CN108865331A - A kind of preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline - Google Patents

A kind of preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline Download PDF

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Publication number
CN108865331A
CN108865331A CN201810550647.XA CN201810550647A CN108865331A CN 108865331 A CN108865331 A CN 108865331A CN 201810550647 A CN201810550647 A CN 201810550647A CN 108865331 A CN108865331 A CN 108865331A
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aniline
fluid
polyaniline
preparation
compound
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张文玲
刘迎丹
王义茹
刘�文
管彤
刘昆
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Qingdao University
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Qingdao University
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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
    • C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
    • 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
    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/061—Carbides; Hydrides; Nitrides
    • 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
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/046—Polyamines, i.e. macromoleculars obtained by condensation of more than eleven amine monomers
    • 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
    • C10M2229/02—Unspecified siloxanes; Silicones
    • C10M2229/025—Unspecified siloxanes; Silicones used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02—Pour-point; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/04—Detergent property or dispersant property

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

The invention belongs to electric currents to become intellectual material technical field, be related to a kind of compound two-dimentional transition metal carbide ER fluid preparation method of polyaniline, and in particular to a kind of Ti3C2Tx/polyaniline(PANI)(Ti3C2Tx compound polyphenylamine) composite material by electric current become liquid technology of preparing；Ti is obtained by hf etching3C2Aniline (aniline) monomer is further adsorbed onto Ti by Electrostatic Absorption by Tx3C2The surface Tx, in Ti under ammonium persulfate initiation3C2The method of the surface Tx and interlayer in-situ polymerization；Main includes preparation Ti3C2Tx powder, the Ti of aniline intercalation3C2Tx mixed solution, prepare composite material, prepares ER fluid；Its ER fluid shear yield strength with higher and lower viscosity for preparing；Its preparation process is complete, good product effect, and stability is high, and application environment is friendly.

