CN111004675A - Fibrous composite material electrorheological fluid and preparation method thereof - Google Patents
Fibrous composite material electrorheological fluid and preparation method thereof Download PDFInfo
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
- C10M171/001—Electrorheological fluids; smart fluids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/09—Complexes with metals
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/0405—Siloxanes with specific structure used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
- C10M2229/0415—Siloxanes with specific structure containing aliphatic substituents used as base material
Abstract
The invention discloses a fibrous composite electrorheological fluid and a preparation method thereof. The electrorheological fluid comprises a dispersion phase and a dispersion medium, wherein the dispersion medium comprises an insulating liquid, and the dispersion phase comprises fibrous sepiolite-titanium oxyoxalate composite particles which are formed by coating the surface of sepiolite with a fibrous structure with titanium oxyoxalate particles. The preparation method comprises the following steps: mixing a mixed solution containing organic titanate and an organic alcohol solvent with oxalic acid and reacting to form a mixed reaction system; adding the fibrous sepiolite into the mixed reaction system for reaction, and coating the formed titanium oxyoxalate colloid particles on the surface of the fibrous sepiolite through heterogeneous nucleation to obtain fibrous sepiolite-titanium oxyoxalate composite particles; then the electrorheological fluid is uniformly dispersed in the insulating liquid to obtain the electrorheological fluid. The fibrous composite electrorheological fluid has the advantages of large dynamic shear stress, good suspension stability and the like, and has wide raw material sources, simple process and short preparation period.
Description
Technical Field
The invention relates to an electrorheological fluid and a preparation method thereof, in particular to an electrorheological fluid of a fibrous composite material and a preparation method thereof, belonging to the technical field of electrorheological fluids.
Background
Electrorheological fluids are complex fluids formed by mixing dielectric particles (dispersed phase) with insulating liquids (dispersions), and the dielectric particles form chains or columnar structures under the action of an electric field, so that the suspension can be transformed into liquid-solid-like state. The rheological property of the electrorheological fluid is continuously adjustable, quick response (a few milliseconds) and the peculiar property of reversible transformation, so that the electrorheological fluid becomes the optimal intelligent material with adjustable hardness. The electrorheological fluid can realize electromechanical integrated intelligent control, and is used for manufacturing damping systems, shock absorption and noise reduction systems, electromechanical coupling control, robot parts, rehabilitation equipment and the like. The electrorheological fluid evaluation report of the U.S. department of energy predicts that if the electrorheological fluid breaks through in engineering application, the economic benefit can reach billions of dollars per year.
Titanyl oxalate is considered to be an electrorheological material with wide application prospect due to its high dielectric constant and large amount of polar groups. Although the titanium oxyoxalate material has high yield stress, people find that the titanium oxyoxalate material has the bottleneck of low dynamic shear strength and stability through practical application. The synthesis of the titanium oxyoxalate particles with shape anisotropy is considered to be an effective way for solving the problem, and the theoretical calculation result of electrorheological fluid shows that under the condition of applying an electric field, ellipsoidal or fibrous particles with the same volume have larger long-axis polarization capability and electrorheological effect than spherical particles, the electrorheological activity of the particles is increased along with the increase of the length-diameter ratio of the particles, and meanwhile, the fibrous particles are easier to form a firm chain network structure under the action of the electric field, so that the fibrous particles have stronger shear failure resistance, higher dynamic shear strength and stability.
However, titanium oxyoxalate is difficult to synthesize a one-dimensional nanostructure by general physical and chemical methods due to the characteristics of its own structure, and no relevant report is reported at present.
Disclosure of Invention
The invention mainly aims to provide the fibrous composite electrorheological fluid with high dynamic shear strength and high stability, which has stable structure, no pollution, no corrosion and good industrial applicability, thereby overcoming the defects in the prior art.
The invention also aims to provide a preparation method of the fibrous composite electrorheological fluid, which has the advantages of low raw material cost, simple preparation process and short production period.
In order to achieve the purpose, the invention adopts the following technical scheme:
the embodiment of the invention provides a fibrous composite electrorheological fluid which comprises a dispersion phase and a dispersion medium, wherein the dispersion medium comprises an insulating liquid, the dispersion phase is uniformly dispersed in the dispersion medium, the dispersion phase comprises fibrous sepiolite-titanyl oxalate composite particles, and the fibrous sepiolite-titanyl oxalate composite particles are formed by coating the surface of sepiolite with a fibrous structure with titanyl oxalate particles.
