CN101768503B - Titanium oxyoxalate electrorheological fluid and preparation method thereof - Google Patents
Titanium oxyoxalate electrorheological fluid and preparation method thereof Download PDFInfo
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- CN101768503B CN101768503B CN 200810163796 CN200810163796A CN101768503B CN 101768503 B CN101768503 B CN 101768503B CN 200810163796 CN200810163796 CN 200810163796 CN 200810163796 A CN200810163796 A CN 200810163796A CN 101768503 B CN101768503 B CN 101768503B
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Abstract
The invention relates to a titanium oxyoxalate electrorheological fluid and a preparation method thereof. The titanium oxyoxalate electrorheological fluid is characterized by using titanyl oxalate particles in nanometer to micron sizes as a dispersing phase and uniformly dispersing in silicon oil to form the suspended liquid. The titanyl oxalate particles in the suspended liquid have the volume concentration of 5-40 percent. The preparation method of the titanium oxyoxalate electrorheological fluid comprises the following steps of: firstly, carrying out a chemical precipitation reaction of oxalic acid and titanium of the same mol number in an alcohol solvent to prepare titanyl oxalate particles; uniformly mixing the titanyl oxalate particles with the silicon oil; and obtaining the titanium oxyoxalate electrorheological fluid. The titanium oxyoxalate electrorheological fluid provided by the invention has strong electrorheological effect, reaches the stress yield of 120kPs and the dynamic shearing stress of 40kPa when an external electric field is 5kV/mm, has the advantages of small current density, no toxicity, environmental protection, and the like and has favorable application prospects. Moreover, the needed raw materials are easily obtained and have low cost, and the preparation process is simple and has short cycle.
Description
Technical field
The present invention relates to electrorheological fluid and preparation method thereof, specifically refer to a kind of titanium oxyoxalate electrorheological fluid and preparation method thereof.
Background technology
Electrorheological fluid is the even suspension liquid body that a kind of oneself viscosity can noticeable change under External Electrical Field, has the quality of controlled change, and its yielding stress, Young's modulus can change according to effector's will.It usually is dispersed in the transformer oil of low-k by the solia particle with high-k and forms, and it is a kind of suspension under usual conditions, and the transformation of liquid-solid can occur under the effect of electric field for it.When electric field strength was significantly less than certain threshold value, electrorheological fluid was in a liquid state; When strength of electric field was much higher than this threshold value, it just became solid-state.Near the threshold value of strength of electric field, the viscosity of electrorheological fluid becomes greatly with the increase of strength of electric field, between also liquid also between the solid states of matter.
It has been generally acknowledged that this variation is because the small-particle that disperses in the electrorheological fluid is polarized to electric dipole under electric field action, thereby produce the variation that strong electrostatic attraction causes the liquid macroscopic viscosity between these dipoles.Particle becomes ordered arrangement by unordered stochastic distribution in this process, usually forms certain chain and columnar structure, and this microtexture has a significant impact the macro-mechanical property of electrorheological fluid.The character of particulate solid material has determined the quality of electrorheological fluid performance, is the key component of electrorheological fluid.
The continuously adjustable peculiar character of electrorheological fluid soft or hard under electric field action has extensive and important using value, such as clutch coupling, stopper, damping system, vibroshock, buncher, valve, electromechanical coupling control etc.The main performance index of estimating microparticle material is the size of the dynamic shearing stress that can provide, and the dynamic shear stress hard intensity is just high.In addition, it is high that stability is wanted, and electric conductivity is little.Insulating liquid has silicone oil, edible oil, mineral oil usually, and insulating liquid should have higher boiling point, and stability, erosion resistance is good.Found that at present multiple electrorheological fluid can become effectiveness by generation current, but the shearing resistance of existing most electrorheological fluid is low, generally is not higher than 10kPa, can't reach the industrial application level, realizes the engineering using value.
