CN114890393B - Low-temperature preparation method of BN microsphere - Google Patents
Low-temperature preparation method of BN microsphere Download PDFInfo
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- CN114890393B CN114890393B CN202210296958.4A CN202210296958A CN114890393B CN 114890393 B CN114890393 B CN 114890393B CN 202210296958 A CN202210296958 A CN 202210296958A CN 114890393 B CN114890393 B CN 114890393B
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- 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
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a low-temperature preparation method of BN microspheres, which comprises the steps of preparing a homogeneous solution with mass concentration of 0.1-0.5 g/ml in a solvent by taking trichloroborazine as a raw material; and (3) carrying out solvothermal treatment on the homogeneous solution for 1-12 h at the temperature of 120-220 ℃, naturally placing or quenching to room temperature, and centrifuging to obtain BN microspheres. The preparation method provided by the invention has the advantages of simple process, no need of adding any additive, low cost, high yield of over 99.6 percent, high purity of the prepared BN microsphere, uniform morphology and small dispersity.
Description
Technical Field
The invention relates to the technical field of organic synthesis, in particular to a low-temperature preparation method of BN microspheres.
Background
The Boron Nitride (BN) ceramic has high thermal conductivity and high stability, can be used in an oxidizing atmosphere below 900 ℃ and an inert atmosphere above 2800 ℃, and can be used as a lining of a heating container, so that the sintering temperature can be greatly reduced, and the compactness and flexibility of the container are obviously improved. BN also has unique physical and chemical properties such as electrical insulation, low dielectric property, self-lubricating property, shielding property, high chemical stability and the like, and the BN and the composite material thereof are excellent high-temperature wave-transparent, corrosion-resistant, radiation-resistant and high-frequency high-voltage insulating heat-dissipating materials.
At present, the preparation methods of BN powder mainly comprise a borax synthesis method, a urea method and a halide synthesis method, the BN powder obtained by the synthesis methods is uncontrollable in shape, the synthesis temperature is above 1000 ℃, the synthesis cost is high, the purity is low, and the process is complex.
Disclosure of Invention
The invention provides a low-temperature preparation method of BN microspheres, which is used for overcoming the defects of high synthesis cost, complex process and the like in the prior art.
In order to achieve the above purpose, the invention provides a low-temperature preparation method of BN microsphere, comprising the following steps:
s1: under the anhydrous and anaerobic condition, trichloroborazine (TCB) is dissolved in an organic solvent to prepare a homogeneous solution with the concentration of 0.1-0.5 g/ml;
s2: under the anhydrous and anaerobic condition, placing the homogeneous solution into a reaction kettle, sealing, and then performing solvothermal reaction, wherein the solvothermal reaction is carried out at the temperature of 120-220 ℃ for 1-12 h;
s3: and naturally or quenching to room temperature after the reaction is finished to obtain BN microspheres.
In order to achieve the above purpose, the invention also provides a BN microsphere prepared by the low-temperature preparation method; the BN microsphere is solid microsphere with purity greater than 99%, and microsphere diameter distribution is 1-5 μm.
In order to achieve the above purpose, the invention also provides an application of the BN microsphere, wherein the BN microsphere prepared by the low-temperature preparation method or the BN microsphere is applied to fire-resistant, lubricating, heat shielding and reactor structural materials.
Compared with the prior art, the invention has the beneficial effects that:
the low-temperature preparation method of BN microsphere provided by the invention uses trichloroborazine as raw material, prepares the trichloroborazine into 0.1-0.5 g/ml homogeneous solution, and then places the homogeneous solution in a reaction kettle for solvothermal reaction, wherein the reaction kettle has certain pressure due to heating in the solvothermal reaction process, and the forward direction of solvothermal reaction can be promoted under the action of pressure, thus obviously reducing the temperature required by the reaction and further lowering the cost. The preparation method provided by the invention has the advantages of simple process, no need of adding any additive, low cost and high purity (> 99.6%) of the BN microsphere, uniform morphology and small dispersity, and the yield is over 99%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM photograph of solid BN microspheres prepared in example 4;
FIG. 2 is an infrared spectrum of the BN solid microsphere prepared in example 4.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical solutions of the embodiments of the present invention may be combined with each other, but it is necessary to be based on the fact that those skilled in the art can implement the technical solutions, and when the technical solutions are contradictory or cannot be implemented, the combination of the technical solutions should be considered as not existing, and not falling within the scope of protection claimed by the present invention.