The embodiment of the invention also provides a preparation method of the fibrous composite electrorheological fluid, which comprises the following steps:
mixing a mixed solution containing organic titanate and an organic alcohol solvent with oxalic acid, and reacting at 0-50 ℃ for 1-3 h to form a mixed reaction system;
adding fibrous sepiolite into the mixed reaction system, and reacting for 2-10 h at 0-20 ℃, so that the formed titanium oxyoxalate colloid particles are coated on the surface of the fibrous sepiolite through heterogeneous nucleation, thereby obtaining fibrous sepiolite-titanium oxyoxalate composite particles;
and uniformly dispersing the fibrous sepiolite-titanyl oxalate composite particles in insulating liquid to obtain the fibrous composite electrorheological fluid.
The embodiment of the invention also provides the fibrous composite material electrorheological fluid prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes the theory of electrorheological material design that fibrous particles are easy to form a firm chain network structure under the action of an electric field, so that the electrorheological material has stronger shear failure resistance, higher dynamic shear strength and stability as guidance, and aims at solving the problem that the titanium oxyoxalate is difficult to synthesize a one-dimensional nano structure by common physical and chemical methods due to the structural characteristics of the titanium oxyoxalate. The natural nano fibrous sepiolite is used as a carrier, the adsorption and growth processes of titanium oxyoxalate colloid particles on the surface are controlled through heterogeneous nucleation, the sepiolite @ titanium oxyoxalate composite particles with the nano fibrous structure are synthesized for the first time, and the sepiolite @ titanium oxyoxalate composite particles are mixed with insulating liquid to prepare the fibrous composite electrorheological fluid. Compared with the traditional titanium oxyoxalate particle electrorheological fluid, the fibrous composite electrorheological fluid obtained by the invention has the advantages of large dynamic shear stress, good suspension stability and the like under the conditions of the same volume fraction and external electric field intensity, and has wide raw material source, low cost, simple process and short preparation period.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanning electron micrograph of titanyl oxalate prepared according to comparative example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the nano fibrous sepiolite @ titanyl oxalate prepared in example 1 of the present invention.
Fig. 3 is a graph of the dynamic shear application versus the electric field of the electrorheological fluids prepared in comparative example 1 and example 1 of the present invention.
Fig. 4 is a graph of the standing anti-settling rate of the electrorheological fluids prepared in comparative example 1 and example 1 of the present invention as a function of time.
Detailed Description
The sepiolite is a silicate clay mineral with a layer chain structure, the micro morphology of the sepiolite generally has two types of granular shape and fibrous shape, wherein the nano fibrous sepiolite has high length-diameter ratio and is easy to modify and modify the surface, and the sepiolite is a good carrier material. If the unique one-dimensional nano material characteristics of the fibrous sepiolite can be utilized, the nano core-shell structure is formed by controlling the adsorption and growth processes of the titanium oxyoxalate on the surface, and the method is a very feasible way for realizing the controllable preparation of the one-dimensional nano titanium oxyoxalate material.
In view of the defects in the prior art, the inventor of the present invention provides a technical scheme of the present invention through long-term research and a great deal of practice, and the present invention takes an electrorheological material design theory that fibrous particles are easy to form a firm chain network structure under the action of an electric field, so that the electrorheological material has stronger shear failure resistance, higher dynamic shear strength and stability as guidance, and aims at the problem that titanium oxyoxalate is difficult to synthesize a one-dimensional nano structure through a common physical and chemical method due to the structural characteristics of the titanium oxyoxalate. The natural nano fibrous sepiolite is used as a carrier, the adsorption and growth processes of titanium oxyoxalate colloid particles on the surface are controlled through heterogeneous nucleation, the sepiolite @ titanium oxyoxalate composite particles with the nano fibrous structure are synthesized for the first time, and the sepiolite @ titanium oxyoxalate composite particles are mixed with insulating liquid to prepare the fibrous composite electrorheological fluid.
The technical solution, its implementation and principles, etc. will be further explained as follows.
