CN110016804B - High-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid and preparation method thereof - Google Patents
High-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid and preparation method thereof Download PDFInfo
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- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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Abstract
The invention discloses a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid, which comprises the following raw materials in parts by weight: 140-160 parts of spherical silica, 30-50 parts of polyethylene glycol 400, 10-20 parts of polyethylene glycol 8005-10 parts of graphene and 1-4 parts of montmorillonite. The invention has the advantages of simple preparation process, low production cost and the like, more importantly, the shear thickening effect is obvious, the viscosity is high in the shearing process, the characteristic is obvious, the heat conducting property is excellent, and a new breakthrough is made in the characteristic of the flexible protective material prepared from the shear thickening liquid.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid and a preparation method thereof.
Background
Shear thickening fluids are generally in the form of liquids or dispersions, and when subjected to shear or impact exceeding a certain threshold, the viscosity of the shear thickening fluid rapidly increases, exhibiting the general resistance of a solid. When the external force is removed, the shear thickening fluid restores the original state, and the behavior is reversible non-Newtonian fluid behavior. The unique shear thickening property of the STF enables the STF to be widely applied to various protective materials.
STF is a nanoparticle solution in a solid-liquid mixed state, consisting of extremely fine silicon microparticles dispersed and suspended in an organic solvent. In the selection of the dispersion medium, the dispersion medium is generally required to be nontoxic, stable, not easy to deteriorate, wide in applicable temperature range, not too large in viscosity and certain in suspension capacity. Common dispersion media are Ethylene Glycol (EG), Propylene Glycol (PG), Butylene Glycol (BG), most commonly polyethylene glycol (PEG).
With the intensive research on the shear thickening liquid, the shear thickening characteristics of the shear thickening liquid are found to have different strengths in the mixture ratios of different raw materials, and in the compression-resistant and shock-proof field, the more obvious the shear thickening characteristics are, the better the finished product effect is.
Disclosure of Invention
In order to solve the problems in the prior art, the applicant of the present invention provides a high viscosity heat dissipation ultraviolet resistant shear thickening liquid and a preparation method thereof. The invention has the advantages of simple preparation process, low production cost and the like, more importantly, the shear thickening effect is obvious, the viscosity is high in the shearing process, the characteristic is obvious, the heat conducting property is excellent, and a new breakthrough is made in the characteristic of the flexible protective material prepared from the shear thickening liquid.
The technical scheme of the invention is as follows:
a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid comprises the following raw materials in parts by weight: 140-160 parts of spherical silica, 30-50 parts of polyethylene glycol 400, 10-20 parts of polyethylene glycol 8005-10 parts of graphene and 1-4 parts of montmorillonite.
The particle size of the graphene is 2-10 nm; the particle size of the spherical silica particles is 10-20 nm, and the particle size of the montmorillonite particles is 150-200 nm.
A preparation method of a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid comprises the following steps:
(1) adding 1-4 parts of montmorillonite, 5-10 parts of graphene and 140-160 parts of spherical nano-silica particles into 40-70 parts of a mixed solution of polyethylene glycol 400 and polyethylene glycol 800 at the temperature of 25 ℃, starting an ultrasonic wave and a constant speed stirrer, wherein the ultrasonic wave is 20000-30000 Hz, the rotating speed of the constant speed stirrer is 1200r/min, adding 1 part of graphene after adding 25 parts of spherical nano-silica particles, circulating in a reciprocating manner, finally adding 1-4 parts of montmorillonite, and dispersing for 60-100 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, standing for 12-20 hours at the temperature of 25-45 ℃, removing bubbles, and obtaining stable high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid; the raw materials are calculated according to parts by mass.
The high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid is used for compounding fiber fabrics by padding, spraying or plastic package technology.
The graphene is pretreated, and the pretreatment method comprises the following steps: mixing nano-sized graphene with a silane coupling agent KH570, dissolving in absolute ethyl alcohol, and performing ultrasonic dispersion, suction filtration and vacuum drying to obtain the surface-modified nano-graphite.
