CN112877810A - Preparation method of porous boron nitride fiber with high specific surface area - Google Patents
Preparation method of porous boron nitride fiber with high specific surface area Download PDFInfo
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- CN112877810A CN112877810A CN202110136581.1A CN202110136581A CN112877810A CN 112877810 A CN112877810 A CN 112877810A CN 202110136581 A CN202110136581 A CN 202110136581A CN 112877810 A CN112877810 A CN 112877810A
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 93
- 239000000835 fiber Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims description 15
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 14
- 239000004327 boric acid Substances 0.000 claims description 14
- 229920000877 Melamine resin Polymers 0.000 claims description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000004020 conductor Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims 2
- 238000000967 suction filtration Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 4
- PWTIWIZYPHOOGL-UHFFFAOYSA-N B(O)OBO.N1=C(N)N=C(N)N=C1N Chemical compound B(O)OBO.N1=C(N)N=C(N)N=C1N PWTIWIZYPHOOGL-UHFFFAOYSA-N 0.000 abstract description 3
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- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
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- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000002134 carbon nanofiber Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
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- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
Abstract
The invention belongs to the field of preparation of boron nitride fibers, and relates to a preparation method of porous boron nitride fibers with high specific surface area. And (3) carrying out water bath, suction filtration and drying to obtain a melamine diboronic acid precursor, and calcining at high temperature to obtain the boron nitride fiber. PEG is used as an organic solvent and doped in the precursor fiber, so that the surface activity of the precursor fiber is improved, and the PEG is decomposed during high-temperature calcination to generate gas, so that the pore content and the specific surface area of the boron nitride fiber are improved. The porous boron nitride fiber obtained by the invention has higher purity and lower crystallinity. The fiber surface has many defects that provide a large number of surface adsorption sites. The diameter of the prepared boron nitride fiber is 1-2 μm, and the length is 4-10 μm. Has uniform fiber structure and high specific surface area reaching 874m2(ii) in terms of/g. Solves the problems of high cost, toxic raw materials, long production period and the like of the current porous boron nitride fiber technology.
Description
Technical Field
The technical scheme of the invention relates to the field of preparation of boron nitride fibers, in particular to preparation of porous boron nitride fibers with high specific surface area.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The constituent elements of boron nitride are boron (B) atoms and nitrogen (N) atoms, with four different crystal structures, most commonly Hexagonal Boron Nitride (HBN). Others also exist, Rhombohedral Boron Nitride (RBN), Cubic Boron Nitride (CBN), and Wurtzite Boron Nitride (WBN). And it has a structure similar to graphite and is therefore also called "white graphite". Boron nitride has very excellent properties: high hardness, high thermal conductivity, low dielectric constant, high-temp resistance and chemical corrosion resistance. And thus are widely used in various fields such as: heat conducting materials, electronic products, the aviation field and the like.
The porous boron nitride is a novel porous material, has rich pore channel structures and has a high specific surface area. At present, the preparation method of the porous boron nitride fiber mainly comprises the following steps: template element substitution, hard template replication, self-assembly, and the like. However, these methods have many disadvantages, such as the need of toxic organic solvent, the need of liquid nitrogen in the preparation process, high cost and certain danger, and the long production cycle of the freeze-drying technology, which is not suitable for large-scale production.
Disclosure of Invention
Aiming at the problems of high cost, toxic raw materials, long production period and the like of the current porous boron nitride fiber technology, the preparation method of the porous boron nitride fiber is safe and efficient and can be produced in a large scale. The invention adopts PEG to modify the boron nitride precursor, and has the advantages of simple synthesis method, cheap and easily obtained raw materials, no toxicity and no harm.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a method for preparing a porous boron nitride fiber having a high specific surface area, comprising:
reacting boric acid, melamine and polyethylene glycol (PEG) 600 serving as raw materials in a water bath to form white floccule, and drying after suction filtration to obtain a boron nitride precursor;
and calcining the boron nitride precursor to obtain the porous boron nitride fiber with high specific surface area.
The invention provides a safe, convenient and efficient preparation method of porous boron nitride fibers.