As an aspect of the technical solution of the present invention, a fibrous composite electrorheological fluid includes a dispersed phase and a dispersion medium, the dispersion medium includes an insulating liquid, the dispersed phase is uniformly dispersed in the dispersion medium, the dispersed phase includes fibrous sepiolite-titanyl oxalate composite particles (i.e., fibrous sepiolite @ titanyl oxalate composite particles), and the fibrous sepiolite-titanyl oxalate composite particles are formed by coating titanyl oxalate particles on the surface of sepiolite having a fibrous structure.
In some embodiments, the mass ratio of the fibrous sepiolite to the titanyl oxalate in the fibrous sepiolite-titanyl oxalate composite particles is 1: 0.2-2.
In some embodiments, the content of the fibrous sepiolite-titanyl oxalate composite particles in the fibrous composite electrorheological fluid is 10 to 20 vol%.
Furthermore, the fibrous composite electrorheological fluid takes sepiolite with a fibrous structure coated with titanyl oxalate particles as a disperse phase, and is uniformly dispersed in insulating liquid to prepare suspension liquid with the volume concentration of 10-20 vol%.
In some embodiments, the fibrous sepiolite is a nano sepiolite with a diameter of 20-50 nm and a length of 0.5-3 μm.
Further, the insulating liquid is a liquid insulating medium used in the art for electro-rheological fluids, and can be silicone oil, preferably methyl silicone oil and/or hydroxyl silicone oil, but is not limited thereto.
In conclusion, the fibrous composite electrorheological fluid has the advantages of large dynamic shear stress, good suspension stability and the like, and has stable structure, no pollution, no corrosion and good industrial applicability.
As another aspect of the technical scheme of the invention, the related preparation method of the fibrous composite electrorheological fluid comprises the following principles: firstly, by a liquid phase method, the nano fibrous sepiolite is used as a carrier, and the pH value of a reaction system is regulated and controlled by ammonia water, so that titanium oxyoxalate colloid particles are coated on the surface of the nano fibrous sepiolite through heterogeneous nucleation to form uniform and stable fibrous sepiolite @ titanium oxyoxalate particles. And then uniformly mixing the fibrous sepiolite @ titanium oxyoxalate particles with insulating liquid to obtain the fibrous sepiolite @ titanium oxyoxalate electrorheological fluid.
Specifically, the preparation method of the fibrous composite electrorheological fluid provided by the invention comprises the following steps:
mixing a mixed solution containing organic titanate and an organic alcohol solvent with oxalic acid, and reacting at 0-50 ℃ for 1-3 h to form a mixed reaction system;
adding fibrous sepiolite into the mixed reaction system, and reacting for 2-10 h at 0-20 ℃, so that the formed titanium oxyoxalate colloid particles are coated on the surface of the fibrous sepiolite through heterogeneous nucleation, thereby obtaining fibrous sepiolite-titanium oxyoxalate composite particles;
and uniformly dispersing the fibrous sepiolite-titanyl oxalate composite particles in insulating liquid to obtain the fibrous composite electrorheological fluid.
In some embodiments, the molar ratio of the organotitanate to organic alcohol solvent is 1: 100-200.
In some embodiments, the molar ratio of organic titanate to oxalic acid is 1: 1.
in some embodiments, the method of making comprises: and adjusting the pH value of the mixed solution to 1-2 by adopting an acidic substance.
Further, the acidic substance includes any one or a combination of two or more of acetic acid, hydrochloric acid, nitric acid, and the like, but is not limited thereto.
In some embodiments, the organic titanate includes any one or a combination of two or more of tetrabutyl titanate, tetraethyl titanate, tetraisopropyl titanate, and the like, but is not limited thereto.
In some embodiments, the organic alcohol solvent includes any one or a combination of two or more of ethanol, isopropanol, n-butanol, and the like, but is not limited thereto.
In some embodiments, the method of making comprises: adding fibrous sepiolite into the mixed reaction system, reacting for 2-10 h at 0-20 ℃, adding an alkaline substance into the mixed reaction system under the stirring condition, and adjusting the pH value of the mixed reaction system to 4-5, so that the formed titanium oxyoxalate colloid particles are coated on the surface of the fibrous sepiolite through heterogeneous nucleation, thereby obtaining the fibrous sepiolite-titanium oxyoxalate composite particles.
Further, the alkaline substance includes ammonia, but is not limited thereto.
Further, the preparation method further comprises the following steps: and after the reaction is finished, filtering, washing and drying the obtained reaction liquid to obtain the fibrous sepiolite-titanyl oxalate composite particles.
