CN108441287A

CN108441287A - A kind of preparation method of the nano combined er materials of Mxene/PS

Info

Publication number: CN108441287A
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: 2018-08-24
Anticipated expiration: 2038-04-25
Also published as: CN108441287B

Abstract

The invention belongs to nana intelligent technical field of composite materials, disclose a kind of technology of preparing with electrorheological property material, a kind of novel nano-dispersed stabilizer is obtained by etching, aoxidizing Mxene, and Mxene/ poly styrene composite materials are prepared using one step of Pickering emulsion polymerizations；Including etching the preparation of Mxene, aoxidizing the preparation of Mxene and being mixed with step；Its preparation process is simple, it is easy to operate, Mxene after oxidation is with higher boundary's electrical property, compared to pure titinium dioxide, Mxene after oxidation has C layers, with the electric conductivity for meeting electric current change, dispersion stabilizer is cooked with the Mxene after oxidation, passes through the method synthesis oxidation Mxene/PS of emulsion polymerization, under the action of extra electric field, with higher shear stress and lower leakage current density, there are excellent ER properties, used raw material is simple and easy to get in experiment, it is at low cost, clean nontoxic, the reaction time is shorter, is with a wide range of applications.

Description

A kind of preparation method of the nano combined er materials of Mxene/PS

Technical field：

The invention belongs to nana intelligent technical field of composite materials, disclose a kind of preparation with electrorheological property material Technology obtains a kind of novel nano-dispersed stabilizer by etching, aoxidizing Mxene, and utilizes Pickering (pik woods) breasts One step of liquid polymerization prepares Mxene/ polystyrene (PS) composite material.

Background technology：

ER fluid is a kind of intellectual material by electric field controls, and oil (such as dimethyl of insulation is dispersed in by polarizable particles Silicone oil, hydrocarbon ils, mineral oil, corn oil etc.) it forms, polarizable particles form chain structure under the action of extra electric field, and Shear stress increases with the increase of extra electric field, and by controlling external electrical field, ER fluid may be implemented from liquid to solid-state Can convert, change the rheology and viscoelastic property of liquid.Estimated current becomes liquid, and that there are still particle suspension stabilities is poor, leaks electricity The shortcomings of current density is larger and the response time is slower, cannot meet the needs of engineer application.Therefore, seeking offer one kind has The preparation side of the nano combined er materials of Mxene/PS of high dispersion stability, high shear yield stress and low leakage current density Method is with good economic efficiency and social benefit.

Invention content：

It is an object of the invention to overcome defect of the existing technology, seek to design a kind of nano combined electricity of Mxene/PS The preparation method of rheo-material.

To achieve the above object, the nano combined er material preparation processes of Mxene/PS of the present invention, including with Lower step：

(1) preparation of Mxene is etched：Weigh the raw material Ti of 3~7g₃AlC₂, then with plastic cylinder measure 50~100ml hydrogen Fluoric acid is placed in plastic bottle, by raw material Ti₃AlC₂It is added slowly in hydrofluoric acid, 50 is stirred under the rotating speed of 200~500rmp ~90h is cleaned with deionized water to neutrality, Mxene after freeze-drying is etched；

(2) preparation of Mxene is aoxidized：Mxene after first weighing 0.5~0.9g etchings with electronic balance is placed in 100ml and burns Cup in, then with graduated cylinder measure 50~100ml the ultra-pure water (Mxene after etching：UP~1：100) it is placed in beaker, by super Sound wave cell disruptor crushes 20~50min of processing by Mxene is aoxidized, and is then added to 1~2ml hydrogen peroxide above-mentioned It in solution, is uniformly dispersed, above-mentioned mixed solution is transferred in 200ml reaction kettles, 15~25h of hydro-thermal at 180~220 DEG C, Freeze-drying obtains oxidation Mxene after the Off-white product obtained after reaction cleans 3~6 times with deionized water.

(3) further, it takes the oxidation Mxene that 0.1~0.4g steps (2) obtain to be dispersed in 5~20ml ultra-pure waters, surpasses Sound obtains uniform MXene reaction solutions for 10 minutes, and 2.0~3.5ml styrene is dissolved in the ethanol solution of 30~50ml, Magnetic agitation obtains uniform styrene reaction solution, then uniformly mixes MXene reaction solutions with styrene reaction solution, 15~30min is crushed using cell disruptor, is then placed in flask, 0.01~0.06mg initiations are added after leading to nitrogen 30min Agent azodiisobutyronitrile (AIBN：Styrene~1:100), 8~14h of mechanical agitation at 50~70 DEG C, afterwards with deionized water and Freeze-drying obtains finished product, the i.e. nano combined er materials of Mxene/PS after methanol cleans 3~6 times.

Compared with prior art, the present invention its preparation process is simple, easy to operate, the Mxene after oxidation is with higher Boundary's electrical property, compared to pure titinium dioxide, the Mxene after oxidation has C layers, has the electric conductivity for meeting electric current change, with oxidation Mxene afterwards cooks dispersion stabilizer, by the method synthesis oxidation Mxene/PS of emulsion polymerization, under the action of extra electric field, With higher shear stress and lower leakage current density, there are excellent ER properties, used original in experiment Expect it is simple and easy to get, it is at low cost, cleaning it is nontoxic, the reaction time is shorter, is with a wide range of applications.

