CN111944331A - Surface modification treatment method of anti-settling boron carbide powder - Google Patents
Surface modification treatment method of anti-settling boron carbide powder Download PDFInfo
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- CN111944331A CN111944331A CN202010772840.5A CN202010772840A CN111944331A CN 111944331 A CN111944331 A CN 111944331A CN 202010772840 A CN202010772840 A CN 202010772840A CN 111944331 A CN111944331 A CN 111944331A
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- boron carbide
- carbide powder
- aminoethyl
- settling
- surface modification
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention aims to disclose a surface modification treatment method of anti-settling boron carbide powder, which comprises the following steps: (1) obtaining boron carbide powder with uniform particle size by screening, then adding the boron carbide powder into a dilute acid solution, heating and stirring for 2-4h, performing ultrasonic dispersion for 30-60min, filtering, and drying in the shade at room temperature to form an acidic micromolecule coating layer; (2) adding n-butanol, distilled water and surface modifier into the dried boron carbide powder, reacting at 40-60 deg.C for 3-4h, repeatedly washing, drying in the shade, and vacuum drying to obtain double-coated boron carbide powder; compared with the prior art, the ultrasonic redispersion of the boron carbide powder and the surface absorption of the dilute acid solution can form an acidic micromolecule coating layer which has a synergistic effect with the surface modifier, and the method is beneficial to improving the modification effect of the boron carbide, simple, low in cost and convenient to popularize, and achieves the purpose of the invention.
Description
Technical Field
The invention relates to a surface modification treatment method of boron carbide powder, in particular to a surface modification treatment method of anti-settling boron carbide powder.
Background
Boron carbide as the most efficient neutron shielding absorber has been widely applied in the fields of nuclear power, military industry and irradiation-related equipment. In particular, the high dispersibility and the high stability in the preparation, storage and use processes of the coating taking a liquid material as a matrix, a pouring encapsulating material and a coating cladding material become the key points of the material quality.
When the inorganic particles are modified by the coupling agent, the inorganic particles can generate grafting reaction with the surface active groups of the coupling agent to form stable chemical bonding effect, and the number of partial polar functional groups is reduced. Meanwhile, a chemical affinity effect is established between the coupling agent and the matrix, so that the chemical bond combination of the filler and the matrix is formed, the compatibility of a two-phase interface is improved, and the performance of the composite material is improved. The organosilicon and the B are improved due to the coupling effect of the coupling agent4The interface compatibility of C reduces the interface defects and the possible gaps and improves the interface compatibilityThe wetting ability of the organic silicon resin to the boron carbide powder improves the dispersion state of the boron carbide powder in the organic silicon resin base material. Under acidic conditions, B4C and silane coupling agent are subjected to hydrolytic condensation, and the silane coupling agent is grafted to B4C, surface of the substrate. The silane coupling agent is a molecule containing four functional groups, and has a reactive group capable of being chemically combined with inorganic materials (such as glass, silica sand, metal and the like) and a reactive group capable of being chemically combined with organic materials (such as synthetic resin and the like) in the molecule, so that the modified B4C may be better compatible with organic materials.
Therefore, a method for surface modification treatment of anti-settling boron carbide powder is particularly needed to solve the existing problems.
Disclosure of Invention
The invention aims to provide a surface modification treatment method of anti-settling boron carbide powder, aiming at the defects of the prior art, and the method is simple in process and good in modification effect.
The technical problem solved by the invention can be realized by adopting the following technical scheme:
the surface modification treatment method of the anti-settling boron carbide powder is characterized by comprising the following steps of:
(1) obtaining boron carbide powder with uniform particle size by screening, then adding the boron carbide powder into a dilute acid solution, heating and stirring for 2-4h, performing ultrasonic dispersion for 30-60min, filtering, and drying in the shade at room temperature to form an acidic micromolecule coating layer;
(2) adding n-butyl alcohol, distilled water and a surface modifier into the dried boron carbide powder in the shade, reacting for 3-4h at the temperature of 40-60 ℃, repeatedly washing, drying in the shade and then drying in vacuum to obtain the boron carbide powder with double coating layers.
In one embodiment of the present invention, the boron carbide powder is nano-scale and micro-scale powder, and the form of the boron carbide powder includes various forms such as spherical, flake, rod and fiber.