The mass ratio of the graphene to the silane coupling agent KH570 is 1: 5-20; the dosage of the absolute ethyl alcohol is 15-30 times of the total mass of the graphite and the silane coupling agent KH 570.
And carrying out freeze drying treatment on the pretreated graphene.
The montmorillonite is treated by a cationic surfactant cetyl trimethyl ammonium bromide, the mass ratio of the montmorillonite to the cetyl trimethyl ammonium bromide is 5: 3-3.5, and the mass ratio of the montmorillonite to the aqueous solution is 20-30: 1.
The beneficial technical effects of the invention are as follows:
besides conventional silica particles, graphene is also added to the used dispersed phase. Graphene is a single-layer sheet-like structure carbon material composed of honeycomb carbon, has the thickness of about 0.334nm, has the advantages of large specific surface area, good thermal stability and chemical stability, strong hydrophobicity, easiness in chemical modification and the like, and has ultrahigh thermal conductivity (about 5000 W.m < -1 >. K < -1 >), and the properties enable the graphene to be better applied to the field of heat conduction materials. Graphene is a two-dimensional material, the van der Waals acting force between layers of graphene is weak, and the graphene has excellent friction characteristics, so that the flow property of the graphene is better than that of common shear thickening liquid, particles are agglomerated under the action of shear stress, and the graphene layers have smaller friction force and can drive silicon dioxide particles to be agglomerated together more quickly, so that the critical viscosity is achieved at a lower shear rate, and the viscosity is higher than that of the common shear thickening liquid, so that the graphene has a better effect in the aspects of compression resistance and shock absorption.
The pretreated graphene is subjected to surface modification, the graphene is dispersed as a result of combination of large steric hindrance and strong electrostatic interaction between the graphene and modifier molecules, the surfactant molecules are adsorbed on two sides of graphene sheet layers, and aggregation between the graphene sheet layers can be effectively avoided by virtue of electrostatic repulsion or van der Waals force, so that the graphene is dispersed more uniformly in a solution. The added montmorillonite has strong adsorption capacity and cation exchange performance, and has good ultraviolet resistance.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the present invention.
FIG. 2 is a schematic view of a padding process for compounding a shear thickening fluid with a fabric according to the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
A preparation method of a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid comprises the following steps:
(1) at the temperature of 25 ℃, adding 1 part of montmorillonite, 5 parts of graphene and 140 parts of spherical nano-silica particles into a mixed solution of 30 parts of polyethylene glycol 400 and 10 parts of polyethylene glycol 800, turning on an ultrasonic wave and a constant speed stirrer, wherein the ultrasonic wave is 25000 Hz, the rotating speed of the constant speed stirrer is 1200r/min, adding 1 part of graphene after adding 25 parts of spherical nano-silica particles, performing reciprocating circulation, finally adding 1 part of montmorillonite, and dispersing for 80 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, standing for 16 hours at the temperature of 30 ℃, removing bubbles, and obtaining stable high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid; the raw materials are calculated according to parts by mass.
Example 2
A preparation method of a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid comprises the following steps:
(1) adding 2 parts of montmorillonite, 7 parts of graphene and 150 parts of spherical nano-silica particles into a mixed solution of 40 parts of polyethylene glycol 400 and 15 parts of polyethylene glycol 800 at the temperature of 25 ℃, starting an ultrasonic wave and a constant speed stirrer, wherein the ultrasonic wave is 25000 Hz, the rotating speed of the constant speed stirrer is 1200r/min, adding 1 part of graphene after adding 25 parts of spherical nano-silica particles, circulating in a reciprocating manner, finally adding 2 parts of montmorillonite, and dispersing for 80 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, standing for 16 hours at the temperature of 25 ℃, removing bubbles, and obtaining stable high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid; the raw materials are calculated according to parts by mass.
