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Method for modifying nanometer oxide through supercritical ethanol

A nano-oxide and supercritical technology, which is applied in the treatment of dyed low-molecular-weight organic compounds, the production of bulk chemicals, and fibrous fillers, etc., can solve the problems of complex process and unsatisfactory dispersion of matrix resin, and achieves simple acquisition of raw materials, The effect of reducing agglomeration and simple operation

Active Publication Date: 2018-01-19
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

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  • Method for modifying nanometer oxide through supercritical ethanol
  • Method for modifying nanometer oxide through supercritical ethanol
  • Method for modifying nanometer oxide through supercritical ethanol

Examples

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Embodiment 1

[0026] A method for modifying nanometer oxides with supercritical ethanol. A method for modifying the surface of nanometer oxides with supercritical ethanol. In the first step, 100 parts of ethanol and 10 parts of nano-alumina are uniformly mixed and placed in a reaction kettle, which is strictly sealed; in the second step, the temperature of the supercritical equipment reaches 240°C , place the sealed reactor in supercritical equipment for heating; in the third step, start timing when the pressure reaches 6 MPa; in the fourth step, put the reactor into the cooling pool to cool the cooling water to ice In a water bath, the temperature is 0°C, and the cooling time is 40 min. Step 5: Take out the treated nanoparticles and place them in a vacuum oven for drying. After complete drying, grind them to obtain surface-treated nanoparticles.

[0027] The supercritical equipment consists of a reactor with a pressure gauge (1), a heating pool (2), and a cooling pool (3), see figure 1 ; ...

Embodiment 2

[0032] A method for modifying nanometer 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 reaction kettle with a pressure gauge, which is strictly sealed; in the second step, the sealed reaction kettle in the previous step is placed in a heating tank 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, and the time is 10 minutes; the fourth step, turn the reactor off after the specified time Quickly put it into a cooling pool for cooling, the cooling water is an ice water bath, the temperature is 0°C, and the cooling time is 60 min; the fifth step is to take out the treated nanoparticles and place them in a vacuum oven for drying, and grind them with a mortar after they are completely dry After the treatment, t...

Embodiment 3

[0038] 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 reaction kettle with a pressure gauge, and strictly sealed; in the second step, the upper The first sealed reaction kettle is placed in a heating furnace with a temperature control device for heating, and the preset temperature is 240 °C; the third step is to observe the pressure gauge value on the reaction kettle, and start timing when the pressure gauge value reaches 6 MPa. 5 min; the fourth step, after reaching the specified time, quickly put the reactor into the cooling pool for cooling, the cooling water is an ice water bath, the temperature is 0°C, and the cooling time is 40 min; the fifth step, take out the treated nanoparticles Put it in a vacuum oven and dry it. After it is completely dried, it will be ground in a mortar to get the surface-treated nano-alumina.

[0039] The obtained modified nano-...

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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 in particular relates to a modification method for surface treatment of nanoparticles in a 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 scale, ultrafine particles with a size of 1-100nm. Mainly include nano-alumina, nano-silicon dioxide, nano-titanium dioxide, etc. Nano-oxides show strong volume effect (small size effect), quantum size effect, surface effect and macroscopic quantum tunneling because the ratio of surface atoms to the total number of bulk atoms increases sharply with the decrease of particle size. Effect, and then show a series of excellent properties in many aspects such as light, electricity, thermodynamics and chemical reactions. Taking nano-alumina as an...

Claims

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Application Information

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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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