In one embodiment of the present invention, the dilute acids include, but are not limited to, hydrochloric acid, sulfuric acid, nitric acid, benzoic acid, and small molecule organic acids.
In one embodiment of the invention, the surface modifier is aminomethyl trimethoxysilane, aminoethyl trimethoxysilane, aminopropyltrimethoxysilane, aminomethyl triethoxysilane, aminoethyl triethoxysilane, aminopropyltriethoxysilane (KH550), N-aminoethyl-aminopropyltrimethoxysilane, N-aminoethyl-aminopropyltriethoxysilane, N-aminoethyl-aminopropylmethyldimethoxysilane, N-aminoethyl-aminopropylmethyldiethoxysilane, aminomethyl methyldimethoxysilane, aminoethyl-methyldimethoxysilane, aminopropylmethyldimethoxysilane, aminomethyl methyldiethoxysilane, aminoethyl-methyldiethoxysilane, aminopropylmethyldiethoxysilane (JH-M902), glycidyloxypropyltrimethoxysilane (KH560), Methyl phenyl trimethoxy silane, and the like.
Compared with the prior art, the surface modification treatment method of the anti-settling boron carbide powder has the advantages that the ultrasonic redispersion of the boron carbide powder and the surface absorption of the dilute acid solution can form an acidic micromolecule coating layer, the surface modification agent and the micromolecule coating layer have a synergistic effect, the modification effect of the boron carbide is improved, the method is simple, the cost is low, the popularization is convenient, and the purpose of the invention is realized.
The features of the present invention will be apparent from the accompanying drawings and from the detailed description of the preferred embodiments which follows.
Drawings
FIG. 1 is a schematic diagram showing a modification mechanism of the method for surface modification treatment of boron carbide powder according to the present invention;
FIG. 2 is a schematic representation of the bonding of the surface modifying agents of the present invention;
FIG. 3 is an SEM illustration of boron carbide before and after modification according to the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below by combining the specific drawings.
As shown in fig. 1 to 3, the method for surface modification treatment of anti-settling boron carbide powder of the present invention comprises the following steps:
sieving boron carbide powder, placing in a three-neck flask, adding a dilute acid solution, reacting for 2-4h at room temperature, performing synchronous ultrasonic dispersion for 30-60min, filtering, and drying in the shade at room temperature to obtain powder A, wherein the mass fraction of the dilute acid is 0.5% -1%;
putting the powder A into a three-neck flask, adding n-butane, distilled water and a surface modifier, heating to 40-60 ℃, carrying out surface modification for 3-4h, washing, drying in the shade, and then putting into a vacuum drying oven below 60 ℃ to prepare the boron carbide powder with double coating layers.
The boron carbide powder is nano-scale and micron-scale powder, and the form of the boron carbide powder comprises various forms such as spherical, flaky, rod-shaped, fibrous and the like.
Such dilute acids include, but are not limited to, hydrochloric acid, sulfuric acid, nitric acid, benzoic acid, and small molecule organic acids.
The surface modifier is aminomethyl trimethoxy silane, aminoethyl trimethoxy silane, aminopropyl trimethoxy silane, aminomethyl triethoxy silane, aminoethyl triethoxy silane, aminopropyl triethoxy silane (KH550), N-aminoethyl-aminopropyl trimethoxy silane, N-aminoethyl-aminopropyl triethoxy silane, N-aminoethyl-aminopropyl methyl dimethoxy silane, n-aminoethyl-aminopropylmethyldiethoxysilane, aminomethylmethyldimethoxysilane, aminoethylmethyldimethoxysilane, aminopropylmethyldimethoxysilane, aminomethylmethyldiethoxysilane, aminoethylmethyldiethoxysilane (JH-M902), glycidoxypropyltrimethoxysilane (KH560), methylphenyltrimethoxysilane, or a mixture of two or more thereof.
