CN100412177C - Blended titanium dioxide electric rheological liquid and its preparing method - Google Patents
Blended titanium dioxide electric rheological liquid and its preparing method Download PDFInfo
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- CN100412177C CN100412177C CNB2006101127931A CN200610112793A CN100412177C CN 100412177 C CN100412177 C CN 100412177C CN B2006101127931 A CNB2006101127931 A CN B2006101127931A CN 200610112793 A CN200610112793 A CN 200610112793A CN 100412177 C CN100412177 C CN 100412177C
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Abstract
The blended titania electric rheological liquid consists of dispersed phase of micron or nanometer level blended titania particle and dispersing medium of methyl silicone oil in the volume ratio of 0.05-0.5. During the preparation process, blended titania particle is first prepared via adding polar amide compound selected from formamide, acetamide, amido thiourea, etc. in 1-30 wt% and then mixed with methyl silicone oil. Blending strong polar amide compound into titania can raise the yield strength of the electric rheological liquid. In addition, the electric rheological liquid has stable structure, small current density, less settling, no pollution, low cost, simple preparation process and high yield.
Description
Technical field
The present invention relates to a kind of electro-rheologic fluid material and preparation method thereof, specifically relate to a kind of blended titanium dioxide electric rheological liquid material and preparation method thereof.
Background technology
Electrorheological fluid is the complex fluid that is mixed by nanometer to the dielectric grain and the insulating liquid of micro-meter scale.Its " electric rheological effect " is meant that its fluidic viscosity changes with external electric field.When not having External Electrical Field, electrorheological fluid is liquid state usually, and its viscosity is similar with oil.When External Electrical Field during in electrorheological fluid, its apparent viscosity becomes big with the increase in outfield.When external electric field is enough big (greater than 1000V/mm), electrorheological fluid can change the class solid matter that intensity can be compared with general solid into, and its shearing resistance increases with strength of electric field.This " liquid-solid " changes is reversible, and its fringe time is generally in the millisecond magnitude.Be the adjustable intelligent material of unique soft or hard degree, thereby have extensive and important use value.Can be used for clutch coupling, vibroshock, stopper, electromechanical coupling control etc.USDOE is thought " electrorheological fluid will make industry and some departments of technology revolutionary change occur " in May, 1992 " electrorheological fluid assessment report ".Although electric rheological effect just was found before 50 years, start research boom after the eighties in last century again, electrorheological fluid is not widely used, and this mainly is because the electrorheological fluid shearing resistance is low, can only reach about 10 kPas, can not satisfy the requirement that engineering is used.
As in Chinese patent application: disclosed in 99115944.6,00105602.6,00113752.2,02114516.4,02114691.8, China has carried out a large amount of work aspect electric titania rheological liquid.But the electrorheological fluid of titanium dioxide that makes with these methods or cladding titanium dioxide and methyl-silicone oil preparation, shearing resistance is too low, and its shearing resistance＜10kPa under the 3000V/mm electric field action still can not satisfy the requirement that engineering is used.
Summary of the invention
It is too low to the objective of the invention is to overcome existing electric titania rheological liquid shearing resistance, can not satisfy the defective of engineering application requiring, thereby provide a kind of shearing resistance height, Stability Analysis of Structures, current density little, pollution-free, and the cost of material is low, the simple blended titanium dioxide electric rheological liquid of preparation technology.
Another object of the present invention is to provide the preparation method of above-mentioned blended titanium dioxide electric rheological liquid.