Summary of the invention
Technical problem to be solved by this invention is the present situation for prior art, and a kind of titanium oxyoxalate electrorheological fluid with high shear strength, low current density is provided, its Stability Analysis of Structures, pollution-free, good without the burn into industrial applicability.
Another technical problem to be solved by this invention is the present situation for prior art, and the preparation method of the titanium oxyoxalate electrorheological fluid that a kind of raw materials cost is low, preparation technology is simple, with short production cycle is provided.
It is as follows that the present invention solves the problems of the technologies described above the technical scheme that adopts: this titanium oxyoxalate electrorheological fluid is characterized in that: its be with nanometer to the titanium oxyoxalate particle of micron-scale as disperse phase, be dispersed in the suspension liquid that forms in the silicone oil; And the volumetric concentration of this suspension liquid mesoxalic acid oxygen titanium particle is 5～40%.
Preferably, described silicone oil can be selected from methyl-silicone oil or hydroxy silicon oil.
The preparation method of above-mentioned titanium oxyoxalate electrorheological fluid, oxalic acid and titanium salt the chemical precipitation reaction preparation titanium oxyoxalate particle in organic alcohol solvent of its principle for using first identical mole number, then the titanium oxyoxalate particle is evenly mixed with silicone oil, obtain titanium oxyoxalate electrorheological fluid.Specifically comprise the steps:
1. the preparation of titanium oxyoxalate particle
Titanium salt and organic alcohol solvent are mixed take the ratio of mol ratio as 1: 20～70, and the pH value of control solution obtains solution A less than 2; Preferably, described titanium salt can be selected from tetrabutyl titanate, titanium tetrachloride, tetraethyl titanate or titanium isopropylate; PH value can be regulated by dripping hydrochloric acid or nitric acid;
Get with the oxalic acid of the identical mole number of titanium salt and be dissolved in the Organic Alcohol, be mixed with oxalic acid solution B;
Place agitator at the uniform velocity to stir solution A, simultaneously solution B is splashed in the solution A; Along with the adding of B, precipitation forms gradually; After reacting completely, then the sedimentation and filtration with generating will precipitate oven dry, obtain the titanium oxyoxalate particle that nanometer distributes to micron-scale;
2. the preparation of titanium oxyoxalate electrorheological fluid
The titanium oxyoxalate particle that 1. step is obtained evenly mixes with silicone oil, and the volumetric concentration that is mixed with the titanium oxyoxalate particle is 5～40% titanium oxyoxalate electrorheological fluid, obtains titanium oxyoxalate electrorheological fluid of the present invention.
Preferably, described silicone oil can be selected from methyl-silicone oil or hydroxy silicon oil.
Titanium oxyoxalate electrorheological fluid provided by the invention, be formulated with the oxalic acid of identical mole number and the titanium salt titanium oxyoxalate that precipitin reaction makes in organic alcohol solvent and insulating liquid medium, its required starting material very easily obtain, and are with low cost, preparation technology is simple, and the cycle is short; Prepared titanium oxyoxalate electrorheological fluid has strong electric rheopectic effect.When extra electric field was 5kV/mm, its yielding stress reached 120kPa, and dynamic shearing stress can reach 40kPa, and had the many merits such as current density is little, nontoxic, pollution-free, and good application prospect is arranged.