Example 1
Sieving boron carbide powder, putting 100g of the boron carbide powder into a three-neck flask, adding 200mL of 1% hydrochloric acid solution, stirring and reacting at room temperature for 1h, synchronously performing ultrasonic dispersion for 30min, filtering, and drying in the shade at room temperature to obtain powder A;
adding 50g of powder A into a three-neck flask, adding 80ml of N-butane, 120ml of distilled water and 10g of N-aminoethyl-aminopropylmethyldiethoxysilane, heating to 48 ℃, carrying out surface modification for 3h, filtering, washing, drying in the shade, and then carrying out vacuum drying at 60 ℃ to prepare the boron carbide powder with the double coating layers.
Example 2:
sieving boron carbide powder, putting 100g of the boron carbide powder into a three-neck flask, adding 200mL of 0.5% tartaric acid solution, stirring and reacting at room temperature for 3.5h, synchronously performing ultrasonic dispersion for 30min, filtering, and drying in the shade at room temperature to obtain powder A;
adding 80ml of n-butane, 120ml of distilled water and KH55015g into 50g of powder A in a three-neck flask, heating to 60 ℃, carrying out surface modification for 4h, filtering, washing, drying in the shade, and then carrying out vacuum drying at 60 ℃ to prepare the boron carbide powder with double coating layers.
Example 3:
sieving boron carbide powder, putting 100g of the boron carbide powder into a three-neck flask, adding 200mL of 0.8% benzoic acid solution, stirring and reacting at room temperature for 2.5h, synchronously performing ultrasonic dispersion for 45min, filtering, and drying in the shade at room temperature to obtain powder A;
adding 50g of powder A into a three-neck flask, adding 80ml of n-butane, 120ml of distilled water and JH-M9028 g, heating to 55 ℃, carrying out surface modification for 3h, filtering, washing, drying in the shade, and then carrying out vacuum drying at 60 ℃ to prepare the boron carbide powder with the double coating layers.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined by the appended claims and their equivalents.
Claims (4)
1. The surface modification treatment method of the anti-settling boron carbide powder is characterized by comprising the following steps of:
(1) obtaining boron carbide powder with uniform particle size by screening, then adding the boron carbide powder into a dilute acid solution, heating and stirring for 2-4h, performing ultrasonic dispersion for 30-60min, filtering, and drying in the shade at room temperature to form an acidic micromolecule coating layer;
(2) adding n-butyl alcohol, distilled water and a surface modifier into the dried boron carbide powder in the shade, reacting for 3-4h at the temperature of 40-60 ℃, repeatedly washing, drying in the shade and then drying in vacuum to obtain the boron carbide powder with double coating layers.
2. The method for surface modification treatment of anti-settling boron carbide powder according to claim 1, wherein the boron carbide powder is nano-sized or micro-sized, and the form of the boron carbide powder includes various forms such as spherical, flake, rod, and fiber.
3. The method for surface modification treatment of anti-settling boron carbide powder according to claim 1, wherein the dilute acids include, but are not limited to, hydrochloric acid, sulfuric acid, nitric acid, benzoic acid, and small molecule organic acids.
4. The method for surface modification treatment of anti-settling boron carbide powder according to claim 1, wherein the surface modifier is aminomethyl trimethoxysilane, aminoethyl trimethoxysilane, aminopropyltrimethoxysilane, aminomethyl triethoxysilane, aminoethyl triethoxysilane, aminopropyltriethoxysilane (KH550), N-aminoethyl-aminopropyltrimethoxysilane, N-aminoethyl-aminopropyltriethoxysilane, N-aminoethyl-aminopropylmethyldimethoxysilane, N-aminoethyl-aminopropylmethyldiethoxysilane, aminomethyl methyldimethoxysilane, aminoethyl methyldimethoxysilane, aminopropylmethyldimethoxysilane, aminomethyl methyldiethoxysilane, aminoethyl methyldiethoxysilane, aminopropylmethyldiethoxysilane (JH-M902), or a mixture thereof, Glycidyl ether oxypropyl trimethoxysilane (KH560), methyl phenyl trimethoxysilane, etc.
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| CN202010772840.5A CN111944331A (en) | 2020-08-04 | 2020-08-04 | Surface modification treatment method of anti-settling boron carbide powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113881247A (en) * | 2021-10-18 | 2022-01-04 | 上海核工程研究设计院有限公司 | Surface grafting modification treatment method for anti-settling boron carbide powder |
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Application publication date: 20201117 |