Example 3
A preparation method of a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid comprises the following steps:
(1) adding 4 parts of montmorillonite, 10 parts of graphene and 160 parts of spherical nano-silica particles into a mixed solution of 50 parts of polyethylene glycol 400 and 20 parts of polyethylene glycol 800 at the temperature of 25 ℃, starting an ultrasonic wave and a constant speed stirrer, wherein the ultrasonic wave is 25000 Hz, the rotating speed of the constant speed stirrer is 1200r/min, adding 1 part of graphene after adding 25 parts of spherical nano-silica particles, circulating in a reciprocating manner, finally adding 4 parts of montmorillonite, and dispersing for 80 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, standing for 16 hours at the temperature of 25 ℃, removing bubbles, and obtaining stable high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid; the raw materials are calculated according to parts by mass.
The graphene is pretreated, and the pretreatment method comprises the following steps: mixing 0.2g of nano-sized graphene with 2g of silane coupling agent KH570, dissolving in 40g of absolute ethyl alcohol, performing ultrasonic dispersion for 10 hours, and performing suction filtration, wherein the filter cake is cleaned by the absolute ethyl alcohol; and (3) putting the filter cake into a vacuum drying oven, drying for 4h at 80 ℃, and crushing the filter cake to obtain the surface modified nano graphite, namely the graphene.
And carrying out freeze drying treatment on the pretreated graphene at the temperature of-30 ℃ and under the pressure of 5 Pa.
The montmorillonite is modified, and the modification method comprises the following steps: adding 10 parts of montmorillonite into 300 parts of aqueous solution, placing the mixture in an oven, heating the mixture to 70 ℃, taking out the mixture after 1 hour, stirring the mixture for 2 hours by using a constant-speed stirrer, adding 6 parts of hexadecyl trimethyl ammonium bromide, continuing stirring for 2 hours, standing the mixture for 1 hour, taking out the mixture, placing the mixture in an oven at 80 ℃, and taking out the mixture after 12 hours to obtain the montmorillonite.
Example 4
A preparation method of a high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid comprises the following steps:
(1) adding 4 parts of montmorillonite, 10 parts of graphene and 160 parts of spherical nano-silica particles into a mixed solution of 50 parts of polyethylene glycol 400 and 20 parts of polyethylene glycol 800 at the temperature of 25 ℃, starting an ultrasonic wave and a constant speed stirrer, wherein the ultrasonic wave is 25000 Hz, the rotating speed of the constant speed stirrer is 1200r/min, adding 1 part of graphene after adding 25 parts of spherical nano-silica particles, performing reciprocating circulation, finally adding 4 parts of montmorillonite, and dispersing for 80 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, standing for 16 hours at the temperature of 25 ℃, removing bubbles, and obtaining stable high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid; the raw materials are calculated according to parts by mass.
The montmorillonite is modified, and the modification method comprises the following steps: adding 10 parts of montmorillonite into 300 parts of aqueous solution, placing the mixture in an oven, heating the mixture to 70 ℃, taking out the mixture after 1 hour, stirring the mixture for 2 hours by using a constant-speed stirrer, adding 6 parts of hexadecyl trimethyl ammonium bromide, continuing stirring for 2 hours, standing the mixture for 1 hour, taking out the mixture, placing the mixture in an oven at 80 ℃, and taking out the mixture after 12 hours to obtain the montmorillonite.
Comparative example
150 parts by mass of 12nm spherical silica particles were gradually added to 50 parts by mass of a polyethylene glycol solution. And (2) at the temperature of 25 ℃, using ultrasonic waves and a constant speed stirrer, wherein the ultrasonic waves are 20000 Hz, the rotating speed of the constant speed stirrer is 1200r/min, after uniform dispersion, placing the mixture in a vacuum oven, standing the mixture for 10 hours at the temperature of 25 ℃, removing bubbles, and finally obtaining the shear thickening fluid with stable physical and chemical properties.
Test example:
1. and (3) viscosity testing: and opening the rotational rheometer, connecting the measuring rotor to the measuring head, and waiting for the host to automatically identify the model of the rotor. And (4) carrying out zero-gap correction, clicking a "↓" button to lift the measuring head by a certain height, and heating a proper amount of sample to the central position of the temperature control lower plate. Clicking a "↓" button to test the descending of the rotor, and cleaning redundant samples around the rotor according to the prompt. After cleaning, the lamina is lowered to the measurement position. After the test procedure was set, the viscosity of the products obtained in the examples and comparative examples was measured, and the results are shown in table 1 below.