Description of drawings
Fig. 1: the relation of the yielding stress of the titanium oxyoxalate electrorheological fluid of different volumes concentration and strength of electric field in the embodiment of the invention 1;
Fig. 2: the relation of the current density of the titanium oxyoxalate electrorheological fluid of different volumes concentration and strength of electric field in the embodiment of the invention 1;
Fig. 3: the relation of the shearing resistance of the titanium oxyoxalate electrorheological fluid of 30% volumetric concentration and shearing rate in the embodiment of the invention 1;
Fig. 4: the relation of the apparent viscosity of the titanium oxyoxalate electrorheological fluid of 30% volumetric concentration and shearing rate in the embodiment of the invention 1;
Fig. 5: the XRD figure spectrum of the embodiment of the invention 1 mesoxalic acid oxygen titanium particle;
Fig. 6: the infrared transmission spectra figure of the embodiment of the invention 1 mesoxalic acid oxygen titanium particle.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
17.4ml tetrabutyl titanate and ethanol were mixed in 1: 50 in molar ratio, stir, the pH value that then drips hydrochloric acid control solution is 2.0, obtains stabilizing solution A; To be dissolved in the ethanol with the oxalic acid of the identical mole number of tetrabutyl titanate, be mixed with the oxalic acid ethanolic soln B of 1mol/l; Solution A placed on the stirrer stir, get the 50ml solution B it is splashed in the solution A, form gradually precipitation; After reacting completely, with the sedimentation and filtration post-drying that generates, namely obtain the titanium oxyoxalate particle that nanometer distributes to micron-scale.The XRD figure of titanium oxyoxalate particle is composed as shown in Figure 5, and as can be seen from Figure 5, this titanium oxyoxalate particle is amorphous state; Fig. 6 is the infrared transmission spectra figure of this titanium oxyoxalate particle, the as seen from Figure 6 charateristic avsorption band of its carboxyl, hydroxyl.
This titanium oxyoxalate particle is evenly mixed with methyl-silicone oil, be mixed with the titanium oxyoxalate solids volume concentration and be 10%, 20% and 30% titanium oxyoxalate electrorheological fluid.The ER properties of this suspension is measured with the cylinder method of masurement of rotational rheometer, and its yield strength is measured under the proof stress mode condition, and its shearing resistance is measured under the speed control pattern.Relation by measuring its yielding stress and strength of electric field as shown in Figure 1, the relation of current density and strength of electric field is as shown in Figure 2.Volumetric concentration be the shearing resistance of electrorheological fluid of 30% titanium oxyoxalate and shearing rate relation as shown in Figure 3, the relation of apparent viscosity and shearing rate is as shown in Figure 4.
Embodiment 2
5.5ml titanium tetrachloride and Virahol were mixed in 1: 40 in molar ratio, stir, the pH value that then drips nitric acid control solution is 1.5, obtains stabilizing solution A; To be dissolved in the Virahol with the oxalic acid of the identical mole number of titanium tetrachloride, be mixed with 0.5mol/l oxalic acid aqueous isopropanol B; Solution A placed on the stirrer stir, get the 100ml solution B it is splashed in the solution A, form gradually precipitation; After reacting completely, with the sedimentation and filtration post-drying that generates, namely obtain the titanium oxyoxalate particle that needed nanometer distributes to micron-scale.
This titanium oxyoxalate particle is evenly mixed with hydroxy silicon oil, be mixed with volumetric concentration and be 15%, 20% and 30% titanium oxyoxalate electrorheological fluid.When extra electric field V=4.0kV/mm, the yield strength of 15% electrorheological fluid is 16kPa, and current density is 8uA/cm
2The yield strength of 20% electrorheological fluid can reach 60kPa, and current density is 18uA/cm
2The yield strength of 30% electrorheological fluid can reach 84kPa, and current density is 25uA/cm
2
Embodiment 3
17.4ml tetrabutyl titanate and propyl alcohol were mixed in 1: 30 in molar ratio, stir, the pH value that then drips hydrochloric acid or nitric acid control solution is 1.0, obtains stabilizing solution A; To be dissolved in the propyl alcohol with the oxalic acid of the identical mole number of tetrabutyl titanate, be mixed with 0.5mol/l oxalic acid propanol solution B; Solution A placed on the stirrer stir, get the 100ml solution B it is splashed in the solution A, form gradually precipitation; With the sedimentation and filtration post-drying that generates, namely obtain the titanium oxyoxalate particle that needed nanometer distributes to micron-scale after reacting completely.
