CN101979481B - Electrorheological fluid of attapulgite and titanium oxygen compound composite material - Google Patents
Electrorheological fluid of attapulgite and titanium oxygen compound composite material Download PDFInfo
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Abstract
The invention discloses an electrorheological fluid of an attapulgite and titanium oxygen compound composite material. The electrorheological fluid comprises a continuous phase and a dispersed phase dispersed in the continuous phase, wherein the continuous phase is a liquid insulating medium; the dispersed phase is the attapulgite and titanium oxygen compound composite material; the diameter of the attapulgite is between 10 and 70 nm; the length is between 60 nm and 2 mu m; and the mass concentration of the dispersed phase in the electrorheological fluid is between 5 and 75 percent. Compared with the electrorheological fluid of titanium oxygen particles, the electrorheological fluid of the attapulgite and titanium oxygen compound composite material of the invention has the advantages of high yield stress, low leakage current density, high suspension stability and the like; the cost of raw materials is low; the process is simple; and the preparation period is short.
Description
Technical field
The present invention relates to the ER fluid field, be specifically related to a kind of Attapulgite and titanyl compound composite material by electric current and become liquid.
Background technology
ER fluid is the complicated colloidal dispersion that is mixed by the semi-conductor dielectric grain (disperse phase) of nanometer to micro-meter scale and insulating liquid (dispersion medium or title external phase).When not applying external electric field, ER fluid demonstrates the mechanical characteristic of Newtonian fuid, under the extra electric field effect, and the rapid chainization of dielectric grain, equivalent viscosity obviously increases even type of changing into solid, and demonstrates the mechanical characteristic of non-Newtonian fluid.ER fluid is because the regulatable prominent feature of its performance; Demonstrate bigger meliority at aspects such as electromechanical integration, automatic controls than prior art; Can be applicable to devices such as vibroshock, clutch coupling, stopper, deoscillator, is a kind of intelligent material that has development prospect.
Yet most ER fluids have existed ys low excessively (general ys＜30kPa), problems such as anti-sedimentation capacity difference, so since over half a century, electro-rheological technology never obtains widespread usage.The titanyl compound ER fluid is one type of giant electro-rheological liquid that new development is in recent years got up, and more than the big one magnitude of the comparable traditional electrical rheology of its ys liquid, has very strong application prospect.This material adopts sol-gel method and coprecipitation method preparation more, and the pattern of products obtained therefrom is irregular, the wide and serious agglomeration of distribution of sizes, thus influence its ER properties.Recently, it is found that the ER fluid of one-dimensional material has good suspension stability and electric rheological effect, thereby, the ER fluid of the one-dimensional material that begins one's study.
Summary of the invention
The invention provides a kind of Attapulgite and titanyl compound composite material by electric current and become liquid with good electric rheological effect and suspension stability.
The present invention find Attapulgite be a kind of layer of chain-like structure contain Shuifu County's zeopan clay mineral; Its crystal becomes bar-shaped, fibrous agrregate; The diameter of single fiber crystalline substance is generally about 20nm; Length generally can reach 1 μ m, meets the dimensional standard of nano material, is a kind of natural monodimension nanometer material.Be that nucleome is applied to ER fluid and does not also appear in the newspapers at present with the Attapulgite.
A kind of Attapulgite and titanyl compound composite material by electric current become liquid; Comprise external phase and be dispersed in the disperse phase in the external phase; Described external phase is liquid insulating medium; Described disperse phase is Attapulgite and titanyl compound matrix material, and the diameter of described Attapulgite is 10nm～70nm, and length is 60nm～2 μ m;
The mass concentration of disperse phase is 5%～75% in the described ER fluid.
The preparation method of described Attapulgite and titanyl compound matrix material comprises:
(1) with solubility calcium salt compound and organic acid water-soluble with ethanol mixed solvent in, add Attapulgite again, mix, regulating the pH value is 4～7, obtains suspension liquid a;
Wherein, the mole number of calcium ion is 0～0.3mol in every liter of mixed solvent, and calcium ion and organic acid mol ratio are 1: 1～4; The gram number of Attapulgite is 0.1g～1.0g in every liter of mixed solvent; Water and alcoholic acid volume ratio are 1: 2～10 in described water and the ethanol mixed solvent;
(2) with oxalic acid water-soluble with ethanol mixed solvent in, be added dropwise to the titanium salt compound again, stir while dripping, until formation solution b;
Wherein, the concentration of titanium ion is 0.1mol/L～0.3mol/L among the described solution b, and the mol ratio of titanium ion and oxalic acid is 1: 0～3.5; Water and alcoholic acid volume ratio are 1: 0～3 in described water and the ethanol mixed solvent;
(3) while stirring suspension liquid a is added drop-wise among the solution b, forms milky white precipitate gradually, after reacting completely, the deposition ageing after scouring that generates is centrifugal, and the throw out that obtains obtains Attapulgite and titanyl compound matrix material through vacuum-drying and constant pressure and dry.