Description of the drawings：

Fig. 1 is the transmission electron microscope figure of oxidation Mxene/PS nanocomposites prepared by embodiment.

Fig. 2 is the scanning electron microscope diagram of oxidation Mxene/PS nanocomposites prepared by the present invention.

Fig. 3 is the ER properties figure of oxidation Mxene/PS nanocomposites prepared by embodiment.

Specific implementation mode：

It further illustrates by way of example and in conjunction with the accompanying drawings.

Embodiment 1：

The present embodiment is chosen oxidation Mxene and is combined with polystyrene spheres, and specific preparation process is：

(1) preparation of Mxene is etched：The raw material Ti of 5g is first weighed with electronic balance₃AlC₂, then measured with plastic cylinder The hydrofluoric acid of 75ml is placed in plastic bottle, by raw material Ti₃AlC₂It is added slowly in hydrofluoric acid, is stirred under the rotating speed of 250rmp 72h is mixed, is cleaned to neutrality with deionized water, Mxene after freeze-drying is etched；

(2) preparation of Mxene is aoxidized：Mxene after first weighing 0.7g etchings with electronic balance is placed in 100ml beakers, The UP water for measuring 70ml with graduated cylinder again is placed in beaker, then 1.5ml hydrogen peroxide is added to above-mentioned by cell pulverization 30min It in solution, is uniformly dispersed, above-mentioned mixed solution is transferred in 200ml reaction kettles, the hydro-thermal 20h at 200 DEG C, after reaction Freeze-drying obtains oxidation Mxene after obtained Off-white product cleans 3 times with deionized water.

(3) further, the oxidation Mxene that 0.3g steps (2) obtain is dispersed in 5ml UP water, ultrasonic 10min is obtained To uniform (a) solution, 2.5ml styrene is dissolved in the ethanol solution of 40ml, it is molten that magnetic agitation obtains uniform (b) Then liquid uniformly mixes (a) solution with (b) solution, crush 30min using cell disruptor, obtain (c) solution, then add Enter into round-bottomed flask, lead to nitrogen 30min, 0.025g AIBN, the mechanical agitation 10h at 65 DEG C, obtained ash are added later Freeze-drying obtains oxidation Mxene/PS ball composite materials after white product deionized water and methanol are respectively washed 3 times.

The nano combined er materials of Mxene/PS manufactured in the present embodiment are as depicted in figs. 1 and 2, illustrate that Mxene/PS receives Nano composite material successfully synthesizes, and size is more uniform；It is not having with excellent ER properties as shown in Figure 3 In the case of having extra electric field, Newtonian fluid is showed；When there is extra electric field, shear stress with the increase of extra electric field and by It is cumulative to add.

Claims

1. a kind of preparation method of the nano combined er materials of Mxene/PS, it is characterised in that specific preparation process, including with Lower step：

(1) preparation of Mxene is etched：Weigh the raw material Ti of 3~7g₃AlC₂, then with plastic cylinder measure 50~100ml hydrofluoric acid It is placed in plastic bottle, by raw material Ti₃AlC₂Be added slowly in hydrofluoric acid, under the rotating speed of 200~500rmp stir 50~ 90h is cleaned with deionized water to neutrality, Mxene after freeze-drying is etched；

(2) preparation of Mxene is aoxidized：Mxene after first weighing 0.5~0.9g etchings with electronic balance is placed in 100ml beakers, The ultra-pure water for measuring 50~100ml with graduated cylinder again is placed in beaker, and will aoxidize Mxene by ultrasonic cell disruptor carries out powder 1~2ml hydrogen peroxide, is then added in above-mentioned solution, is uniformly dispersed by 20~50min of broken processing, by above-mentioned mixed solution It is transferred in 200ml reaction kettles, 15~25h of hydro-thermal at 180~220 DEG C, the Off-white product obtained after reaction is spent Freeze-drying obtains oxidation Mxene after ionized water cleans 3~6 times.

(3) further, the oxidation Mxene that 0.1~0.4g steps (2) obtain is taken to be dispersed in 5~20ml ultra-pure waters, ultrasound 10 Minute obtains uniform MXene reaction solutions, 2.0~3.5ml styrene is dissolved in the ethanol solution of 30~50ml, magnetic force Uniform styrene reaction solution is stirred to get, then uniformly mixes MXene reaction solutions with styrene reaction solution, is used Cell disruptor crushes 15~30min, is then placed in flask, and 0.01~0.06mg initiator idols are added after leading to nitrogen 30min Nitrogen bis-isobutyronitrile, 8~14h of mechanical agitation at 50~70 DEG C, is freeze-dried after cleaning 3~6 times with deionized water and methanol afterwards Obtain finished product, the i.e. nano combined er materials of Mxene/PS.