This titanium oxyoxalate particle is evenly mixed with methyl-silicone oil, be mixed with volumetric concentration and be 10%, 20% and 30% titanium oxyoxalate electrorheological fluid of the present invention.When extra electric field V=5.0kV/mm, the yield strength of 10% electrorheological fluid is 10kPa, and shearing resistance is 5kPa, and current density is 8uA/cm
2The yield strength of 20% electrorheological fluid can reach 68kPa, and shearing resistance is 20kPa, and current density is 15uA/cm
2The yield strength of 30% electrorheological fluid can reach 96kPa, and shearing resistance is 32kPa, and current density is 20uA/cm
2
Embodiment 4
5.5ml titanium tetrachloride and methyl alcohol were mixed in 1: 60 in molar ratio, stir, the pH value that then drips hydrochloric acid or nitric acid control solution is 1.5, obtains stabilizing solution A; To be dissolved in the methyl alcohol with the oxalic acid of the identical mole number of titanium tetrachloride, be mixed with 2mol/l methyl ethyl oxalate alcoholic solution B; Solution A placed on the stirrer stir, get the 25ml solution B it is splashed in the solution A, form gradually precipitation; After reacting completely, with the sedimentation and filtration post-drying that generates, namely obtain the titanium oxyoxalate particle that needed nanometer distributes to micron-scale.
This titanium oxyoxalate particle is evenly mixed with methyl-silicone oil, be mixed with volumetric concentration and be 15%, 25% and 35% titanium oxyoxalate electrorheological fluid.When extra electric field V=4.0kV/mm, the yield strength of 15% electrorheological fluid is 16kPa, and shearing resistance is 7kPa, and current density is 8uA/cm
2The yield strength of 20% electrorheological fluid can reach 70kPa, and shearing resistance is 25kPa, and current density is 18uA/cm
2The yield strength of 30% electrorheological fluid can reach 90kPa, and shearing resistance is 35kPa, and current density is 25uA/cm
2
Embodiment 5
10.3ml tetraethyl titanate and propyl carbinol were mixed in 1: 30 in molar ratio, stir, the pH value that then drips hydrochloric acid control solution is 0.5, obtains stabilizing solution A; To be dissolved in the propyl carbinol with the oxalic acid of the identical mole number of tetraethyl titanate, be mixed with 0.5mol/l oxalic acid butanol solution B; Solution A placed on the stirrer stir, get the 100ml solution B it is splashed in the solution A, form gradually precipitation; After reacting completely, with the sedimentation and filtration post-drying that generates, namely obtain the titanium oxyoxalate particle that needed nanometer distributes to micron-scale.This titanium oxyoxalate particle is evenly mixed with hydroxy silicon oil, be mixed with volumetric concentration and be 40% titanium oxyoxalate electrorheological fluid.When extra electric field V=4.0kV/mm, the yield strength of electrorheological fluid can reach 120kPa, and shearing resistance is 34kPa, and current density is 30uA/cm
2
Embodiment 6
14.8ml titanium isopropylate and ethanol were mixed in 1: 45 in molar ratio, stir, the pH value that then drips hydrochloric acid or nitric acid control solution is 0, obtains stabilizing solution A; To be dissolved in the Virahol with the oxalic acid of the identical mole number of titanium isopropylate, be mixed with lmol/l oxalic acid aqueous isopropanol B; Solution A placed on the stirrer stir, get the 50ml solution B it is splashed in the solution A, form gradually precipitation; After reacting completely, with the sedimentation and filtration post-drying that generates, namely obtain the titanium oxyoxalate particle that needed nanometer distributes to micron-scale.This titanium oxyoxalate particle is evenly mixed with methyl-silicone oil, be mixed with volumetric concentration and be 45% titanium oxyoxalate electrorheological fluid of the present invention.When extra electric field V=4.0kV/mm, the yield strength of electrorheological fluid can reach 125kPa, and shearing resistance is 36kPa, and current density is 35uA/cm
2
Claims (3)