In the step (1), described solubility calcium salt compound is selected solubility calcium salt compound commonly used for use, can select calcium acetate, anhydrous nitric acid calcium, four water-calcium nitrate, Calcium Chloride Powder Anhydrous, Calcium dichloride dihydrate or calcium chloride hexahydrate etc. for use.Said calcium ion derives from the solubility calcium salt compound.
Described organic acid is selected organic acid commonly used for use, can select in formic acid, acetate, the Hydrocerol A etc. one or more for use.
The purity of described Attapulgite is preferably at least 80%.
In the step (2), described titanium salt compound is selected titanium salt compound commonly used for use, can select titanium tetrachloride, titanium tetrabromide, tetrabutyl titanate, tetraethyl titanate or isopropyl titanate for use.
In the step (3), described ageing condition optimization was: room temperature to 70 ℃ following ageing 2 hours～24 hours.
Described vacuum-drying condition optimization was: 50 ℃～60 ℃ vacuum-dryings 10 hours～24 hours.
Described constant pressure and dry condition optimization was: 100 ℃～130 ℃ constant pressure and dries 2 hours～5 hours.
The liquid insulating medium that described liquid insulating medium selects for use this area ER fluid to use can be selected silicone oil for use, preferable methyl silicone oil or hydroxy silicon oil.
Described Attapulgite and titanyl compound composite material by electric current become the preparation method of liquid; Adopt the conventional preparation method of this area ER fluid; Generally comprise: Attapulgite and titanyl compound matrix material and liquid insulating medium are mixed, be mixed with ER fluid.
Compared with prior art, the present invention has following advantage:
The disperse phase that Attapulgite of the present invention and titanyl compound composite material by electric current become liquid is Attapulgite and titanyl compound matrix material; This matrix material be with bar-shaped micro-nano Attapulgite be nucleome and on Attapulgite the material of composite titanium oxycompound; When polarization takes place in it in electric field; Than existing spherical nanometer dielectric grain orientations takes place more easily, between electrode, form multiple-limb bunch, make ER fluid have higher ys and lower initial viscosity.
Attapulgite of the present invention and titanyl compound composite material by electric current become liquid and have advantages such as yielding stress is big, leakage current density is low, suspension stability is good, and material cost is cheap, and technology is simple, and preparation cycle is short.
Description of drawings
Fig. 1 is the Attapulgite of embodiment 1 preparation and the stereoscan photograph of titanyl compound matrix material;
Fig. 2 is titanyl compound ER fluid and the Attapulgite of embodiment 2 preparations and the rate of descent and the time chart that the titanyl compound composite material by electric current becomes liquid of Comparative Examples 2 preparations;
Fig. 3 is titanyl compound ER fluid and the Attapulgite of embodiment 4 preparations and the rate of descent and the time chart that the titanyl compound composite material by electric current becomes liquid of Comparative Examples 2 preparations;
Fig. 4 is that the Attapulgite and the titanyl compound composite material by electric current of embodiment 5 preparations becomes the static yield strength of liquid and the graph of a relation of electrorheological density and strength of electric field.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed explanation.
Comparative Examples 1
Using Hydrogen chloride adjusting water and ethanol volume ratio is the pH value to 5 of 100ml water/alcoholic acid mixing solutions of 1: 2, obtains solution a.It is in water/ethanol mixed solvent of 1: 1 that 0.04mol oxalic acid is dissolved in 100ml water and ethanol volume ratio, is added dropwise to the 0.02mol tetrabutyl titanate again, stirs while dripping, until forming clear solution b; Keep stirring, solution a is added dropwise among the clear solution b, form milky white precipitate gradually, after reacting completely, the deposition ageing at room temperature that generates 5 hours; Washing of precipitate after the ageing is centrifugal; The product that obtains was put in 50 ℃ of vacuum drying ovens dry 24 hours; 120 ℃ of constant pressure and dries of warp are 4 hours again, obtain titanyl compound, can know that through inductively coupled plasma atomic emission (ICP) analysis wherein titanium elements quality percentage composition is 19.0%.