The drugs/reagents used are all commercially available without specific description.
The invention provides a low-temperature preparation method of BN microspheres, which comprises the following steps:
s1: under the anhydrous and anaerobic condition, dissolving trichloroborazine in an organic solvent to prepare a homogeneous solution with the concentration of 0.1-0.5 g/ml;
s2: under the anhydrous and anaerobic condition, placing the homogeneous solution into a reaction kettle, sealing, and then performing solvothermal reaction, wherein the solvothermal reaction is carried out at the temperature of 120-220 ℃ for 1-12 h;
s3: and naturally or quenching to room temperature after the reaction is finished to obtain BN microspheres.
Preferably, the solvothermal reaction is at 200 ℃ for 6 hours.
Preferably, the organic solvent is at least one of toluene, xylene, dichlorobenzene, and n-pentane.
Preferably, the volume ratio of the homogeneous solution in the solvothermal reaction kettle is not more than 3/4.
Preferably, the concentration of the homogeneous solution is 0.1g/ml; the solvothermal reaction is carried out at 220 ℃ for 1h.
Preferably, the concentration of the homogeneous solution is 0.3g/ml; the solvothermal reaction is carried out at 200 ℃ for 6 hours.
Preferably, the concentration of the homogeneous solution is 0.5g/ml; the solvothermal reaction is carried out at 220 ℃ for 1h.
Preferably, the concentration of the homogeneous solution is 0.5g/ml; the solvothermal reaction is carried out at 200 ℃ for 6 hours.
The invention also provides BN microsphere which is prepared by the low-temperature preparation method; the BN microsphere is solid microsphere with purity greater than 99%, and microsphere diameter distribution is 1-5 μm.
The invention also provides an application of the BN microsphere, and the BN microsphere prepared by the low-temperature preparation method or the BN microsphere is applied to the fields of fire resistance, lubrication, heat shielding, reactor structural materials and the like.
Example 1
The embodiment provides a low-temperature preparation method of BN microspheres, which comprises the following steps:
s1: dissolving trichloroborazine in an organic solvent under anhydrous and anaerobic conditions to prepare a homogeneous solution of 0.1g/ml;
s2: placing the homogeneous solution into a 200mL reaction kettle under the anhydrous and anaerobic condition, sealing, and performing solvothermal reaction at 220 ℃ for 1h;
s3: and naturally or quenching to room temperature after the reaction is finished to obtain the BN solid microsphere.
Example 2
This example provides a low temperature process for preparing BN microspheres with a homogeneous solution concentration of 0.5g/ml compared to example 1, the other process being the same as in example 1.
Example 3
This example provides a low temperature process for preparing BN microspheres with a homogeneous solution concentration of 0.3g/ml compared to example 1, the other process being the same as in example 1.
Example 4
The embodiment provides a low-temperature preparation method of BN microspheres, which comprises the following steps:
s1: dissolving trichloroborazine in an organic solvent under anhydrous and anaerobic conditions to prepare a homogeneous solution of 0.3g/ml;
s2: placing the homogeneous solution into a 200mL reaction kettle under anhydrous and anaerobic conditions, sealing, and performing solvothermal reaction at 200 ℃ for 6 hours;
s3: and naturally or quenching to room temperature after the reaction is finished to obtain the BN solid microsphere.
As shown in FIG. 1, the SEM photograph of the BN solid microsphere prepared in this example shows that the diameter of the prepared BN microsphere is within the range of 2.+ -. 0.5. Mu.m.
The infrared spectrum of the BN solid microsphere prepared in the embodiment is shown in figure 2, and the prepared BN infrared spectrum is basically consistent with the infrared spectrum of commercial BN.