The objective of the invention is to realize by the following technical solutions:
Blended titanium dioxide electric rheological liquid provided by the invention, its disperse phase are the admixture titanium dioxide granule of micron to nano-scale, and dispersion medium is a methyl-silicone oil, and the volume ratio of disperse phase and dispersion medium is 5～50%;
Described admixture titanium dioxide granule prepares for using sol gel reaction, specifically comprises the steps:
1) preparation of three kinds of components:
The titanium alkoxide is mixed with dehydrated alcohol 1: 20 in molar ratio～25, and the pH value of dripping hydrochloric acid or nitric acid regulator solution is 2～3, mixes, and obtains first component;
Deionized water and dehydrated alcohol 1: 2 in molar ratio～3 are mixed, obtain second component;
The amides polar compound is dissolved in the deionized water, is mixed with 8～30mol/l aqueous solution, obtain the 3rd component;
2) three components mix:
Second component after adding first component under the magnetic agitation or under the ultrasound condition, is added the 3rd component, add the back and continue stirring or ultrasonic up to forming gel, then room temperature ageing 5～100 hours; The mixed volume ratio of three kinds of components is first component: second component: the 3rd component=20～25: 18～25: 1;
3) preparation admixture titanium dioxide granule: with step 2) through aged gel 20～120 ℃ of vacuum-dryings 8～12 hours, the product that obtains is used deionized water and washing with alcohol repeatedly, the percentage composition of doping amides polar compound is 1～30wt% in the admixture titanium dioxide granule, the powder that obtains after the centrifugation in air in 50 ℃ of dryings more than 48 hours, 120 ℃ of dryings 3 hours, obtain the admixture titanium dioxide granule of micron again to nano-scale.
Described amides polar compound is one or more the mixture that is selected from methane amide, ethanamide, thiosemicarbazide, TCH, urea, thiocarbamide, the or derivatives thereof.
The viscosity of described methyl-silicone oil is 5～500mm
2/ s.
The invention provides a kind of preparation method of above-mentioned blended titanium dioxide electric rheological liquid, it prepares the admixture titanium dioxide granule for using sol gel reaction earlier, mixes with methyl-silicone oil again, specifically comprises the steps:
1) preparation of three kinds of components:
The titanium alkoxide is mixed with dehydrated alcohol 1: 20 in molar ratio～25, and the pH value of dripping hydrochloric acid or nitric acid regulator solution is 2～3, mixes, and obtains first component; Described titanium alkoxide is tetrabutyl titanate, tetraethyl titanate or titanium isopropylate;
Deionized water and dehydrated alcohol 1: 2 in molar ratio～3 are mixed, obtain second component;
Also can add hydrolysis reaction and the condensation reaction rate that diethanolamine is regulated the titanium alkoxide in second component, the mol ratio of diethanolamine and titanium alkoxide is 1: 8～10.
The amides polar compound is dissolved in the deionized water, is mixed with 8～30mol/l aqueous solution, obtain the 3rd component; Described amides polar compound is one or more the mixture that is selected from methane amide, ethanamide, thiosemicarbazide, TCH, urea, thiocarbamide, the or derivatives thereof.
2) three components mix:
Second component after adding first component under the magnetic agitation or under the ultrasound condition, is added the 3rd component, add the back and continue stirring or ultrasonic, made gel aging in 5～100 hours in the room temperature ageing then up to forming gel; The mixed volume ratio of three kinds of components is first component: second component: the 3rd component=20～25: 18～25: 1;
3) preparation admixture titanium dioxide granule: with step 2) through aged gel 20～120 ℃ of vacuum-dryings 8～48 hours, the product that obtains is used deionized water and washing with alcohol repeatedly, and it is 1～30wt% that control deionized water and alcoholic acid amount and washing times make the percentage composition of adulterated amides polar compound in the admixture titanium dioxide granule; The powder that obtains after the centrifugation in 50 ℃ of dryings more than 48 hours, 120 ℃ of dryings 3 hours, promptly obtains the admixture titanium dioxide granule of micron to nano-scale again in air;
4) preparation electrorheological fluid: admixture titanium dioxide granule and viscosity that step 3) is obtained are 5～500mm
2The methyl-silicone oil of/s 5～50% mixes by volume, obtains blended titanium dioxide electric rheological liquid of the present invention.
Blended titanium dioxide electric rheological liquid provided by the invention, be to adopt sol-gel method, by the strong polar amides of admixture in titanium dioxide or derivatives thereof molecule, form the admixture titanium dioxide granule of micron or nanoscale, formulated with methyl-silicone oil again, it has effectively improved the electrorheological fluid yield strength of titanium dioxide, admixture TiO
2With methyl-silicone oil by volume mark be mixed with 30% electrorheological fluid, during extra electric field 3000V/mm, yield strength can reach more than the 160kPa.And the Stability Analysis of Structures of blended titanium dioxide electric rheological liquid provided by the invention, current density is little, and free settling is not pollution-free, and the cost of material is low, and preparation technology is simple, the productive rate height.