1. titanium oxyoxalate electrorheological fluid is characterized in that: its be with nanometer to the titanium oxyoxalate particle of micron-scale as disperse phase, be dispersed in the suspension liquid that forms in the silicone oil; And the volumetric concentration of this suspension liquid mesoxalic acid oxygen titanium particle is 5～40%;
The preparation method of this titanium oxyoxalate electrorheological fluid comprises the steps:
1. the preparation of titanium oxyoxalate particle
Tetrabutyl titanate, titanium tetrachloride, tetraethyl titanate or titanium isopropylate and organic alcohol solvent are mixed take the ratio of mol ratio as 1: 20～70, and the pH value of control solution obtains solution A less than or equal to 2;
Get with the oxalic acid of tetrabutyl titanate, titanium tetrachloride, tetraethyl titanate or the identical mole number of titanium isopropylate and be dissolved in the Organic Alcohol, be mixed with oxalic acid solution B;
Place agitator at the uniform velocity to stir solution A, simultaneously solution B is splashed in the solution A; Along with the adding of B, precipitation forms gradually; After reacting completely, then the sedimentation and filtration with generating will precipitate oven dry, obtain the titanium oxyoxalate particle that nanometer distributes to micron-scale;
2. the preparation of titanium oxyoxalate electrorheological fluid
The titanium oxyoxalate particle that 1. step is obtained evenly mixes with silicone oil, and the volumetric concentration that is mixed with the titanium oxyoxalate particle is 5～40% titanium oxyoxalate electrorheological fluid.
2. titanium oxyoxalate electrorheological fluid according to claim 1, it is characterized in that: described silicone oil is methyl-silicone oil or hydroxy silicon oil.
3. titanium oxyoxalate electrorheological fluid according to claim 1 is characterized in that: step is controlled the pH value of solution less than or equal to 2 by adding hydrochloric acid or nitric acid in 1..
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| CN101979481B (en) * | 2010-10-18 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Electrorheological fluid of attapulgite and titanium oxygen compound composite material |
| CN101993760A (en) * | 2010-11-19 | 2011-03-30 | 中国科学院宁波材料技术与工程研究所 | Titanium oxygen base material electrorheological fluid and preparation method thereof |
| CN103952210B (en) * | 2014-05-13 | 2016-01-20 | 中国科学院宁波材料技术与工程研究所 | A kind of method preventing electrorheological fluid dispersion medium from volatilizing |
| CN111004675A (en) * | 2019-12-09 | 2020-04-14 | 中国科学院宁波材料技术与工程研究所 | Fibrous composite material electrorheological fluid and preparation method thereof |
| CN112028286B (en) * | 2020-09-16 | 2023-09-19 | 华东理工大学 | Heterogeneous fiber combined deoiling synergistic micro-nano suspended particle removing device and removing method |
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| CN1345919A (en) * | 2000-09-25 | 2002-04-24 | 西北工业大学 | Rareearth doped modified barium carbonate current rheological liquid and preparation process thereof |
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| CN1345919A (en) * | 2000-09-25 | 2002-04-24 | 西北工业大学 | Rareearth doped modified barium carbonate current rheological liquid and preparation process thereof |
| CN1490388A (en) * | 2002-09-16 | 2004-04-21 | �������ӿƼ���ѧ | Electric rheological liquid |
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Application publication date: 20100707 Assignee: Ningbo magweite Electric Appliance Co.,Ltd. Assignor: NINGBO INSTITUTE OF MATERIALS TECHNOLOGY & ENGINEERING, CHINESE ACADEMY OF SCIENCES Contract record no.: X2023980033744 Denomination of invention: Titanium Oxalate Electrorheological Fluid and Its Preparation Method Granted publication date: 20130109 License type: Common License Record date: 20230323 |
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Application publication date: 20100707 Assignee: NINGBO YOKEY PRECISION TECHNOLOGY Co.,Ltd. Assignor: NINGBO INSTITUTE OF MATERIALS TECHNOLOGY & ENGINEERING, CHINESE ACADEMY OF SCIENCES Contract record no.: X2023980034039 Denomination of invention: Titanium Oxalate Electrorheological Fluid and Its Preparation Method Granted publication date: 20130109 License type: Common License Record date: 20230329 |