CN108221383B - Preparation method and application of low-temperature-resistant shear thickening liquid - Google Patents
Preparation method and application of low-temperature-resistant shear thickening liquid Download PDFInfo
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- CN108221383B CN108221383B CN201810076408.5A CN201810076408A CN108221383B CN 108221383 B CN108221383 B CN 108221383B CN 201810076408 A CN201810076408 A CN 201810076408A CN 108221383 B CN108221383 B CN 108221383B
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
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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
- D06M11/79—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 with silicon dioxide, silicic acids or their salts
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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Abstract
The invention discloses a preparation method of low-temperature-resistant shear thickening liquid, which comprises the following steps: (1) adding 300-480 parts of positively charged micro-nano spherical silicon dioxide particles into 100-250 parts of a dispersion medium at the temperature of 25-55 ℃, adding 2 parts of polytetrafluoroethylene powder, stirring at the rotating speed of 800r/min by using a ribbon stirrer, and dispersing for 30-80 minutes to obtain a uniform dispersion liquid; (2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, and standing for 5-15 hours at the temperature of 25-55 ℃ to obtain a shear thickening liquid with obvious low temperature resistance effect; the raw materials are calculated according to parts by mass. The invention solves the problem that the normal shear thickening liquid fails due to freezing at low temperature, and makes a great breakthrough in the application range and use conditions of the flexible protective material prepared from the shear thickening liquid.
Description
Technical Field
The invention relates to the technical field of low-temperature-resistant materials, in particular to a method for preparing low-temperature-resistant shear thickening liquid by utilizing micro-nano spherical silicon dioxide particles and application thereof.
Background
Shear thickening fluids are generally in the form of liquids or dispersions, which rapidly increase in viscosity when subjected to shear or impact beyond a certain threshold, and exhibit the general resistance of solids. When the external force is removed, the shear thickening fluid restores the original state, which is a reversible non-Newtonian fluid behavior. The unique shear thickening property makes STF widely used in various protective materials. Since the protective material is often used in a severe low-temperature environment, the shear thickening liquid can be frozen in the low-temperature environment at present, so that the shear thickening behavior is ineffective, and the application range of the shear thickening liquid is greatly limited. Therefore, it is necessary to research and develop a shear thickening liquid which still has shear thickening behavior under the condition of-35 ℃ to-30 ℃.
Disclosure of Invention
Aiming at the problems in the prior art, the applicant provides a preparation method and application of a low-temperature-resistant shear thickening fluid. The method has the advantages of simple and convenient process, low production cost and the like, more importantly solves the problem that the normal shear thickening liquid fails due to freezing at low temperature, and makes great breakthrough in the application range and the use condition of the flexible protective material prepared from the shear thickening liquid.
The technical scheme of the invention is as follows:
a method of preparing a low temperature resistant shear thickening fluid, the method comprising the steps of:
(1) adding 300-480 parts of positively charged micro-nano spherical silicon dioxide particles into 100-250 parts of a dispersion medium at the temperature of 25-55 ℃, adding 2 parts of polytetrafluoroethylene powder, stirring at the rotating speed of 800r/min by using a ribbon stirrer, and dispersing for 30-80 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, and standing for 5-15 hours at the temperature of 25-55 ℃ to obtain a shear thickening liquid with obvious low temperature resistance effect; the raw materials are calculated according to parts by mass.
The preparation method of the micro/nano sphere-shaped silicon dioxide particles with positive charges comprises the following steps: taking SiO2Adding anhydrous toluene and 3-aminopropyltrimethoxysilane into the particles in a 1000mL four-mouth bottle, ultrasonically mixing for 30min, condensing and refluxing at 110 ℃, and magnetically stirring for 24 h; after the reaction is finished, repeatedly washing the reaction product by using deionized water, ethanol and acetone in sequence; then drying in vacuum at 50 ℃ to obtain the micro-nano sphere-shaped silicon dioxide particles with positive charges.
The SiO2The mass ratio of the anhydrous toluene to the 3-aminopropyltrioxymethylsilane is 300-480: 0.22: 0.005.
The particle diameter of the micro-nano sphere-shaped silicon dioxide particles with positive charges is 10 nm-10 mu m.
The dispersion medium is a polymer with negative charges, good temperature sensitivity, low temperature resistance and heat insulation.
The dispersion medium is a mixture of polyether polyol and silicone oil, wherein the polyether polyol contains 0.01% of anionic surfactant AS-1, and the molecular weight of the polyether polyol is 2000-8000; wherein the mass ratio of the polyether polyol to the silicone oil is 4-1: 1.
The application of the low-temperature-resistant shear thickening liquid can be used for preparing a flexible light protective material, and the protective material can be applied in the environment of the temperature of-35 ℃ to-30 ℃.
The low-temperature-resistant shear thickening liquid can be used for compounding the fiber fabric by a hand lay-up forming technology, a vacuum padding technology, a spraying technology or a plastic package technology.