In a second aspect of the present invention, there is provided a porous boron nitride fibre having a high specific surface area prepared by any one of the above methods. The diameter of the boron nitride fiber prepared by the invention is 1-2 μm, and the length is 4-10 μm. Has uniform fiber structure and high specific surface area reaching 874m2(ii)/g; has higher purity and lower crystallinity. The fiber surface has many defects that provide a large number of surface adsorption sites.
In a third aspect of the invention, the application of the porous boron nitride fiber with high specific surface area in the preparation of heat conduction materials, electronic products and aerospace devices is provided.
The porous boron nitride fiber prepared by the invention has a uniform fiber structure and a higher specific surface area, and the preparation method is simple, so the porous boron nitride fiber is expected to be widely applied to preparation of heat conduction materials, electronic products and aerospace devices.
The invention has the beneficial effects that:
(1) the porous boron nitride fiber obtained by the method has higher purity and lower crystallinity. The fiber surface has many defects that provide a large number of surface adsorption sites.
(2) The diameter of the boron nitride fiber prepared by the invention is 1-2 μm, and the length is 4-10 μm. Has uniform fiber structure and high specific surface area reaching 874m2/g。
(3) The method adopts boric acid, melamine and PEG600 as raw materials. And (3) carrying out water bath, suction filtration and drying to obtain a melamine diboronic acid precursor, and calcining at high temperature to obtain the boron nitride fiber. PEG is used as a surfactant to be doped in the precursor fiber, so that the surface activity of the precursor fiber is improved, and the PEG is decomposed during high-temperature calcination to generate gas, so that the pore content and the specific surface area of the boron nitride fiber are improved.
(4) The surfactant used in the present invention is non-toxic, harmless and more biocompatible than other surfactants. The prepared boron nitride fiber is more uniform and has smoother surface.
(5) The preparation method is simple, convenient to operate, high in practicability and easy to popularize.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is an SEM photograph of boron nitride fibers produced in example 1 of the present invention.
FIG. 2 is an SEM image of a boron nitride fiber produced in comparative example 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
Interpretation of terms
In the present invention, "PEG" means: polyethylene glycol.
In the present invention, "PVP" means: polyvinylpyrrolidone
In view of the problems of complicated preparation process, long production period, unsafe raw materials and the like of the existing porous boron nitride fiber, the invention provides a preparation method of the porous boron nitride fiber with high specific surface area.
The invention provides a preparation method of porous boron nitride fiber with high specific surface area, which comprises the steps of heating boric acid, melamine and PEG in water bath, naturally cooling, filtering and drying to obtain a precursor. And calcining the precursor in a nitrogen atmosphere, and heating in air to remove carbon.
Experiments show that the boron nitride fiber with high specific surface area can be obtained by adding PEG and drying to prepare the boron nitride precursor. Meanwhile, the specific surface area of the boron nitride fiber can be improved by changing the content of PEG.
In one or more embodiments of this embodiment, the ratio of boric acid to melamine is 3:1 to produce the boron nitride precursor.
Research and development find that: if the temperature of the water bath is lower than 90 ℃, reactants cannot be fully dissolved, and the generation of precursor products is also influenced. Thus, in one or more embodiments of this embodiment, the water bath temperature is 90 ℃ to allow for sufficient dissolution of the melamine and boric acid before the reaction to produce melamine diboronic acid.
In one or more embodiments of this embodiment, the filtration membrane used for suction filtration is a teflon membrane to effectively achieve solid-liquid separation.
In one or more embodiments of this embodiment, the drying temperature is 90 ℃ to 95 ℃ to remove the residual solvent on the surface of the boron nitride precursor.
In one or more embodiments of this embodiment, the calcination temperature is 900 ℃; in the series of examples, the temperature rise speed is 5 ℃/min, and the nitrogen flow is 50-100ml/min, so that the boron nitride precursor is converted into the boron nitride fiber with high specific surface area.
In one or more embodiments of this embodiment, the temperature of the incubation in air is 500-. The holding time is 30 min. And (3) removing carbon in the boron nitride fibers by heat treatment in the air to obtain the boron nitride fibers with higher purity.
In one or more embodiments of this embodiment, the feedstock is heated in a water bath with agitation to allow the feedstock to react sufficiently until a clear solution is obtained.
