CN108441287B

CN108441287B - Preparation method of Mxene/PS nano composite electrorheological material

Info

Publication number: CN108441287B
Application number: CN201810380211.0A
Authority: CN
Inventors: 张文玲; 刘迎丹; 郑雯
Original assignee: Qingdao University
Current assignee: Qingdao University
Priority date: 2018-04-25
Filing date: 2018-04-25
Publication date: 2020-12-15
Anticipated expiration: 2038-04-25
Also published as: CN108441287A

Abstract

The invention belongs to the technical field of nano intelligent composite materials, and discloses a preparation technology of a material with electrorheological property, wherein a novel nano dispersion stabilizer is obtained by etching and oxidizing Mxene, and the Mxene/polystyrene composite material is prepared by a Pickering emulsion polymerization method in one step; the method comprises the steps of preparation of etching Mxene, preparation of oxidizing Mxene and mixed preparation; the preparation process is simple, the operation is convenient, the oxidized Mxene has higher electrical performance, compared with pure titanium dioxide, the oxidized Mxene has a C layer and has conductivity meeting electrorheological property, the oxidized Mxene is used as a dispersion stabilizer, the oxidized Mxene/PS is synthesized by an emulsion polymerization method, under the action of an external electric field, the oxidized Mxene/PS has higher shear stress and lower leakage current density, and has excellent electrorheological property.

Description

Preparation method of Mxene/PS nano composite electrorheological material

The technical field is as follows:

the invention belongs to the technical field of nano intelligent composite materials, and discloses a preparation technology of a material with electrorheological property.

Background art:

the electrorheological fluid is an intelligent material controlled by an electric field, and consists of polarized particles dispersed in insulating oil (such as dimethyl silicone oil, hydrocarbon oil, mineral oil, corn oil and the like), the polarizable particles form a chain structure under the action of an external electric field, the shearing stress is increased along with the increase of the external electric field, and the conversion of the electrorheological fluid from a liquid state to a solid state can be realized by controlling the external electric field, so that the rheological and viscoelastic properties of the fluid are changed. The current electrorheological fluid still has the defects of poor particle suspension stability, larger leakage current density, slower response time and the like, and can not meet the requirements of engineering application. Therefore, the preparation method of the Mxene/PS nano composite electrorheological material with high dispersion stability, high shear yield stress and low leakage current density is sought to be provided, and the Mxene/PS nano composite electrorheological material has good economic benefit and social benefit.

The invention content is as follows:

the invention aims to overcome the defects in the prior art and seek to design a preparation method of an Mxene/PS nano composite electrorheological material.

In order to realize the aim, the preparation process of the Mxene/PS nano composite electrorheological material comprises the following steps:

(1) preparation of etched Mxene: weighing 3-7 g of raw material Ti₃AlC₂Then, 50-100 ml of hydrofluoric acid is measured by a plastic measuring cylinder and placed in a plastic bottle, and the raw material Ti₃AlC₂Slowly adding the mixture into hydrofluoric acid, stirring for 50-90 hours at a rotating speed of 200-500 rmp, cleaning the mixture to be neutral by using deionized water, and freeze-drying the mixture to obtain etched Mxene;

(2) preparation of oxidized Mxene: firstly, 0.5-0.9 g of etched Mxene is weighed by an electronic balance and placed in a 100ml beaker, then 50-100 ml of ultrapure water (UP-1: 100) is weighed by a measuring cylinder and placed in the beaker, the Mxene oxide is crushed for 20-50 min by an ultrasonic cell crusher, then 1-2 ml of hydrogen peroxide is added into the solution and uniformly dispersed, the mixed solution is transferred into a 200ml reaction kettle, hydrothermal reaction is carried out for 15-25 h at 180-220 ℃, after the reaction is finished, an off-white product is washed for 3-6 times by deionized water and then is frozen and dried, and the Mxene oxide is obtained.

(3) Further, 0.1-0.4 g of the oxidized Mxene obtained in the step (2) is dispersed in 5-20 ml of ultrapure water, ultrasonic treatment is carried out for 10 minutes to obtain a uniform MXene reaction solution, 2.0-3.5 ml of styrene is dissolved in 30-50 ml of ethanol solution, magnetic stirring is carried out to obtain a uniform styrene reaction solution, then the MXene reaction solution and the styrene reaction solution are uniformly mixed, a cell crusher is used for crushing for 15-30 min, then the obtained product is placed in a flask, nitrogen is introduced for 30min, 0.01-0.06 mg of initiator azobisisobutyronitrile (AIBN: styrene-1: 100) is added, mechanical stirring is carried out for 8-14 h at 50-70 ℃, then deionized water and methanol are used for cleaning for 3-6 times, and freeze drying is carried out to obtain a finished product, namely the Mxene/PS nano composite electrorheological material.