Embodiment
Embodiment 1,
Tetrabutyl titanate and dehydrated alcohol were mixed in 1: 20 in molar ratio, add the pH value to 2 of hydrochloric acid conditioning solution, mix, obtain first component; Deionized water and dehydrated alcohol were mixed in 1: 2 in molar ratio, obtain second component; According to admixture amount difference, ethanamide, thiosemicarbazide, urea, thiocarbamide are dissolved in the deionized water, be mixed with the aqueous solution of 8～30mol/l, obtain the 3rd component.After second component under agitation added first component, add the 3rd component, three kinds of component add-ons 20: 20: 1 by volume.Adding the back that finishes continues to stir up to forming water white gel, then room temperature ageing 24 hours.
With this through aged gel 100 ℃ of vacuum-dryings 12 hours, obtain powder, with deionized water and washing with alcohol repeatedly, the admixture amount of amides polar compound is 1～30wt% in titanium dioxide granule, the powder that obtains after the centrifugation in box-type furnace in 50 ℃ of dryings more than 48 hours, 120 ℃ of dryings 3 hours, promptly obtain the admixture titanium dioxide granule of micron again to nanoscale.
With this admixture titanium dioxide granule and 10mm
2/ S methyl-silicone oil 30% mixes by volume, obtains blended titanium dioxide electric rheological liquid of the present invention.The yield strength and the current density of different admixture amount electric titania rheological liquids are as shown in table 1 under extra electric field 3kV/mm condition.
Table 1 prepares blended titanium dioxide electric rheological liquid performance index (volume fraction 30%) with tetrabutyl titanate
Embodiment 2,
Tetraethyl titanate and dehydrated alcohol were mixed in 1: 25 in molar ratio, add the pH value to 2 of nitric acid regulator solution, mix, obtain first component; Deionized water and dehydrated alcohol were mixed in 1: 3 in molar ratio, obtain second component; According to admixture amount difference, ethanamide, thiosemicarbazide, urea, thiocarbamide are dissolved in the deionized water, be mixed with the aqueous solution of 8～30mol/l, obtain the 3rd component.After second component under agitation added first component, add the 3rd component, three kinds of component add-ons 25: 25: 1 by volume.Adding the back that finishes continues to stir up to forming water white gel, then room temperature ageing 48 hours.
With this through aged gel 120 ℃ of vacuum-dryings 8 hours, obtain powder, with deionized water and washing with alcohol repeatedly, the admixture amount of amides polar compound is 1～30wt% in titanium dioxide granule, the powder that obtains after the centrifugation in box-type furnace in 50 ℃ of dryings more than 48 hours, 120 ℃ of dryings 3 hours, promptly obtain the admixture titanium dioxide granule of micron～nanoscale again.
With this admixture titanium dioxide granule and 50mm
2/ s methyl-silicone oil 30% mixes by volume, obtains blended titanium dioxide electric rheological liquid of the present invention.The yield strength and the current density of different admixture amount electric titania rheological liquids are as shown in table 1 under extra electric field 3kV/mm condition.
Table 2 prepares blended titanium dioxide electric rheological liquid performance index (volume fraction 30%) with tetraethyl titanate
Embodiment 3,
Titanium isopropylate and dehydrated alcohol were mixed in 1: 23 in molar ratio, add the pH value to 2.5 of hydrochloric acid conditioning solution, mix, obtain first component; Deionized water and dehydrated alcohol were mixed in 1: 3 in molar ratio, and the adding diethanolamine is regulated the hydrolysis reaction of titanium isopropylate and the speed of condensation reaction, the diethanolamine that is added and the mol ratio of titanium isopropylate are 1: 9, mix, and obtain second component; According to admixture amount difference, ethanamide, thiosemicarbazide, urea, thiocarbamide are dissolved in the deionized water, be mixed with the aqueous solution of 8～30mol/l, obtain the 3rd component.After second component under agitation added first component, add the 3rd component, three kinds of component add-ons 20: 18: 1 by volume.Adding the back that finishes continues to stir up to forming water white gel, then room temperature ageing 48 hours.