In comparative example 1 of the present invention, a method of preparing PVP-modified boron nitride fiber is provided. The boron nitride fiber obtained in comparative example 1 had a non-uniform morphology compared to example 1.
A preparation method of porous boron nitride fiber. The method mainly comprises four steps. Mainly comprises the steps of preparing a precursor in water bath, drying after suction filtration, calcining in a nitrogen atmosphere, and removing carbon by air heat treatment.
(1) Adding boric acid, melamine and PEG600 into a container containing deionized water, then placing the container into a water bath kettle, wherein the water bath temperature is 90 ℃, and stirring the mixture until the solution is clear. Naturally cooling to obtain white floccule, and performing suction filtration to obtain white solid.
(2) Wherein the concentration of melamine is 0.125mol/ml, the concentration of boric acid is 0.375mol/ml, and the molar ratio of boric acid to melamine is 3: 1. The content of PEG600 is 0.5%, 1%, 2%.
(3) Placing the white solid obtained in the step 1 in an oven at the temperature of between 85 and 90 ℃, and preserving heat for 3 to 4 hours. Obtaining white solid, namely the boron nitride precursor.
(4) And preserving the heat of the boron nitride precursor obtained in the third step for 2 hours at 900 ℃ in nitrogen to obtain the porous boron nitride fiber with high specific surface area.
(5) The nitrogen flow in step 4 is 50-100 ml/min.
(6) And heating the prepared boron nitride fiber from room temperature to 500 ℃ in the air, and keeping the temperature for 30min to remove carbon in the boron nitride fiber.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1
A method for preparing porous boron nitride fiber with high specific surface area, which comprises the following steps:
(1) place the weighing paper and clean beaker on an electronic balance, pick 4.635g of boric acid, 3.15g of melamine, and 2g of PEG600 with a clean spatula, and place them in the beaker. The measuring cylinder was used to remove 200ml of deionized water and poured into the same beaker.
(2) Placing the mixed solution in a water bath kettle, and heating in a water bath. The temperature of the water bath was 90 ℃ until the mixed solution became a clear solution. Stopping heating, gradually cooling the mixed solution to room temperature, gradually separating out white floccule precipitate from the solution, carrying out suction filtration on the obtained solution, placing the obtained solid in an oven for drying, wherein the drying temperature is 90 ℃, and the heat preservation time is 3 hours, thus obtaining the boron nitride precursor.
(3) And placing the obtained precursor in a tubular furnace to calcine in nitrogen atmosphere, wherein the calcining temperature is 900 ℃, and keeping the temperature at 900 ℃ for 2 hours. Obtaining the boron nitride fiber.
(4) Gradually heating the obtained boron nitride fiber to 500 ℃ in the air atmosphere, preserving the heat for 30min, removing carbon in the boron nitride fiber, and cooling to room temperature to obtain the porous boron nitride fiber with high specific surface area.
As a result: the carbon nanofiber material prepared in example 1 was subjected to specific surface area measurement, and when the PEG content was 1%, the specific surface area of the prepared boron nitride fiber was 714.0075m2/g。
Example 2
A method for preparing porous boron nitride fiber with high specific surface area, which comprises the following steps:
(1) the weighing paper and clean beaker were placed on an electronic balance, and 4.635g of boric acid, 3.15g of melamine, and 4g of PEG600 were removed with a clean spatula and placed in the beaker. The measuring cylinder was used to remove 200ml of deionized water and poured into the same beaker.
(2) Placing the mixed solution in a water bath kettle, and heating in a water bath. The temperature of the water bath was 90 ℃ until the mixed solution became a clear solution. Stopping heating, gradually cooling the mixed solution to room temperature, gradually separating out white floccule precipitate from the solution, carrying out suction filtration on the obtained solution, placing the obtained solid in an oven for drying, wherein the drying temperature is 90 ℃, and the heat preservation time is 3 hours, thus obtaining the boron nitride precursor.
(3) And placing the obtained precursor in a tubular furnace to calcine in nitrogen atmosphere, wherein the calcining temperature is 900 ℃, and keeping the temperature at 900 ℃ for 4 hours. Obtaining the boron nitride fiber.