With titanyl compound that makes and dimethyl silicone oil (viscosity is 50 centistokes (cst)) uniform mixing (mass percentage concentration of titanyl compound is 61%); Promptly make the titanyl compound ER fluid; The null field viscosity of this titanyl compound ER fluid is 9.9Pas; Static yield stress in the electric field of 5kV/mm is 43kPa, and leakage current density is 25 μ A/cm
2
Comparative Examples 2
Take by weighing the titanyl compound matrix material 1.5g of Comparative Examples 1 preparation, mix with 30mL dimethyl silicone oil (viscosity is 50cst), obtain the titanyl compound ER fluid, the mass percentage concentration of titanyl compound is 5%.
Get the above-mentioned titanyl compound ER fluid of 5mL and put into graduated cylinder, leave standstill and measure the suspension stability of ER fluid with direct observational method, as shown in Figure 2.
Embodiment 1
Selecting purity is 98% attapulgite clay crushing screening, becomes the attapulgite clay powder, is 20nm～30nm through scanning electron microscopic observation to the diameter of attapulgite clay powder, and length is 60nm～200nm.
It is in 100ml water/alcoholic acid mixing solutions of 1: 2 that the above-mentioned attapulgite clay powder of 0.05g is added entry and ethanol volume ratio, stirs, with the pH value to 5 of Hydrogen chloride regulator solution; Obtain suspension liquid a.It is in water/ethanol mixed solvent of 1: 1 that 0.04mol oxalic acid is dissolved in 100ml water and ethanol volume ratio, is added dropwise to the 0.02mol tetrabutyl titanate again, stirs while dripping, until forming clear solution b; Keep stirring, suspension liquid a is added dropwise among the solution b, form milky white precipitate gradually, after reacting completely, the deposition ageing at room temperature that generates 5 hours; Washing of precipitate after the ageing is centrifugal; The product that obtains was put in 50 ℃ of vacuum drying ovens dry 24 hours; 120 ℃ of constant pressure and dries of warp are 4 hours again; Obtain Attapulgite and titanyl compound matrix material, can know that through inductively coupled plasma atomic emission (ICP) analysis wherein titanium elements quality percentage composition is 18.3%.This matrix material stereoscan photograph is as shown in Figure 1, and most titanyl compound is coated on the Attapulgite, forms bar-shaped composite structure, and the titanyl compound of small portion exists with particulate state, mixes with bar-shaped composite structure.
With the above-mentioned Attapulgite that makes and titanyl compound matrix material and dimethyl silicone oil (viscosity is 50cst) uniform mixing (mass percentage concentration of Attapulgite and titanyl compound matrix material is 61% in the ER fluid); Promptly make Attapulgite and titanyl compound composite material by electric current and become liquid; The null field viscosity of this ER fluid is 6.2Pas; Static yield stress in the electric field of 5kV/mm is 70kPa, and leakage current density is 21 μ A/cm
2Compare with the titanyl compound ER fluid of Comparative Examples 1 preparation, null field viscosity and leakage current density that the Attapulgite of embodiment 1 preparation and titanyl compound composite material by electric current become liquid reduce, and yielding stress significantly increases.
Take by weighing the Attapulgite and the titanyl compound matrix material 1.5g of embodiment 1 preparation; Mix with 30mL dimethyl silicone oil (viscosity is 50cst); Obtain Attapulgite and titanyl compound composite material by electric current and become liquid, the mass percentage concentration of Attapulgite and titanyl compound matrix material is 5% in the ER fluid.
Get above-mentioned Attapulgite of 5mL and titanyl compound composite material by electric current and become liquid and put into graduated cylinder, leave standstill and measure the suspension stability of ER fluid with direct observational method, as shown in Figure 2.Can find out from Fig. 2: compare with the titanyl compound ER fluid of Comparative Examples 2 preparations, the suspension stability that the Attapulgite of embodiment 2 preparations and titanyl compound composite material by electric current become liquid is significantly improved; The particularly long-term back (30 days) of placing, the variation of the rate of descent of the Attapulgite of embodiment 2 preparations and titanyl compound composite material by electric current change liquid is less than 3%; And the variation of the rate of descent of the titanyl compound ER fluid of Comparative Examples 2 preparations is greater than 20%.
Selecting purity is 88% attapulgite clay crushing screening, becomes the attapulgite clay powder, is 40nm～50nm through scanning electron microscopic observation to the diameter of attapulgite clay powder, length 400nm～600nm.