The beneficial technical effects of the invention are as follows:
the applicant of the invention adopts polyether polyol and silicone oil as dispersion media, molecular chains containing C-O-C bonds on polyether polyol main chains are easy to rotate, the molecular chains have high flexibility and good low-temperature performance, and the heat conductivity coefficient is small; the silicone oil has a freezing point of less than-50 deg.C, thermal conductivity of 0.134-0.159W/M.K; the invention makes the disperse phase and the disperse medium respectively carry opposite charges, and the two phases can be better combined, so that the solution is more stable.
The invention adopts the polytetrafluoroethylene powder, which is low temperature resistant, and can keep 5% of elongation even if the temperature is reduced to-196 ℃, and the polytetrafluoroethylene powder, polyether glycol, silicone oil and other multiple components are mutually matched and act synergistically in the application of the invention, so that the low temperature resistant shear thickening liquid is finally prepared.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
FIG. 2 is a schematic view of a padding process for compounding the low temperature resistant shear thickening fluid and the fabric.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
A method of preparing a low temperature resistant shear thickening fluid, the method comprising the steps of:
(1) adding 80 parts of a mixture of 8000 parts of polyether polyol containing 0.01% of anionic surfactant AS-1 and 20 parts of silicone oil and 2 parts of polytetrafluoroethylene into a three-neck flask, and uniformly mixing to prepare a mixed dispersion medium;
(2) 300 parts of SiO with the particle size of 20nm2Putting the particles into a 1000mL four-mouth bottle, adding 250mL of anhydrous toluene and 5mL of 3-aminopropyltrimethoxysilane, ultrasonically mixing for 30min, condensing and refluxing at 110 ℃, and magnetically stirring for 24 h; after the reaction is finished, repeatedly washing the reaction product by using deionized water, ethanol and acetone in sequence; then vacuum drying is carried out at 50 ℃ to prepare micro-nano sphere silicon dioxide particles with positive charges;
(3) adding the micro-nano sphere silicon dioxide particles with positive charges prepared in the step (2) into the mixed dispersion medium prepared in the step (1), stirring the mixture at the temperature of 25 ℃ by using a ribbon stirrer at the rotating speed of 800r/min, and dispersing the mixture for 80 minutes to obtain uniform dispersion liquid;
(4) and (3) placing the dispersion liquid in a vacuum oven, standing for 10 hours at the temperature of 25 ℃, removing bubbles, and finally obtaining the shear thickening liquid with stable physical and chemical properties. The raw materials are calculated according to parts by mass.
Example 2
A method of preparing a low temperature resistant shear thickening fluid, the method comprising the steps of:
(1) adding 60 parts of a mixture of 8000 parts of polyether polyol containing 0.01% of anionic surfactant AS-1, 40 parts of silicone oil and 2 parts of polytetrafluoroethylene into a three-neck flask, and uniformly mixing to prepare a mixed dispersion medium;
(2) 400 parts of SiO with the particle size of 20nm2Putting the particles into a 1000mL four-mouth bottle, adding 250mL of anhydrous toluene and 5mL of 3-aminopropyltrimethoxysilane, ultrasonically mixing for 30min, condensing and refluxing at 110 ℃, and magnetically stirring for 24 h; after the reaction is finished, repeatedly washing the reaction product by using deionized water, ethanol and acetone in sequence; then vacuum drying is carried out at 50 ℃ to prepare micro-nano sphere silicon dioxide particles with positive charges;
(3) adding the micro-nano sphere silicon dioxide particles with positive charges prepared in the step (2) into the mixed dispersion medium prepared in the step (1), stirring the mixture at the temperature of 30 ℃ by using a ribbon stirrer at the rotating speed of 800r/min, and dispersing the mixture for 60 minutes to obtain uniform dispersion liquid;
(4) and (3) placing the dispersion liquid in a vacuum oven, standing for 8 hours at the temperature of 40 ℃, removing bubbles, and finally obtaining the shear thickening liquid with stable physical and chemical properties. The raw materials are calculated according to parts by mass.
Example 3
A method of preparing a low temperature resistant shear thickening fluid, the method comprising the steps of:
(1) adding 50 parts of a mixture of 8000 parts of polyether polyol containing 0.01% of anionic surfactant AS-1 and 50 parts of silicone oil and 2 parts of polytetrafluoroethylene into a three-neck flask, and uniformly mixing to prepare a mixed dispersion medium;
(2) 480 parts of SiO with the particle size of 20nm2Putting the particles into a 1000mL four-mouth bottle, adding 250mL of anhydrous toluene and 5mL of 3-aminopropyltrimethoxysilane, ultrasonically mixing for 30min, condensing and refluxing at 110 ℃, and magnetically stirring for 24 h; after the reaction is finished, repeatedly washing the reaction product by using deionized water, ethanol and acetone in sequence; then vacuum drying is carried out at 50 ℃ to prepare micro-nano sphere silicon dioxide particles with positive charges;
(3) adding the micro-nano sphere silicon dioxide particles with positive charges prepared in the step (2) into the mixed dispersion medium prepared in the step (1), stirring the mixture at the temperature of 40 ℃ by using a ribbon stirrer at the rotating speed of 800r/min, and dispersing the mixture for 30 minutes to obtain uniform dispersion liquid;
(4) and (3) placing the dispersion liquid in a vacuum oven, standing for 5 hours at the temperature of 50 ℃, removing bubbles, and finally obtaining the shear thickening liquid with stable physical and chemical properties. The raw materials are calculated according to parts by mass.