TABLE 1
The table shows that the initial viscosity of the comparative example is 2 to 3 times of the initial viscosity of the example 1, 3 to 4 times of the initial viscosity of the example 2 and 5 to 6 times of the initial viscosity of the example 3, because the graphene is added, the self friction coefficient of the graphene is only 0.01, and the graphene is a two-dimensional material, and the slip is easy to occur between layers, so the initial viscosity of the example is small. The table shows that the maximum viscosity of example 3 is the largest, the theoretical young modulus of graphene reaches 1.0TPa, the inherent tensile strength is 130GPa, and the strong mechanical properties of the graphene can provide a strong support for the strength of the shear thickening fluid. The particle size of the graphene is small, the graphene belongs to a nanometer level, the graphene is easy to permeate and disperse into a dispersion medium, the use effect of particles is improved, and the graphene is of a lamellar structure, so that aggregation among particles in a thickening stage is facilitated, permeation into among spherical silicon dioxide particles is facilitated, and the shear thickening effect is improved. When the amount of the graphene is too large, the graphene is easy to agglomerate due to the pi-pi interaction between layers, and the maximum viscosity is reduced due to poor dispersibility. However, the graphene described in example 3 has improved dispersibility after pretreatment. Therefore, example 3 is the most effective in strength, and example 4 times.
2. Compounding the shear thickening fluid obtained in the embodiment and the comparative example with the ultra-high molecular weight polyethylene stable fabric through a padding technology, wherein the padding technology is specifically characterized in that a three-dipping and three-pressing mode is adopted, the pressure intensity of an upper pressing roller and a lower pressing roller is 0.2MPa, and the rotating speed of the pressing rollers is 1 rad/s; the test results are shown in table 2, wherein the test results are obtained by placing the test pieces on the same box body, irradiating the box body with the same light source (275W infrared lamp simulating infrared light source in sunlight), testing the temperature in the box body, and testing the performance of the product.
TABLE 2
| Time/min | 0 | 20 | 40 | 60 |
| Example 1 temperature/. degree.C | 25 | 35 | 41 | 55 |
| Example 2 temperature/. degree.C | 25 | 36 | 43 | 58 |
| Example 3 temperature/. degree.C | 25 | 41 | 47 | 62 |
| Example 4 temperature/. degree.C | 25 | 39 | 44 | 60 |
| Comparative example temperature/. degree.C | 25 | 30 | 36 | 47 |
As can be seen from the table, the temperature of the examples and the comparative examples is increased with the increase of time, and the growth of the examples is larger, because the graphene is added in the examples and has excellent heat-conducting property, so the shear thickening fluid of the examples also has excellent heat-conducting property.
3. The shear thickening fluid obtained in the examples and the comparative examples is coated on an ultra-high molecular weight polyethylene plain weave fabric, a simple ultraviolet lamp aging tester is manufactured by self according to the weather resistance experimental standard of the fiber, and the radiation intensity is 4000-4600 mu w/cm2The fabrics of the examples and comparative examples were each placed at a distance of 20cm or less from the uv lamp, and the filter was fixed between the fabric and the uv lamp so that the wavelength of the uv light transmitted through the filter was within the uv-sensitive wavelength band of the fiber. The samples treated by ultraviolet irradiation were taken out at intervals of a certain time, and tensile strength was measured, and the test results are shown in table 3.
TABLE 3
| Time/min | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| 0 | 190Mpa | 218Mpa | 252Mpa | 232Mpa | 150Mpa |
| 30 | 170Mpa | 193Mpa | 208Mpa | 198Mpa | 110Mpa |
| 60 | 140Mpa | 156Mpa | 182Mpa | 173Mpa | 50Mpa |
As can be seen from the data in the table, the tensile strength of the examples is reduced by a smaller amount than that of the comparative examples, so that the ultraviolet resistance of the examples is better, and due to the lamellar structure of the montmorillonite, the ultraviolet resistance of the material can be enhanced, and the tensile strength of the material can be increased.