With the 0.01mol Calcium Chloride Powder Anhydrous be dissolved in contain the 0.015mol Hydrocerol A, water and ethanol volume ratio be in 100ml water/alcoholic acid mixing solutions of 1: 9; Add the above-mentioned attapulgite clay powder of 0.02g again; Stir, the pH value to 6 with the weak ammonia regulator solution obtains suspension liquid a.With 0.02mol oxalic acid water-soluble with the ethanol volume ratio be in 100ml water/ethanol mixed solvent of 1: 1, be added dropwise to the 0.01mol tetrabutyl titanate again, stir while dripping, until formation clear solution b; Keep to stir, suspension liquid a is added dropwise among the solution b, form milky white precipitate gradually, after reacting completely, be deposited in 40 ℃ of following ageings 4 hours what generate; Washing of precipitate after the ageing is centrifugal; The product that obtains was put in 60 ℃ of vacuum drying ovens dry 24 hours; 120 ℃ of constant pressure and dries of warp are 4 hours again; Obtain Attapulgite and titanyl compound matrix material, can know that through inductively coupled plasma atomic emission (ICP) analysis wherein titanium elements quality percentage composition is 9.2%.
With above-mentioned gained Attapulgite and titanyl compound matrix material and dimethyl silicone oil (viscosity is 50cst) uniform mixing (mass percentage concentration of Attapulgite and titanyl compound matrix material is 61% in the ER fluid); Promptly make Attapulgite and titanyl compound composite material by electric current and become liquid; The null field viscosity of this ER fluid is 5.4Pas; Static yield stress in the electric field of 5kV/mm is 56kPa, and leakage current density is 14 μ A/cm
2Compare with the titanyl compound ER fluid of Comparative Examples 1 preparation, null field viscosity and leakage current density that the Attapulgite of embodiment 3 preparations and titanyl compound composite material by electric current become liquid significantly reduce, and yielding stress increases.
Take by weighing the Attapulgite and the titanyl compound matrix material 1.5g of embodiment 3 preparations; Mix with 30mL dimethyl silicone oil (viscosity is 50cst); Obtain Attapulgite and titanyl compound composite material by electric current and become liquid, the mass percentage concentration of Attapulgite and titanyl compound matrix material is 5% in the ER fluid.
Get above-mentioned Attapulgite of 5mL and titanyl compound composite material by electric current and become liquid and put into graduated cylinder, leave standstill and measure the suspension stability of ER fluid with direct observational method, as shown in Figure 3.Can find out from Fig. 3: compare with the titanyl compound ER fluid of Comparative Examples 2 preparations, the suspension stability that the Attapulgite of embodiment 4 preparations and titanyl compound composite material by electric current become liquid is significantly improved; The particularly long-term back (30 days) of placing, the variation of the rate of descent of the Attapulgite of embodiment 4 preparations and titanyl compound composite material by electric current change liquid is less than 5%; And the variation of the rate of descent of the titanyl compound ER fluid of Comparative Examples 2 preparations is greater than 20%.
Selecting purity is 98% attapulgite clay crushing screening, becomes the attapulgite clay powder, is 20nm～30nm through scanning electron microscopic observation to the diameter of attapulgite clay powder, and length is 60nm～200nm.
With the 0.02mol four water-calcium nitrate be dissolved in contain 0.04mol acetate, water and ethanol volume ratio be in 100ml water/alcoholic acid mixing solutions of 1: 7; Add the above-mentioned attapulgite clay powder of 0.025g again; Stir, the pH value to 5.5 with the weak ammonia regulator solution obtains suspension liquid a.With 0.045mol oxalic acid water-soluble with the ethanol volume ratio be in 100ml water/ethanol mixed solvent of 1: 1, be added dropwise to the 0.02mol isopropyl titanate again, stir while dripping, until formation clear solution b; Keep to stir, suspension liquid a is added dropwise among the solution b, form milky white precipitate gradually, after reacting completely, be deposited in 50 ℃ of following ageings 12 hours what generate; Washing of precipitate after the ageing is centrifugal; The product that obtains was put in 55 ℃ of vacuum drying ovens dry 24 hours; 120 ℃ of constant pressure and dries of warp are 4 hours again; Obtain Attapulgite/titanyl compound matrix material, can know that through inductively coupled plasma atomic emission (ICP) analysis wherein titanium elements quality percentage composition is 9.8%.With gained Attapulgite/titanyl compound matrix material and dimethyl silicone oil (viscosity is 50cst) uniform mixing (mass percentage concentration of Attapulgite and titanyl compound matrix material is 61% in the ER fluid); Promptly make Attapulgite and titanyl compound composite material by electric current and become liquid; Its null field viscosity is 4.7Pas, and the relation of static yield strength and leakage current density and strength of electric field is as shown in Figure 4.