Compared with the prior art, the preparation process is simple, the operation is convenient, the oxidized Mxene has higher electric performance, compared with pure titanium dioxide, the oxidized Mxene has a C layer and has electric conductivity conforming to electrorheological property, the oxidized Mxene is used as a dispersion stabilizer, the oxidized Mxene/PS is synthesized by an emulsion polymerization method, under the action of an external electric field, the oxidized Mxene/PS has higher shear stress and lower leakage current density, and has excellent electrorheological property.

Description of the drawings:

FIG. 1 is a transmission electron microscope image of the oxidized Mxene/PS nanocomposite prepared in the example.

FIG. 2 is a scanning electron microscope image of an oxidized Mxene/PS nanocomposite prepared according to the present invention.

FIG. 3 is a graph of the electrorheological properties of the oxidized Mxene/PS nanocomposites prepared in the examples.

The specific implementation mode is as follows:

the following is a further description by way of example and with reference to the accompanying drawings.

Example 1:

in this embodiment, an oxene oxide is selected to be combined with polystyrene spheres, and the specific preparation process is as follows:

(1) preparation of etched Mxene: firstly, 5g of raw material Ti is weighed by an electronic balance₃AlC₂Measuring 75ml of hydrofluoric acid by using a plastic measuring cylinder, placing the hydrofluoric acid into a plastic bottle, and taking the raw material Ti₃AlC₂Slowly adding the mixture into hydrofluoric acid, stirring for 72 hours at the rotating speed of 250rmp, cleaning the mixture to be neutral by using deionized water, and freeze-drying the mixture to obtain etched Mxene;

(2) preparation of oxidized Mxene: 0.7g of etched Mxene is weighed by an electronic balance and placed in a 100ml beaker, 70ml of UP water is weighed by a measuring cylinder and placed in the beaker, cells are crushed for 30min, 1.5ml of hydrogen peroxide is added into the solution and uniformly dispersed, the mixed solution is transferred into a 200ml reaction kettle, the mixed solution is heated for 20h under 200 ℃, an off-white product obtained after the reaction is finished is washed for 3 times by deionized water and then is frozen and dried to obtain the Mxene oxide.

(3) Further, 0.3g of the oxidized Mxene obtained in the step (2) is dispersed in 5ml of UP water, ultrasonic treatment is carried out for 10min to obtain a uniform solution (a), 2.5ml of styrene is dissolved in 40ml of ethanol solution, magnetic stirring is carried out to obtain a uniform solution (b), then the solution (a) and the solution (b) are uniformly mixed, a cell crusher is used for crushing for 30min to obtain a solution (c), then the solution (c) is added into a round-bottom flask, nitrogen is introduced for 30min, then 0.025g of AIBN is added, mechanical stirring is carried out for 10h at 65 ℃, obtained off-white products are respectively washed for 3 times by deionized water and methanol, and then freeze drying is carried out to obtain the oxidized Mxene/PS sphere composite material.

The Mxene/PS nanocomposite electrorheological material prepared in this example is shown in fig. 1 and fig. 2, which illustrates that the Mxene/PS nanocomposite material has been successfully synthesized and has a uniform size; as shown in fig. 3, the material has excellent electrorheological properties, and shows Newtonian fluid under the condition of no external electric field; when an external electric field is applied, the shearing stress is gradually increased along with the increase of the external electric field.

Claims

1. A preparation method of Mxene/PS nano composite electrorheological material is characterized in that the specific preparation process comprises the following steps:

(2) preparation of oxidized Mxene: firstly, weighing 0.5-0.9 g of etched Mxene by using an electronic balance, placing the Mxene in a 100ml beaker, then weighing 50-100 ml of ultrapure water by using a measuring cylinder, placing the ultrapure water in the beaker, crushing the Mxene by using an ultrasonic cell crusher for 20-50 min, then adding 1-2 ml of hydrogen peroxide into the solution, uniformly dispersing, transferring the mixed solution into a 200ml reaction kettle, carrying out hydrothermal treatment at 180-220 ℃ for 15-25 h, washing an off-white product obtained after the reaction for 3-6 times by using deionized water, and carrying out freeze drying to obtain the Mxene oxide;

(3) further, 0.1-0.4 g of the oxidized Mxene obtained in the step (2) is dispersed in 5-20 ml of ultrapure water, ultrasonic treatment is carried out for 10 minutes to obtain a uniform MXene reaction solution, 2.0-3.5 ml of styrene is dissolved in 30-50 ml of ethanol solution, magnetic stirring is carried out to obtain a uniform styrene reaction solution, then the MXene reaction solution and the styrene reaction solution are uniformly mixed, a cell crusher is used for crushing for 15-30 min, then the obtained product is placed in a flask, nitrogen is introduced for 30min, 0.01-0.06 mg of initiator azodiisobutyronitrile is added, mechanical stirring is carried out for 8-14 h at 50-70 ℃, deionized water and methanol are used for cleaning for 3-6 times, and freeze drying is carried out to obtain a finished product, namely the Mxene/PS nano composite electrorheological material.