In some embodiments, the mass ratio of the fibrous sepiolite to the oxalic acid is 1-2: 1, that is, the addition amount of the fibrous sepiolite is 1-2 times of the mass of the oxalic acid.
In some embodiments, the fibrous sepiolite is a nano sepiolite with a diameter of 20-50 nm and a length of 0.5-3 μm.
Further, the insulating liquid is a liquid insulating medium used in the art for electro-rheological fluids, and can be silicone oil, preferably methyl silicone oil and/or hydroxyl silicone oil, but is not limited thereto.
In some more specific embodiments, the method for preparing the fibrous composite electrorheological fluid specifically comprises the following steps:
① preparation of fibrous sepiolite @ titanyl oxalate particles
Firstly, titanium salt and an organic alcohol solvent are uniformly mixed according to the molar ratio of 1: 100-200, the pH value of the solution is controlled to be between 1 and 2 by dropwise adding a proper amount of acetic acid, then, oxalic acid with the same molar number as that of the titanium salt is added under the stirring condition, the solution reacts for 1 to 3 hours at the temperature of 0 to 50 ℃ to fully react to form a composite solution A, then, a proper amount of fibrous sepiolite is added into the composite solution A to prepare a mixed solution B, a proper amount of ammonia water is added into the mixed solution B under the stirring condition to adjust the pH value to be between 4 and 5, and the reaction is carried out for 2 to 10 hours at the temperature of 0 to 20 ℃ to ensure that titanium oxyoxalate colloid particles are coated on the surface of the fibrous sepiolite through heterogeneous nucleation. And after the reaction is completed, filtering, washing and drying the generated composite suspension to obtain the fibrous sepiolite @ titanyl oxalate particles.
② preparation of fibrous sepiolite @ titanyl oxalate electrorheological fluid
And (2) uniformly mixing the fibrous sepiolite @ titanyl oxalate particles obtained in the step ① with insulating liquid to prepare the fibrous sepiolite @ titanyl oxalate electrorheological fluid with the volume concentration of the fibrous sepiolite @ titanyl oxalate particles being 10-20%, so as to obtain the fibrous composite electrorheological fluid.
As another aspect of the technical solution of the present invention, it relates to an electrorheological fluid of fibrous composite material prepared by the aforementioned method.
Compared with the traditional titanium oxyoxalate particle electrorheological fluid, the fibrous composite electrorheological fluid obtained by the invention has the advantages of large dynamic shear stress, low leakage current density, good suspension stability and the like under the conditions of the same volume fraction and external electric field intensity, and has wide raw material source, low cost, simple process and short preparation period.
It is to be understood that within the scope of the present invention, the above-described features of the present invention and those specifically described below (e.g., in the examples) may be combined with each other to form new or preferred embodiments. Not to be reiterated herein, but to the extent of space.
The technical solutions of the present invention will be described in further detail below with reference to several preferred embodiments and accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. In the following examples, experimental methods without specific conditions noted are generally performed under conventional conditions or conditions recommended by the manufacturer, based on a full understanding of the present invention.
Comparative example 1
Mixing 17.4ml of tetrabutyl titanate and ethanol according to the molar ratio of 1: 50, uniformly stirring, and then dropwise adding hydrochloric acid to control the pH value of the solution to be 2.0 to obtain a stable solution A; adding oxalic acid with the same mole number as tetrabutyl titanateDissolving in ethanol to prepare 1mol/l oxalic acid ethanol solution B; stirring the solution A on a stirrer, and dripping 50ml of the solution B into the solution A to gradually form a precipitate; after the reaction is completed, filtering and drying the generated precipitate to obtain the nano-sized to micron-sized titanium oxyoxalate particles, wherein the SEM atlas of the titanium oxyoxalate particles is shown in figure 1, and the titanium oxyoxalate particles are in irregular granular shapes as can be seen from figure 1. The titanium oxyoxalate particles are evenly mixed with methyl silicone oil to prepare the titanium oxyoxalate electrorheological fluid with the volume concentration of the titanium oxyoxalate particles being 15 percent. The electrorheological property of the titanium oxyoxalate electrorheological fluid is measured by a cylinder measuring method of a rotary rheometer, and the dynamic shear strength of the titanium oxyoxalate electrorheological fluid is measured by controlling the shear rate to be 1S-1Measured under the conditions. The dynamic shear stress is measured in relation to the electric field strength as shown in FIG. 3. The suspension stability of the titanium oxyoxalate electrorheological fluid is measured by adopting a standing observation method, and the relationship between the standing anti-settling rate and the time is shown in figure 4.