(4) Gradually heating the obtained boron nitride fiber to 500 ℃ in the air atmosphere, preserving the heat for 30min, removing carbon in the boron nitride fiber, and cooling to room temperature to obtain the porous boron nitride fiber with high specific surface area.
As a result: the carbon nanofiber material prepared in example 2 was subjected to specific surface area detection, and when the PEG content was 2%, the specific surface area of the prepared boron nitride fiber was 874.5861m2The increase in PEG content increases the specific surface area compared to example 1.
Comparative example 1
(1) The weighing paper and clean beaker were placed on an electronic balance, and 4.635g of boric acid, 3.15g of melamine, and 2g of PVP K-30 were removed with a clean spatula and placed in the beaker. The measuring cylinder was used to remove 200ml of deionized water and poured into the same beaker.
(2) Placing the mixed solution in a water bath kettle, and heating in a water bath. The temperature of the water bath was 90 ℃ until the mixed solution became a clear solution. Stopping heating, gradually cooling the mixed solution to room temperature, gradually separating out white floccule precipitate from the solution, carrying out suction filtration on the obtained solution, placing the obtained solid in an oven for drying, wherein the drying temperature is 90 ℃, and the heat preservation time is 3 hours, thus obtaining the boron nitride precursor.
(3) And placing the obtained precursor in a tubular furnace to calcine in nitrogen atmosphere, wherein the calcining temperature is 900 ℃, and keeping the temperature at 900 ℃ for 2 hours. Obtaining the boron nitride fiber.
(4) Gradually heating the obtained boron nitride fiber to 500 ℃ in the air atmosphere, preserving the heat for 30min, removing carbon in the boron nitride fiber, and cooling to room temperature to obtain the porous boron nitride fiber with high specific surface area.
As a result: the boron nitride fiber obtained in comparative example 1 was subjected to SEM test, and the obtained boron nitride fiber had irregular edges and uneven morphology.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of porous boron nitride fibers with high specific surface area is characterized by comprising the following steps:
reacting boric acid, melamine and polyethylene glycol (PEG) 600 serving as raw materials in a water bath to form a white solid, and drying to obtain a boron nitride precursor;
and calcining the boron nitride precursor to obtain the porous boron nitride fiber with high specific surface area.
2. The method for preparing the porous boron nitride fiber with the high specific surface area according to claim 1, wherein the molar ratio of the boric acid to the melamine is 3-5: 1-3.
3. The method for preparing the porous boron nitride fiber with the high specific surface area according to claim 1, wherein the mass ratio of the boric acid to the polyethylene glycol PEG is 4-6: 1-6.
4. The method for preparing the porous boron nitride fiber with the high specific surface area according to claim 1, wherein the temperature of the water bath is 90-100 ℃.
5. The method for preparing a porous boron nitride fiber with high specific surface area according to claim 1, wherein the drying conditions are as follows: keeping the temperature for 3-4h at 85-90 ℃.
6. The method for preparing porous boron nitride fiber with high specific surface area according to claim 1, wherein the calcination is carried out under the following specific conditions: and (3) preserving the heat for 2-3 hours at 900-1000 ℃ under the protection of inert gas.
7. The method for preparing a porous boron nitride fiber with high specific surface area according to claim 6, wherein the inert gas is nitrogen and the flow rate is 50-100 ml/min.
8. The method for preparing the porous boron nitride fiber with the high specific surface area according to claim 6, wherein the porous boron nitride fiber with the high specific surface area is heated from room temperature to 500-600 ℃ and is kept for 1-2 h.
9. Porous boron nitride fibres with a high specific surface area produced by the method of any one of claims 1 to 8.
10. Use of the porous boron nitride fiber with high specific surface area according to claim 9 for the preparation of heat conducting materials, electronic products, aerospace devices.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114855453A (en) * | 2022-06-17 | 2022-08-05 | 西安理工大学 | Preparation method of high-thermal-conductivity composite material with self-assembled fiber-like monolithic structure |
| CN114940752A (en) * | 2022-03-02 | 2022-08-26 | 中国科学院过程工程研究所 | Catalyst for ring-opening polymerization of epoxy and preparation method and application thereof |
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