Description

A kind of preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline
Technical field：
The invention belongs to electric currents to become intellectual material technical field, be related to a kind of compound two-dimentional transition metal carbide of polyaniline A kind of ER fluid preparation method, and in particular to Ti3C2Tx/polyaniline(PANI)(Ti3C2Tx compound polyphenylamine) it is compound The technology of preparing of material current change liquid；Ti is obtained by hf etching3C2Tx further passes through Electrostatic Absorption for aniline (aniline) monomer is adsorbed onto Ti3C2The surface Tx, in Ti under ammonium persulfate initiation3C2The surface Tx and the side of interlayer in-situ polymerization Method.
Background technique：
ER fluid is a kind of novel intelligent material that liquid-solid phase can occur under the electric field and become, and the rheological equationm of state is in electric field The lower characteristic with quick response and reversible transition of effect.The advantageous feature of electric rheological effect, make its such as automobile absorber, from The fields such as clutch, biomedical devices are with a wide range of applications.Polyaniline (polyaniline, PANI) is a kind of common Er material, but due to its conductivity height cause leak electricity density it is big, polarizability is low, suspension stability is poor the disadvantages of, limit Its industrial application is made.In recent years, researcher's multi-pass is crossed it is compound with some inorganic material, has suitable surrender to obtain The ER fluid of intensity and suspension stability.MXene is a class two-dimensional transition metal carbide or carbonitride, is had unique Two-dimensional layered structure, biggish specific surface area and good electric conductivity, magnetic property and mechanical property, be widely used in energy storage, The multiple fields such as catalysis, absorption.Ti3C2Tx is new inorganic material MXene (Ti3C2Al the product after) etching has unique The features such as two-dimensional structure, higher specific surface area.Therefore, seek a kind of polyaniline composite Ti3C2Tx ER fluid preparation method tool There are good economic benefit and social benefit.
Summary of the invention：
In order to overcome the shortcomings of the prior art, seeking to design a kind of compound two-dimentional transition metal carbide electricity of polyaniline The preparation method of rheology liquid, by by aniline intercalation Ti3C2Tx and in-situ polymerization, are prepared for a kind of electric current with porous structure Become particle, so that lower leakage current is obtained, the ER fluid of good sedimentation stability.
To achieve the above object, the preparation of the compound two-dimentional transition metal carbide ER fluid of polyaniline of the present invention Technique includes the following steps：
(1) hydrofluoric acid that mass percent concentration is 49% is placed in plastic bottle according to the proportion, by titanium aluminum carbide powder By 1:The ratio of 18-25 is dissolved in hydrofluoric acid, and 30-45h is stirred at room temperature, and centrifugation is washed to neutrality, is freeze-dried, is obtained Ti3C2Tx powder；
(2) Ti for obtaining step (1)3C2Tx powder is dissolved in the mixing of 1.25mol/L aniline Yu 0.25mol/L phytic acid In aqueous solution, wherein Ti3C2The mass ratio of Tx powder and aniline is 1:4-8, ultrasound stir 18h after about 8-12min is uniformly dissolved, So that aniline and Ti3C2Sufficient electrostatic reaction, which occurs, for Tx makes aniline be attached to Ti3C2On Tx, the Ti of aniline intercalation is obtained3C2Tx Mixed solution；
(3) in ice-water bath (heat release during due to aniline polymerization, in order to maintain constant reaction temperature), standing is not stirred Under the conditions of to aniline intercalation obtained by step (2) Ti3C2Tx mixed solution and dripping 1mol/L ammonium persulfate aqueous solution causes poly- Close, it is to be polymerized completely after, washing freeze-drying obtain to make aniline polymerization obtain polyaniline composite Ti3C2Tx material；
(4) the polyaniline composite Ti for obtaining step (3)3C2Tx material be added 1-5 times of volume ratio pure water, then to its Dropwise addition sodium hydrate aqueous solution adjusts pH value to 10, and stirring goes doping to make the reduction of its electric conductivity for 24 hours, and freezing is dry after being washed to neutrality Dry, the ratio after resulting powder is fully ground in the agate mortar with 20wt% obtains in being distributed in the silicone oil of 100cS Suspension turbula shaker sufficiently vibrate and form uniform polyaniline composite Ti3C2Tx ER fluid.
Further, in order to wash away excessive hydrofluoric acid, the washing process in step (1) is：Solution is transferred in centrifuge tube, Multiple centrifuge washing is carried out with ultrapure water, revolving speed is 5000 revs/min, and the time is 5 minutes.
Further, in order to wash away by-product, the impurity such as excess acid and aniline, the washing process in step (3) is：Solution It is transferred in centrifuge tube, carries out secondary centrifuging with ethyl alcohol and wash, revolving speed is 5000 revs/min, and the time is 5 minutes, uses ultrapure water Centrifuge washing three times is carried out, revolving speed is 5000 revs/min, and the time is 5 minutes.
Further, in order to make Ti3C2Tx/PANI composite material has porous structure, and the drying process in step (3) is： It is centrifuged channel closure and pricks hole, after being freezed with liquid nitrogen, drying 1 day in freeze drier is added, makes it dry completely.