Example 1
Uniformly mixing 20ml of tetrabutyl titanate and ethanol according to a molar ratio of 1: 150, dropwise adding acetic acid to control the pH value of the solution to be 1.5, adding oxalic acid with the same molar number as that of tetrabutyl titanate under the stirring condition to react for 2 hours at 25 ℃ to form a composite solution A, adding nano fibrous sepiolite (the diameter is 20nm and the length is 0.5 mu m) with the mass of 1.5 times of the oxalic acid into the composite solution A to prepare a mixed solution B, adding ammonia water into the mixed solution B under the stirring condition to adjust the pH value to be 4.5, and reacting for 6 hours at 10 ℃ to ensure that titanium oxyoxalate colloidal particles are coated on the surface of the nano fibrous sepiolite through heterogeneous nucleation. And after the reaction is completed, filtering, washing and drying the generated composite suspension to obtain the sepiolite @ titanyl oxalate particles. The SEM spectrum of the sepiolite @ titanyl oxalate particles is shown in fig. 2, and it can be seen from fig. 2 that the composite particles are fibrous nanostructures; the nano fibrous sepiolite @ titanium oxyoxalate particles are uniformly mixed with methyl silicone oil to prepare the fibrous composite electrorheological fluid with the volume concentration of the sepiolite @ titanium oxyoxalate particles being 15%. The electrorheological property of the fibrous composite electrorheological fluid is measured by a cylinder measuring method of a rotary rheometer, and the dynamic shear strength of the fibrous composite electrorheological fluid is measuredShear rate at controlled rate of 1S-1Measured under the conditions. The dynamic shear stress is measured in relation to the electric field strength as shown in FIG. 3. The suspension stability of the fibrous composite electrorheological fluid is measured by adopting a standing observation method, and the relationship between the standing anti-settling rate and the time is shown in figure 4.
Compared with comparative example 1, it is known that the fibrous composite electrorheological fluid obtained in the embodiment has higher dynamic shear stress and better suspension stability.
Example 2
Uniformly mixing 18ml of tetraethyl titanate and isopropanol according to the molar ratio of 1: 200, dropwise adding acetic acid to control the pH value of the solution to be 2, adding oxalic acid with the same molar number as that of the tetraethyl titanate under the stirring condition to react for 1 hour at 50 ℃ to form a composite solution A, then adding nano fibrous sepiolite (the diameter is 50nm and the length is 3 mu m) with the mass of 2 times of the oxalic acid into the composite solution A to prepare a mixed solution B, adding ammonia water into the mixed solution B under the stirring condition to adjust the pH value to be 5, and reacting for 2 hours at 20 ℃ to ensure that titanium oxyoxalate colloidal particles are coated on the surface of the sepiolite through heterogeneous nucleation. And after the reaction is completed, filtering, washing and drying the generated composite suspension to obtain the sepiolite @ titanyl oxalate particles. The fibrous sepiolite @ titanium oxyoxalate particles and methyl silicone oil are uniformly mixed to prepare the fibrous composite electrorheological fluid with the volume concentration of the sepiolite @ titanium oxyoxalate particles being 20%. When an external electric field V is 4.0kV/mm, the dynamic shearing application of the electrorheological fluid is 28 kPa; the sedimentation resistance after 500 hours of standing was 99%.
Example 3
Uniformly mixing 16ml of tetraisopropyl titanate and n-butanol according to the molar ratio of 1: 100, controlling the pH value of the solution to be 1 by dropwise adding acetic acid, adding oxalic acid with the same molar number as that of the tetraisopropyl titanate under the stirring condition to react for 3 hours at 0 ℃ to form a composite solution A, then adding fibrous sepiolite (the diameter is 30nm and the length is 1.5 mu m) with the mass of 1 time of the oxalic acid into the composite solution A to prepare a mixed solution B, adding ammonia water into the mixed solution B under the stirring condition to adjust the pH value to be 4, and reacting for 10 hours at 0 ℃ to ensure that titanium oxyoxalate colloidal particles are coated on the surface of the fibrous sepiolite through nucleation heterogeneous phase. And after the reaction is completed, filtering, washing and drying the generated composite suspension to obtain the nano fibrous sepiolite @ titanyl oxalate particles. The particles are evenly mixed with methyl silicone oil to prepare the fibrous composite electrorheological fluid of which the volume concentration of the attapulgite/titanyl oxalate particles is 10 percent. When the applied electric field V is 4.0kV/mm, the dynamic shearing application of the electrorheological fluid is 25.5 kPa; the sedimentation resistance after 500 hours of standing was 97%.