With this through aged gel 20 ℃ of vacuum-dryings 48 hours, obtain powder, with deionized water and washing with alcohol repeatedly, the admixture amount of amides polar compound is 1～30wt% in titanium dioxide granule, the powder that obtains after the centrifugation in box-type furnace in 50 ℃ of dryings more than 48 hours, 120 ℃ of dryings 3 hours, promptly obtain the admixture titanium dioxide granule of micron～nanoscale again.
With this admixture titanium dioxide granule and 50mm
2/ s methyl-silicone oil 30% mixes by volume, obtains blended titanium dioxide electric rheological liquid of the present invention.The yield strength and the current density of different admixture amount electric titania rheological liquids are as shown in table 3 under extra electric field 3kV/mm condition.
Table 3 prepares blended titanium dioxide electric rheological liquid performance index (volume fraction 30%) with titanium isopropylate
By the result of table 1, table 2 and table 3 as can be seen, blended titanium dioxide electric rheological liquid provided by the invention by at the strong polar amides of titanium dioxide admixture or derivatives thereof molecule, forms the admixture titanium dioxide granule of micron or nanoscale, effectively improved the electrorheological fluid yield strength of titanium dioxide, and this electrorheological fluid Stability Analysis of Structures, current density is little, not free settling, pollution-free, the cost of material is low, and preparation technology is simple, the productive rate height.
Claims (8)
1. blended titanium dioxide electric rheological liquid, its disperse phase are the admixture titanium dioxide granule of micron to nano-scale, and dispersion medium is a methyl-silicone oil, and the volume ratio of disperse phase and dispersion medium is 5～50%;
Described admixture titanium dioxide granule prepares for using sol gel reaction, specifically comprises the steps:
1) preparation of three kinds of components:
The titanium alkoxide is mixed with dehydrated alcohol 1: 20 in molar ratio～25, and the pH value of dripping hydrochloric acid or nitric acid regulator solution is 2～3, mixes, and obtains first component;
Deionized water and dehydrated alcohol 1: 2 in molar ratio～3 are mixed, obtain second component;
The amides polar compound is dissolved in the deionized water, is mixed with 8～30mol/l aqueous solution, obtain the 3rd component;
2) three components mix:
Second component after adding first component under the magnetic agitation or under the ultrasound condition, is added the 3rd component, add the back and continue stirring or ultrasonic up to forming gel, then room temperature ageing 5～100 hours; The mixed volume ratio of three kinds of components is first component: second component: the 3rd component=20～25: 18～25: 1;
3) preparation admixture titanium dioxide granule: with step 2) through aged gel 20～120 ℃ of vacuum-dryings 8～12 hours, the product that obtains is used deionized water and washing with alcohol repeatedly, the percentage composition of doping amides polar compound is 1～30wt% in the admixture titanium dioxide granule, the powder that obtains after the centrifugation in air in 50 ℃ of dryings more than 48 hours, 120 ℃ of dryings 3 hours, obtain the admixture titanium dioxide granule of micron again to nano-scale.
2. blended titanium dioxide electric rheological liquid as claimed in claim 1, it is characterized in that described amides polar compound is one or more the mixture that is selected from methane amide, ethanamide, thiosemicarbazide, TCH, urea, thiocarbamide, the or derivatives thereof.
3. blended titanium dioxide electric rheological liquid as claimed in claim 1 is characterized in that, the viscosity of described methyl-silicone oil is 5～500mm
2/ S.