Claims (3)
1. The high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid is characterized by comprising the following raw materials in parts by weight: 140-160 parts of spherical silica, 30-50 parts of polyethylene glycol 400, 10-20 parts of polyethylene glycol 800, 5-10 parts of graphene and 1-4 parts of montmorillonite;
the particle size of the graphene is 2-10 nm; the particle size of the spherical silica particles is 10-20 nm, and the particle size of the montmorillonite particles is 150-200 nm;
the graphene is pretreated, and the pretreatment method comprises the following steps: mixing nano-sized graphene with a silane coupling agent KH570, dissolving in absolute ethyl alcohol, and performing ultrasonic dispersion, suction filtration and vacuum drying to obtain surface-modified nano-graphite; the mass ratio of the graphene to the silane coupling agent KH570 is 1: 5-20; the dosage of the absolute ethyl alcohol is 15-30 times of the total mass of the graphite and the silane coupling agent KH 570; carrying out freeze drying treatment on the pretreated graphene;
the montmorillonite is modified, and the modification method comprises the following steps: adding 10 parts of montmorillonite into 300 parts of aqueous solution, placing the mixture in an oven, heating the mixture to 70 ℃, taking out the mixture after 1 hour, stirring the mixture for 2 hours by using a constant-speed stirrer, adding 6 parts of hexadecyl trimethyl ammonium bromide, continuing stirring for 2 hours, standing the mixture for 1 hour, taking out the mixture, placing the mixture in an oven at 80 ℃, and taking out the mixture after 12 hours to obtain the montmorillonite.
2. A method for preparing the high viscosity heat dissipating uv shear resistant thickening fluid of claim 1, comprising the steps of:
(1) adding 1-4 parts of montmorillonite, 5-10 parts of graphene and 140-160 parts of spherical nano-silica particles into 40-70 parts of a mixed solution of polyethylene glycol 400 and polyethylene glycol 800 at the temperature of 25 ℃, starting an ultrasonic wave and a constant speed stirrer, wherein the ultrasonic wave is 20000-30000 Hz, the rotating speed of the constant speed stirrer is 1200r/min, adding 1 part of graphene after adding 25 parts of spherical nano-silica particles, circulating in a reciprocating manner, finally adding 1-4 parts of montmorillonite, and dispersing for 60-100 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, standing for 12-20 hours at the temperature of 25-45 ℃, removing bubbles, and obtaining stable high-viscosity heat-dissipation ultraviolet-resistant shear thickening liquid; the raw materials are calculated according to parts by mass.
3. The use of the high viscosity, heat dissipating, uv shear resistant thickening fluid of claim 1 for the compounding of fabrics by padding, spraying or plastic packaging techniques.
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| US20090047520A1 (en) * | 2007-08-14 | 2009-02-19 | Korea Institute Of Science And Technology | Graphene hybrid material and method for preparing same using chemical vapor deposition |
| CN102733175A (en) * | 2011-04-08 | 2012-10-17 | 江南大学 | Multiple dispersed phase flame retardant shear thickening fluid, its preparation method and application thereof |
| CN102926211A (en) * | 2012-11-14 | 2013-02-13 | 北京化工大学 | Shear thickening fluid based on molecular colloid and preparation method and application of shear thickening fluid |
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| US20090047520A1 (en) * | 2007-08-14 | 2009-02-19 | Korea Institute Of Science And Technology | Graphene hybrid material and method for preparing same using chemical vapor deposition |
| CN102733175A (en) * | 2011-04-08 | 2012-10-17 | 江南大学 | Multiple dispersed phase flame retardant shear thickening fluid, its preparation method and application thereof |
| CN102926211A (en) * | 2012-11-14 | 2013-02-13 | 北京化工大学 | Shear thickening fluid based on molecular colloid and preparation method and application of shear thickening fluid |
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