In conclusion, by the technical scheme, the fibrous composite electrorheological fluid obtained by the invention has the advantages of large dynamic shear stress, low leakage current density, good suspension stability and the like, and has the advantages of wide raw material source, low cost, simple process and short preparation period.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. The fibrous composite electrorheological fluid is characterized by comprising a dispersion phase and a dispersion medium, wherein the dispersion medium comprises an insulating liquid, the dispersion phase is uniformly dispersed in the dispersion medium, the dispersion phase comprises fibrous sepiolite-titanyl oxalate composite particles, and the fibrous sepiolite-titanyl oxalate composite particles are formed by coating titanyl oxalate particles on the surface of sepiolite with a fibrous structure.
2. The fibrous composite electrorheological fluid of claim 1, characterized in that: the mass ratio of the fibrous sepiolite to the titanyl oxalate in the fibrous sepiolite-titanyl oxalate composite particles is 1: 0.2-2;
and/or the content of the fibrous sepiolite-titanyl oxalate composite particles in the fibrous composite electrorheological fluid is 10-20 vol%.
3. The fibrous composite electrorheological fluid of claim 1, characterized in that: the diameter of the fibrous sepiolite is 20-50 nm, and the length of the fibrous sepiolite is 0.5-3 mu m; and/or the insulating liquid comprises methyl silicone oil and/or hydroxyl silicone oil.
4. A method for preparing fibrous composite electrorheological fluid is characterized by comprising the following steps:
mixing a mixed solution containing organic titanate and an organic alcohol solvent with oxalic acid, and reacting at 0-50 ℃ for 1-3 h to form a mixed reaction system;
adding fibrous sepiolite into the mixed reaction system, and reacting for 2-10 h at 0-20 ℃, so that the formed titanium oxyoxalate colloid particles are coated on the surface of the fibrous sepiolite through heterogeneous nucleation, thereby obtaining fibrous sepiolite-titanium oxyoxalate composite particles;
and uniformly dispersing the fibrous sepiolite-titanyl oxalate composite particles in insulating liquid to obtain the fibrous composite electrorheological fluid.
5. The method of claim 4, wherein: the mol ratio of the organic titanate to the organic alcohol solvent is 1: 100-200 parts of; and/or the molar ratio of the organic titanate to the oxalic acid is 1: 1.
6. the production method according to claim 4, characterized by comprising: adjusting the pH value of the mixed solution to 1-2 by adopting an acidic substance; preferably, the acidic substance comprises any one or a combination of more than two of acetic acid, hydrochloric acid and nitric acid.
7. The method of claim 4, wherein: the organic titanate comprises one or the combination of more than two of tetrabutyl titanate, tetraethyl titanate and tetraisopropyl titanate; and/or the organic alcohol solvent comprises any one or the combination of more than two of ethanol, isopropanol and n-butanol.
8. The production method according to claim 4, characterized by comprising: adding fibrous sepiolite into the mixed reaction system, reacting for 2-10 h at 0-20 ℃, adding an alkaline substance into the mixed reaction system under the stirring condition, and adjusting the pH value of the mixed reaction system to 4-5, so that the formed titanium oxyoxalate colloid particles are coated on the surface of the fibrous sepiolite through heterogeneous nucleation to obtain fibrous sepiolite-titanium oxyoxalate composite particles; preferably, the alkaline substance comprises ammonia;
preferably, the preparation method further comprises: and after the reaction is finished, filtering, washing and drying the obtained reaction liquid to obtain the fibrous sepiolite-titanyl oxalate composite particles.
9. The method of claim 4, wherein: the mass ratio of the fibrous sepiolite to the oxalic acid is 1-2: 1; and/or the fibrous sepiolite has a diameter of 20-50 nm and a length of 0.5-3 μm;
and/or the insulating liquid comprises methyl silicone oil and/or hydroxyl silicone oil.
10. An electrorheological fluid of fibrous composite material prepared by the process according to any one of claims 4 to 9.
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