Compared with prior art, the present invention at room temperature, pendulum strain amplitude scanning being carried out under the action of extra electric field and is surveyed The dynamic characteristic test of examination and angular frequency sweep test and rotational shear (relationship of viscosity, shear stress and shear rate), can To find out the ER fluid shear yield strength with higher and lower viscosity of its preparation；Its preparation process is complete, product Effect is good, and stability is high, and application environment is friendly.
Detailed description of the invention：
Fig. 1 is polyaniline composite Ti prepared by the present invention3C2Transmission electron microscope figure of the Tx material in large area.
Fig. 2 is polyaniline composite Ti prepared by the present invention3C2Transmission electron microscope figure of the Tx material in smaller area.
Fig. 3 is polyaniline composite Ti prepared by the present invention3C2The shear stress and shear rate relational graph of Tx ER fluid.
Fig. 4 is polyaniline composite Ti prepared by the present invention3C2The viscosity and shear rate relational graph of Tx ER fluid.
Fig. 5 is polyaniline composite Ti prepared by the present invention3C2Storage/the loss modulus and strain stress relation figure of Tx ER fluid
Fig. 6 is polyaniline composite Ti prepared by the present invention3C2Storage/the loss modulus and angular frequency relationship of Tx ER fluid Figure.
Specific embodiment：
It is described further by way of example and in conjunction with the accompanying drawings.
Embodiment 1：
The polyaniline composite Ti that the present embodiment is related to3C2The material quality part of Tx material matches：1 part of titanium aluminum carbide, hydrogen fluorine 100 parts, 6 parts of aniline, 1.2 parts of phytic acid, 4 parts of ammonium persulfate, 1 part of sodium hydroxide, 30 parts of silicone oil of acid.
The Ti that the present embodiment is related to3C2The preparation process of Tx/PANI composite material specifically includes：
(1) hydrofluoric acid that mass percent concentration is 49% is placed in plastic bottle, titanium aluminum carbide powder is pressed 1:20 Ratio is dissolved in hydrofluoric acid, and 40h is stirred at room temperature, and centrifugation is washed to neutrality, is freeze-dried, is obtained Ti3C2Tx powder；
(2) Ti for obtaining step (1)3C2Tx powder is dissolved in the mixing of 1.25mol/L aniline Yu 0.25mol/L phytic acid In aqueous solution, wherein Ti3C2The mass ratio of Tx powder and aniline is 1:6, ultrasound stirs 18h after about 10min is uniformly dissolved, so that Aniline and Ti3C2Sufficient electrostatic reaction, which occurs, for Tx makes aniline be attached to Ti3C2On Tx, the Ti of aniline intercalation is obtained3C2Tx mixing Solution；
(3) to the Ti of the resulting aniline intercalation of step (2) under ice-water bath, unperturbed state3C2Tx mixed solution and dripping 1mol/L ammonium persulfate aqueous solution cause polymerization, be added dropwise volume be above-mentioned mixed solution half, it is to be polymerized completely after, wash it is cold It is lyophilized dry, obtains polyaniline composite Ti3C2Tx material；
(4) the polyaniline composite Ti for obtaining step (3)3C2Tx material be added 1-5 times of volume ratio pure water, then to its Dropwise addition sodium hydrate aqueous solution adjusts pH value to 10, and stirring goes doping to make the reduction of its electric conductivity for 24 hours, and freezing is dry after being washed to neutrality Dry, the ratio after resulting powder is fully ground in the agate mortar with 20wt% obtains in being distributed in the silicone oil of 100cS Suspension turbula shaker sufficiently vibrate and form uniform polyaniline composite Ti3C2Tx ER fluid.
Further, the washing process in step (1) is：Solution is transferred in centrifuge tube, with ultrapure water carry out repeatedly from Heart washing, revolving speed are 5000 revs/min, and the time is 5 minutes.
Further, the washing process in step (3) is：Solution is transferred in centrifuge tube, carries out secondary centrifuging with ethyl alcohol Washing, revolving speed are 5000 revs/min, and the time is 5 minutes, carry out centrifuge washing three times with ultrapure water, revolving speed is 5000 revs/min Clock, time are 5 minutes；.
Further, the drying process in step (3) is：It is centrifuged channel closure and pricks hole, after being freezed with liquid nitrogen, it is dry that freezing is added It is 1 day dry in dry machine.
As depicted in figs. 1 and 2, gained polyaniline composite Ti3C2In Tx material, PANI is by multiple Ti3C2Tx is connected；
The ER fluid of preparation is tested；It is shear stress and shear rate relational graph such as Fig. 3, it can be with from figure Find out that for shear yield strength of about 100Pa, shear yield strength is higher, and from figure when applying 1.5kV/mm voltage As can be seen that being lower than 10s in shear rate when applying different voltages-1When, shear stress is held essentially constant, and illustrates this hair The material current denaturation of bright preparation can stablize；Such as Fig. 4, this is rotational shear the result of dynamic test, is not applied as can be seen from the figure When added electric field, initial viscosity is about 40Pas, and null field initial viscosity is lower；Such as Fig. 5, this is swing shearing (strain amplitude scanning Test) result, it can be seen that when strain is about 0.0001%-0.004%, storage/loss modulus is kept approximately constant, explanation Material dynamic property in biggish range of strain is stablized；Such as Fig. 6, this is that (strain is 0.003% condition inferior horn to swing shearing Frequency scanning test) as a result, not under same electric field, it can be seen that in 0-100rad/s angular frequency range, storage/loss modulus is several It remains unchanged, illustrates that material dynamic property in biggish range of strain is stablized.