Comparative example
Adding 100 parts of polyethylene glycol into a three-neck flask, slowly adding 300 parts by mass of spherical silicon dioxide particles with the dispersed phase particle size of 20nm, uniformly dispersing at 25 ℃, then placing the dispersion in a vacuum oven, standing at 25 ℃ for 10 hours, removing bubbles, and finally obtaining the shear thickening fluid with stable physicochemical properties. The raw materials are calculated according to parts by mass.
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 samples obtained in the examples of the present invention was measured, and the measurement results are shown in table 1.
TABLE 1
From the data in Table 1, it can be seen that the initial and maximum viscosities and the critical shear rate at low temperature are higher for the examples than for the comparative examples, indicating that the low temperature resistance of the examples is better.
2. Respectively taking 100 parts by volume of each of the low-temperature-resistant shear thickening liquid obtained in the embodiments 1-3 and the comparative shear thickening liquid, respectively adding the low-temperature-resistant shear thickening liquid and the comparative shear thickening liquid into 300 parts by volume of absolute ethyl alcohol for dilution, and then compounding the low-temperature-resistant shear thickening liquid and the ultra-high molecular weight polyethylene stable fabric by using a padding technology, wherein the padding technology is specifically characterized in that a three-dipping three-pressing mode is adopted, the pressure of an upper press roller and a lower press roller is 0.2MPa, and the rotating speed of the press rollers is 1 rad/s. After compounding, removing absolute ethyl alcohol in the material to prepare the light flexible protective material which can be used in severe cold areas. The performance test data of the protective material is shown in table 2.
TABLE 2
3. Testing the heat insulation property: the products of examples 1 to 3 and comparative example were respectively impregnated into ultra-high molecular weight polyethylene plain woven fabrics, placed on five identical boxes, respectively, and the boxes were irradiated with the same light source (275W infrared lamp simulating infrared light source in sunlight), and the temperature in the boxes was measured, with the results shown in table 3.
TABLE 3
It can be seen from table 3 that the temperature change of the comparative example is large, the temperature change of the example is small, and the heat insulation effect is better. And the comparative example has the largest temperature variation range and a large thermal conductivity with the gradual increase of time, so that the heat insulation performance is inferior to that of the example. In contrast, the embodiment has a small thermal conductivity and good heat insulation performance.
Claims (4)
1. A preparation method of low-temperature-resistant shear thickening fluid is characterized by comprising the following steps:
(1) adding 300-480 parts of positively charged micro-nano spherical silicon dioxide particles into 100-250 parts of a dispersion medium at the temperature of 25-55 ℃, adding 2 parts of polytetrafluoroethylene powder, stirring at the rotating speed of 800r/min by using a ribbon stirrer, and dispersing for 30-80 minutes to obtain a uniform dispersion liquid;
(2) then placing the dispersion liquid obtained in the step (1) in a vacuum oven, and standing for 5-15 hours at the temperature of 25-55 ℃ to obtain a shear thickening liquid with obvious low temperature resistance effect; the raw materials are counted by mass;
the preparation method of the micro/nano sphere-shaped silicon dioxide particles with positive charges comprises the following steps: taking SiO2Adding anhydrous toluene and 3-aminopropyltrimethoxysilane into the particles in a 1000mL four-mouth bottle, ultrasonically mixing for 30min, condensing and refluxing at 110 ℃, and magnetically stirring for 24 h; after the reaction is finished, repeatedly washing the reaction product by using deionized water, ethanol and acetone in sequence; then drying in vacuum at 50 ℃ to obtain the micro-nano sphere silicon dioxide particles with positive charges;
the dispersion medium is a mixture of polyether polyol and silicone oil, wherein the dispersion medium contains 0.01% of anionic surfactant AS, and the molecular weight of the polyether polyol is 2000-8000; wherein the mass ratio of the polyether polyol to the silicone oil is 4-1: 1.
2. The method for preparing the nano particles of the micro-sphere of the positive charge according to claim 1, wherein the particle size of the nano particles of the micro-sphere of the positive charge is 10nm to 10 μm.
3. Use of the low temperature resistant shear thickening fluid according to claim 1, wherein the low temperature resistant shear thickening fluid is used for preparing a flexible lightweight protective material, and the protective material can be applied in an environment with a temperature of-35 ℃ to-30 ℃.
4. Use of a low temperature resistant shear thickening fluid according to claim 3, wherein the low temperature resistant shear thickening fluid is used for compounding a fibrous fabric by hand lay-up forming, vacuum padding, spraying or plastic sealing techniques.
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