Can find out from Fig. 4: this Attapulgite and titanyl compound composite material by electric current become the static yield stress of liquid the electric field of 5kV/mm and are 62kPa, and leakage current density is 7.5 μ A/cm
2Compare with the titanyl compound ER fluid of Comparative Examples 1 preparation, null field viscosity and leakage current density that the Attapulgite of embodiment 5 preparations and titanyl compound composite material by electric current become liquid obviously reduce, and yielding stress increases.
Claims (5)
1. Attapulgite and titanyl compound composite material by electric current become liquid; Comprise external phase and be dispersed in the disperse phase in the external phase; Described external phase is liquid insulating medium, it is characterized in that, described disperse phase is Attapulgite and titanyl compound matrix material; The diameter of described Attapulgite is 10nm～70nm, and length is 60nm～2 μ m;
The mass concentration of disperse phase is 5%～75% in the described ER fluid; The preparation method of described Attapulgite and titanyl compound matrix material comprises:
(1) with solubility calcium salt compound and organic acid water-soluble with ethanol mixed solvent in, add Attapulgite again, mix, regulating the pH value is 4～7, obtains suspension liquid a;
Wherein, the mole number of calcium ion is greater than 0 and smaller or equal to 0.3mol in every liter of mixed solvent, and calcium ion and organic acid mol ratio are 1:1～4; The gram number of Attapulgite is 0.1g～1.0g in every liter of mixed solvent; Water and alcoholic acid volume ratio are 1:2～10 in described water and the ethanol mixed solvent;
(2) with oxalic acid water-soluble with ethanol mixed solvent in, be added dropwise to the titanium salt compound again, stir while dripping, until formation solution b;
Wherein, the concentration of titanium ion is 0.1mol/L～0.3mol/L among the described solution b, and the mol ratio of titanium ion and oxalic acid is 1: greater than 0 and smaller or equal to 3.5; Water and alcoholic acid volume ratio are 1 in described water and the ethanol mixed solvent: greater than 0 and smaller or equal to 3;
(3) while stirring suspension liquid a is added drop-wise among the solution b; Form milky white precipitate gradually, after reacting completely, that the deposition ageing after scouring that generates is centrifugal; The throw out that obtains obtains Attapulgite and titanyl compound matrix material through vacuum-drying and constant pressure and dry;
In the step (1), described solubility calcium salt compound is calcium acetate, anhydrous nitric acid calcium, four water-calcium nitrate, Calcium Chloride Powder Anhydrous, Calcium dichloride dihydrate or calcium chloride hexahydrate;
In the step (1), described organic acid is one or more in formic acid, acetate, the Hydrocerol A;
In the step (2), described titanium salt compound is titanium tetrachloride, titanium tetrabromide, tetrabutyl titanate, tetraethyl titanate or isopropyl titanate;
Described liquid insulating medium is a silicone oil.
2. Attapulgite according to claim 1 and titanyl compound composite material by electric current become liquid, it is characterized in that in the step (3), described ageing condition is: room temperature to 70 ℃ following ageing 2 hours～24 hours.
3. Attapulgite according to claim 1 and titanyl compound composite material by electric current become liquid, it is characterized in that in the step (3), described vacuum-drying condition is: 50 ℃～60 ℃ vacuum-dryings 10 hours～24 hours.
4. Attapulgite according to claim 1 and titanyl compound composite material by electric current became liquid, it is characterized in that in the step (3), described constant pressure and dry condition is: 100 ℃～130 ℃ constant pressure and dries 2 hours～5 hours.
5. Attapulgite according to claim 1 and titanyl compound composite material by electric current become liquid, it is characterized in that described silicone oil is methyl-silicone oil or hydroxy silicon oil.
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| CN102660352B (en) * | 2012-05-17 | 2013-11-06 | 大连理工大学 | Glycerin oxotitanium electrorheological fluid and preparation method thereof |
| CN109321328B (en) * | 2018-09-27 | 2021-06-25 | 安徽省华腾农业科技有限公司 | Electrorheological fluid and preparation method thereof |
| CN111004674A (en) * | 2019-12-09 | 2020-04-14 | 中国科学院宁波材料技术与工程研究所 | One-dimensional nano core-shell structure electrorheological fluid and preparation method thereof |
| 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 |
| CN114171279A (en) * | 2021-12-13 | 2022-03-11 | 盱眙县凹土应用技术研发与成果转化中心 | Electromagnetic double-activity rheological fluid with one-dimensional nano core-shell structure and preparation method thereof |
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