4. the preparation method of the described blended titanium dioxide electric rheological liquid of claim 1 is characterized in that using sol gel reaction to prepare the admixture titanium dioxide granule earlier, mixes with methyl-silicone oil again, specifically comprises the steps:
1) preparation of three kinds of components:
The titanium alkoxide is mixed with dehydrated alcohol 1: 20 in molar ratio～25, and the pH value of dripping hydrochloric acid or nitric acid regulator solution is 2～3, mixes, and obtains first component;
Deionized water and dehydrated alcohol 1: 2 in molar ratio～3 are mixed, obtain second component;
The amides polar compound is dissolved in the deionized water, is mixed with 8～30mol/l aqueous solution, obtain the 3rd component;
2) three components mix:
Second component after adding first component under the magnetic agitation or under the ultrasound condition, is added the 3rd component, add the back and continue stirring or ultrasonic up to forming gel, then room temperature ageing 5～100 hours; The mixed volume ratio of three kinds of components is first component: second component: the 3rd component=20～25: 18～25: 1;
3) preparation admixture titanium dioxide granule: with step 2) through aged gel 20～120 ℃ of vacuum-dryings 8～12 hours, the product that obtains is used deionized water and washing with alcohol repeatedly, the percentage composition of doping amides polar compound is 1～30wt% in the admixture titanium dioxide granule, the powder that obtains after the centrifugation in air in 50 ℃ of dryings more than 48 hours, 120 ℃ of dryings 3 hours, obtain the admixture titanium dioxide granule of micron again to nano-scale;
4) preparation electrorheological fluid: admixture titanium dioxide granule and methyl-silicone oil that step 3) is obtained 5～50% mix by volume, obtain blended titanium dioxide electric rheological liquid.
5. the preparation method of blended titanium dioxide electric rheological liquid as claimed in claim 4 is characterized in that, the titanium alkoxide of described step 1) is tetrabutyl titanate, tetraethyl titanate or titanium isopropylate.
6. the preparation method of blended titanium dioxide electric rheological liquid as claimed in claim 4, it is characterized in that, second component of described step 1) also comprises with titanium alkoxide mol ratio being 1: 8～10 diethanolamine, to regulate the hydrolysis reaction and the condensation reaction rate of titanium alkoxide.
7. the preparation method of blended titanium dioxide electric rheological liquid as claimed in claim 4, it is characterized in that the amides polar compound of described step 1) is one or more the mixture that is selected from methane amide, ethanamide, thiosemicarbazide, TCH, urea, thiocarbamide, the or derivatives thereof.
8. the preparation method of blended titanium dioxide electric rheological liquid as claimed in claim 4 is characterized in that, the viscosity of the methyl-silicone oil of described step 3) is 5～500mm
2/ s.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101089164B (en) * | 2006-06-15 | 2010-08-04 | 中国科学院物理研究所 | Polar molecule type electric rheologic liquid |
| CN101486948B (en) * | 2008-12-31 | 2012-05-02 | 中国科学院宁波材料技术与工程研究所 | Titanium dioxide electrorheological liquid having heavy electrorheological effect under low field |
| CN101486947B (en) * | 2008-12-31 | 2012-01-04 | 中国科学院宁波材料技术与工程研究所 | Nano titanium dioxide electrorheological liquid |
| CN106833824B (en) * | 2016-12-06 | 2019-07-12 | 天诺光电材料股份有限公司 | A kind of giant electro-rheological liquid and preparation method thereof |
| CN107043647B (en) * | 2016-12-06 | 2019-11-15 | 天诺光电材料股份有限公司 | A kind of giant electro-rheological liquid dielectric grain and preparation method thereof |
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| CN1490388A (en) * | 2002-09-16 | 2004-04-21 | �������ӿƼ���ѧ | Electric rheological liquid |
| US6984343B1 (en) * | 2004-06-28 | 2006-01-10 | China Patent Investment Limited | Fluid suspensions with electrorheological effect |
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| CN1768913A (en) * | 2004-11-03 | 2006-05-10 | 西北工业大学 | Method for preparing nano-titanium oxide/amide derivative electrorheological fluid |
| CN1768914A (en) * | 2004-11-03 | 2006-05-10 | 西北工业大学 | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide |
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Patent Citations (5)
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|---|---|---|---|---|
| CN1490388A (en) * | 2002-09-16 | 2004-04-21 | �������ӿƼ���ѧ | Electric rheological liquid |
| US6984343B1 (en) * | 2004-06-28 | 2006-01-10 | China Patent Investment Limited | Fluid suspensions with electrorheological effect |
| CN1769403A (en) * | 2004-11-03 | 2006-05-10 | 西北工业大学 | Acetamide modified nanometer titanium oxide electrorheological fluid |
| CN1768913A (en) * | 2004-11-03 | 2006-05-10 | 西北工业大学 | Method for preparing nano-titanium oxide/amide derivative electrorheological fluid |
| CN1768914A (en) * | 2004-11-03 | 2006-05-10 | 西北工业大学 | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide |
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