Claims (5)

1. a kind of preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline, it is characterised in that its preparation process Include the following steps：
(1) hydrofluoric acid that mass percent concentration is 49% is placed in plastic bottle, titanium aluminum carbide powder is pressed 1:The ratio of 18-25 Example is dissolved in hydrofluoric acid, and 30-45h is stirred at room temperature, and centrifugation is washed to neutrality, is freeze-dried, is obtained Ti3C2Tx powder；
(2) Ti for obtaining step (1)3C2Tx powder is dissolved in 1.25mol/L aniline and the mixing of 0.25mol/L phytic acid is water-soluble In liquid, wherein Ti3C2The mass ratio of Tx powder and aniline is 1:4-8, ultrasound stir 18h after about 8-12min is uniformly dissolved, so that Aniline and Ti3C2Sufficient electrostatic reaction, which occurs, for Tx makes aniline be attached to Ti3C2On Tx, the Ti of aniline intercalation is obtained3C2Tx mixing Solution；
(3) it in ice-water bath, does not stir under static conditions to the Ti of aniline intercalation obtained by step (2)3C2Tx mixed solution and dripping 1mol/L ammonium persulfate aqueous solution cause polymerization, it is to be polymerized completely after, washing freeze-drying obtain to obtain aniline polymerization Obtain polyaniline composite Ti3C2Tx material；
(4) the polyaniline composite Ti for obtaining step (3)3C2The pure water of 1-5 times of volume ratio is added in Tx material, then is added dropwise to it Sodium hydrate aqueous solution adjusts pH value to 10, and stirring goes doping to make the reduction of its electric conductivity for 24 hours, is freeze-dried after being washed to neutrality, Ratio after resulting powder is fully ground in the agate mortar with 20wt% obtains in being distributed in the silicone oil of 100cS Suspension turbula shaker, which sufficiently vibrates, forms uniform polyaniline composite Ti3C2Tx ER fluid.
2. the preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline according to claim 1, special Sign is that the washing process in the step (1) is：Solution is transferred in centrifuge tube, carries out multiple centrifuge washing with ultrapure water, Revolving speed is 5000 revs/min, and the time is 5 minutes, to wash away excessive hydrofluoric acid.
3. the preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline according to claim 1, special Sign is that the washing process in the step (3) is：Solution is transferred in centrifuge tube, is carried out secondary centrifuging with ethyl alcohol and is washed, turns Speed is 5000 revs/min, and the time is 5 minutes, carries out centrifuge washing three times with ultrapure water, and revolving speed is 5000 revs/min, and the time is 5 minutes, to wash away by-product, excess acid and aniline impurity.
4. the preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline according to claim 1, special Sign is that the drying process in the step (3) is：It is centrifuged channel closure and pricks hole, after being freezed with liquid nitrogen, be added in freeze drier It is 1 day dry, it makes it dry completely, so as to Ti3C2Tx/PANI composite material has porous structure.
5. the preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline according to claim 1, special Sign is that preparing material quality part proportion is：1 part of titanium aluminum carbide, 100 parts of hydrofluoric acid, 6 parts of aniline, 1.2 parts of phytic acid, ammonium persulfate 4 parts, 1 part of sodium hydroxide, 30 parts of silicone oil.
CN201810550647.XA 2018-05-31 2018-05-31 A kind of preparation method of the compound two-dimentional transition metal carbide ER fluid of polyaniline Pending CN108865331A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1376768A (en) * 2001-03-26 2002-10-30 西北工业大学 Nano-class composite polyphenylamine/montmorillonite material as electric rheologic liquid and its preparing process
CN104232251A (en) * 2014-08-28 2014-12-24 陕西师范大学 Polyaniline composite electrorheological fluid
CN106589362A (en) * 2016-12-22 2017-04-26 陕西科技大学 Polyaniline nano particle/two-dimensional layered titanium carbide composite material and low-temperature preparation method of polyaniline nano particle/two-dimensional layered titanium carbide composite material
CN106750277A (en) * 2016-12-05 2017-05-31 哈尔滨工业大学 A kind of MXene polyaniline composite materials and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1376768A (en) * 2001-03-26 2002-10-30 西北工业大学 Nano-class composite polyphenylamine/montmorillonite material as electric rheologic liquid and its preparing process
CN104232251A (en) * 2014-08-28 2014-12-24 陕西师范大学 Polyaniline composite electrorheological fluid
CN106750277A (en) * 2016-12-05 2017-05-31 哈尔滨工业大学 A kind of MXene polyaniline composite materials and preparation method thereof
CN106589362A (en) * 2016-12-22 2017-04-26 陕西科技大学 Polyaniline nano particle/two-dimensional layered titanium carbide composite material and low-temperature preparation method of polyaniline nano particle/two-dimensional layered titanium carbide composite material

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Application publication date: 20181123