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A kind of method of supercritical ethanol modification nano-oxide

A nano-oxide and supercritical technology, which is applied in the treatment of dyed low-molecular organic compounds, bulk chemical production, and fibrous fillers. The effect of reducing agglomeration and simple operation

Active Publication Date: 2020-08-11
盘锦易立凯泰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the most common method is the method of coating the surface of nano-oxides with silane coupling agent. The dispersion of nano-oxides treated by this method is improved to a certain extent, but the dispersion in the matrix resin is not very ideal, which is Due to the large groups grafted on the surface, and the process is more complicated

Method used

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  • A kind of method of supercritical ethanol modification nano-oxide
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  • A kind of method of supercritical ethanol modification nano-oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A method for modifying nano oxides with supercritical ethanol. A method for surface modification of nano-oxide by supercritical ethanol. In the first step, 100 parts of ethanol and 10 parts of nano-alumina are uniformly mixed and placed in a reactor, strictly sealed; in the second step, the temperature of the supercritical equipment reaches 240°C Place the sealed reactor in the supercritical equipment for heating; in the third step, start timing when the pressure reaches 6 MPa, and in the fourth step, after maintaining the pressure for 5 minutes, quickly put the reactor in the cooling pool to cool the cooling water as ice The temperature of the water bath is 0°C and the cooling time is 40 min. In the fifth step, the treated nanoparticles are taken out and dried in a vacuum oven. After being completely dried, the treated nanoparticles will be obtained after grinding.

[0027] Supercritical equipment, see figure 1 ; Observe the obtained modified nano-alumina under a transmis...

Embodiment 2

[0032] A method for modifying nano oxides with supercritical ethanol. In the first step, 150 parts of ethanol and 15 parts of nano-alumina are uniformly mixed and placed in a reactor with a pressure gauge, and strictly sealed; in the second step, the sealed reactor in the previous step is placed in a heating with a temperature control device Heating in the furnace, the preset temperature is 240.5 ℃; the third step, observe the value of the pressure gauge on the reactor, when the value of the pressure gauge reaches 6.1 MPa, start timing, the time is 10 minutes; the fourth step, the reactor will be set after the specified time is reached Quickly put it into the cooling pool to cool, the cooling water is an ice-water bath, the temperature is 0℃, and the cooling time is 60 min; the fifth step, take out the treated nanoparticles and place them in a vacuum oven to dry, and then grind them in a mortar after they are completely dried After the treatment, the surface-treated nano alumin...

Embodiment 3

[0037] A method for modifying nano-silica with supercritical ethanol. In the first step, 120 parts of ethanol and 10 parts of nano-silica are uniformly mixed and placed in a reactor with a pressure gauge and strictly sealed; in the second step, the upper The sealed reaction kettle is placed in a heating furnace with a temperature control device for heating, and the preset temperature is 240 ℃; the third step, observe the pressure gauge value on the reaction kettle, and start timing when the pressure gauge value reaches 6 MPa. The fourth step is to quickly put the reaction kettle in the cooling pool to cool after the specified time is reached, the cooling water is an ice water bath, the temperature is 0℃, and the cooling time is 40 minutes; the fifth step is to take out the treated nanoparticles Place it in a vacuum oven to dry, and after it is completely dried, it is ground in a mortar to obtain surface-treated nano alumina.

[0038] The obtained modified nano silica and unmodifi...

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Abstract

The present invention belongs to the technical field of material modification, and particularly relates to a modification method for surface treatment of nanoparticles in a supercritical ethanol state. The modification method specifically comprises: 1, uniformly mixing ethanol and a nanometer oxide (particle size of 20-100 nm), placing in a reaction kettle with a pressure gauge, and strictly sealing; 2, placed the sealed reaction kettle in a heating furnace with a temperature control device, and heating at a temperature of 240+ / -1 DEG C; 3, observing the value of the pressure gauge on the reaction kettle, starting timing when the value of the pressure gauge achieves 6+ / -0.5 MPa, and carrying out a thermal insulation and pressure maintaining reaction for 5-10 min; 4, immediately placing thereaction kettle into a cooling pool, and cooling for 30-60 min, wherein cooling water is an ice water bath, and the temperature is 0 DEG C; and 5, taking out the treated nanoparticles, placing in a 130 DEG C vacuum oven, drying for more than 6 h, and grinding in a mortar after completely drying to obtain the surface-treated nanoparticles.

Description

Technical field [0001] The invention belongs to the technical field of material modification, and particularly relates to a modification method for surface treatment of nanoparticles in the state of supercritical ethanol, which utilizes the special properties of supercritical ethanol to improve the surface treatment effect on nanoparticles. Background technique [0002] Nano oxides refer to oxides whose particle size reaches the nanometer level and are ultrafine particles with a size of 1-100 nm. It mainly includes nano alumina, nano silica, and nano titanium dioxide. Because the ratio of the number of surface atoms to the total number of atoms in the bulk phase increases sharply with the decrease of the particle size, nano-oxides show strong volume effects (small size effects), quantum size effects, surface effects and macroscopic quantum tunnels. Effect, and then show a series of excellent performance in many aspects such as light, electricity, thermodynamics and chemical reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/28C09C1/36C09C1/40C09C3/08
CPCY02P20/54
Inventor 代起望李昭迪
Owner 盘锦易立凯泰新材料有限公司
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