ml deionized water, add the 6mol/L hydrochloric acid of 3.5ml～5ml, be made into acidic solution.The 7.5g tetrabutyl titanate is splashed into above-mentioned acidic solution slowly, and normal-temperature reaction got light blue transparent water colloidal sol in 5 hours.6mol/L hydrochloric acid with 0.5g～1g cetyl trimethylammonium bromide and 2ml adds in the 30ml deionized water in addition, after the dissolving, splashes in the above-mentioned transparent water colloidal sol fully, stirs and gets white emulsion after 3 hours.Again with after stirring is uniformly dispersed it in the 5ml dimethyl silicone oil adding 150ml sherwood oil, the petroleum ether solution of dimethyl silicone oil is added in the above-mentioned white emulsion, vigorous stirring was poured liquid in separating funnel standing demix after 5 hours, did not occur two phase stratification after 10 hours.Its oil-water mixture layering situation as shown in Figure 2.
Embodiment six
Light blue transparent water colloidal sol decompression rotary evaporations under 50 ℃ with normal-temperature reaction among the embodiment one obtained in 5 hours obtain white titanium oxide powder.Should the white titanium oxide powder under infrared lamp after dry 3 hours, be scattered in and be made into electrorheological fluid in the dimethyl silicone oil, particles dispersed is fine.
Claims (7)
1. the preparation method of an organic sol variable current fluid of nanometer titanium oxide, the disperse phase that it is characterized in that this electrorheological fluid is a Sodium dodecylbenzene sulfonate surface modification TiOx nano particle, external phase is dimethyl silicone oil, preparing this electrorheological fluid selects for use tetrabutyl titanate to make the hydrolysis presoma, the control reaction conditions is produced titanium oxide transparent water colloidal sol, use Sodium dodecylbenzene sulfonate to do jelling agent and surface-modifying agent, directly produce organic sol variable current fluid of nanometer titanium oxide through the operation of gelling, organic solvent extraction, separation and evaporation.
2. according to the preparation method of the described a kind of organic sol variable current fluid of nanometer titanium oxide of claim 1, it is characterized in that the reaction conditions of producing the titanium oxide water-sol is:
(1) concentration of tetrabutyl titanate is 0.2mol/L～0.6mol/L;
(2) pH value of solution is 0.5～1.5;
(3) temperature is 15 ℃～35 ℃.
3. according to the preparation method of the described a kind of organic sol variable current fluid of nanometer titanium oxide of claim 1, it is characterized in that selecting for use Sodium dodecylbenzene sulfonate to do jelling agent and surface-modifying agent, mass percent concentration is 0.8%～1.5%.
4. according to the preparation method of the described a kind of organic sol variable current fluid of nanometer titanium oxide of claim 1, it is characterized in that organic extractant selects the petroleum ether solution that contains dimethyl silicone oil for use, the mass percent concentration of silicone oil is 3%～10%.
5. according to the preparation method of the described a kind of organic sol variable current fluid of nanometer titanium oxide of claim 1, the volume ratio that it is characterized in that the organic extractant and the water-sol is 1～3.
6. according to the preparation method of the described a kind of organic sol variable current fluid of nanometer titanium oxide of claim 1, it is characterized in that after organic solvent extraction separates, organosol is the rotary evaporation that reduces pressure at normal temperatures, to evaporate then residuum in vacuum drying oven 70 ℃～100 ℃ dry 2～5 hours down, obtain organic sol variable current fluid of nanometer titanium oxide, the disperse phase nano-titanium oxide is an amorphous state, and granularity is 7nm～100nm.
7. according to the preparation method of the described a kind of organic sol variable current fluid of nanometer titanium oxide of claim 1, it is characterized in that preparation technology's method may further comprise the steps:
(1) measure the 50ml deionized water, add the 6mol/L hydrochloric acid of 3.5ml～5ml, be made into acidic solution, the 7.5g tetrabutyl titanate is slowly splashed into above-mentioned acidic solution, room temperature reaction got light blue transparent water colloidal sol in 5 hours;
(2) the 6mol/L hydrochloric acid with 0.64g～1.2g Sodium dodecylbenzene sulfonate and 2ml adds in the 30ml deionized water, after the dissolving fully, splashes into above-mentioned transparent water colloidal sol, stirs and gets white emulsion after 3 hours;
(3) the 5ml dimethyl silicone oil is added after the 150ml petroleum ether and stirring is uniformly dispersed, with the white emulsion in its adding (2), vigorous stirring made in the petroleum ether solution that nano-titanium oxide replaces dimethyl silicone oil in 5 hours;
(4) pour gained liquid in (3) in separating funnel standing demix, the upper strata is the oyster white organosol, lower floor is the aqueous solution, isolate lower layer of water colloidal sol, with the upper strata organosol rotary evaporation that at room temperature reduces pressure, then with residuum in loft drier 80 ℃ dry 3 hours down, obtain organic sol variable current fluid of nanometer titanium oxide.
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| CN104130838A (en) * | 2014-07-04 | 2014-11-05 | 中国兵器科学研究院宁波分院 | Complex formulation electrorheological fluid and preparation method thereof |
| CN106730981B (en) * | 2016-12-16 | 2019-04-26 | 武汉理工力强能源有限公司 | A kind of method of extensive efficiently purifying lithium metal particle |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002121578A (en) * | 2000-10-18 | 2002-04-26 | Neos Co Ltd | Magnetic viscous fluid and usage thereof |
| CN1539933A (en) * | 2003-04-22 | 2004-10-27 | 西北工业大学 | Current variable fluid material of Nano composite granules between kaoline and oxide of titanium, and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002121578A (en) * | 2000-10-18 | 2002-04-26 | Neos Co Ltd | Magnetic viscous fluid and usage thereof |
| CN1539933A (en) * | 2003-04-22 | 2004-10-27 | 西北工业大学 | Current variable fluid material of Nano composite granules between kaoline and oxide of titanium, and preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 纳米TiO2 颗粒的表面改性研究进展. 鄢程，李竟先，潘志东.陶瓷学报，第VOL.23卷第NO.1期. 2002 |
| 纳米TiO2 颗粒的表面改性研究进展. 鄢程，李竟先，潘志东.陶瓷学报，第VOL.23卷第NO.1期. 2002 * |
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