Example 5
This example provides a low temperature process for preparing BN microspheres with a homogeneous solution concentration of 0.5g/ml compared to example 4, the other process being the same as in example 4.
Example 6
This example provides a low temperature process for preparing BN microspheres at a homogeneous solution concentration of 0.1g/ml as compared to example 4, the other process being the same as in example 4.
Example 7
This example provides a low temperature preparation method of BN microsphere, and compared with example 4, the solvothermal reaction temperature is 120 ℃ and the solvothermal reaction time is 12 hours, and the other processes are the same as in example 4.
Example 8
This example provides a low temperature preparation method of BN microsphere, which is compared with example 4, the solvothermal reaction temperature is 150 ℃ and time is 10 hours, and other processes are the same as in example 4.
Example 9
This example provides a low temperature preparation method of BN microsphere, which is compared with example 4, the solvothermal reaction temperature is 180 ℃ and the solvothermal reaction time is 10 hours, and the other processes are the same as in example 4.
It is evident from examples 1 to 9 that the concentration of the homogeneous solution will affect the yield of the final BN microspheres, with the final yield increasing as the concentration of the homogeneous solution increases. The temperature and time of solvothermal reaction directly influence the nucleation rate and growth rate of BN microsphere so as to control the diameter and quality of the microsphere.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the description of the present invention and the accompanying drawings or direct/indirect application in other related technical fields are included in the scope of the invention.
Claims (7)
1. The low-temperature preparation method of the BN microsphere is characterized by comprising the following steps of:
s1: under the anhydrous and anaerobic condition, dissolving trichloroborazine in an organic solvent to prepare a homogeneous solution with the concentration of 0.1-0.5 g/mL; the organic solvent is at least one of toluene, xylene, dichlorobenzene and n-pentane;
s2: under the anhydrous and anaerobic condition, placing the homogeneous solution into a reaction kettle, sealing, and then performing solvothermal reaction, wherein the solvothermal reaction is carried out at the temperature of 120-220 ℃ for 1-12 hours;
s3: naturally or quenching to room temperature after the reaction is finished to obtain BN microspheres; the BN microsphere is solid, the purity is greater than 99%, and the diameter of the microsphere is distributed at 1-5 mu m.
2. The low temperature production method according to claim 1, wherein the solvothermal reaction is performed at 200 ℃ for 6 hours.
3. The low temperature production method according to claim 1, wherein the volume ratio of the homogeneous solution in the solvothermal reactor is not more than 3/4.
4. The low temperature production method according to claim 1, wherein the concentration of the homogeneous solution is 0.1g/mL; the solvothermal reaction is carried out at 220 ℃ for 1h.
5. The low temperature production method according to claim 1, wherein the concentration of the homogeneous solution is 0.3g/mL; the solvothermal reaction is carried out at 200 ℃ for 6 hours.
6. The low temperature production method according to claim 1, wherein the concentration of the homogeneous solution is 0.5g/mL; the solvothermal reaction is carried out at 220 ℃ for 1h.
7. The low temperature production method according to claim 1, wherein the concentration of the homogeneous solution is 0.5g/mL; the solvothermal reaction is carried out at 200 ℃ for 6 hours.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0162137A2 (en) * | 1984-05-21 | 1985-11-27 | Toshiba Tungaloy Co. Ltd. | Method for preparing boron nitride |
| EP0544570A1 (en) * | 1991-11-28 | 1993-06-02 | Elf Atochem S.A. | Process for the preparation of boron nitride and the obtaind boron nitride |
| CN103395752A (en) * | 2013-08-09 | 2013-11-20 | 哈尔滨工业大学（威海） | Preparation method for boron nitride micron solid ball |
| CN106348262A (en) * | 2016-11-24 | 2017-01-25 | 陕西聚洁瀚化工有限公司 | Preparation method of BN (boron nitride) |
-
2022
- 2022-03-24 CN CN202210296958.4A patent/CN114890393B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0162137A2 (en) * | 1984-05-21 | 1985-11-27 | Toshiba Tungaloy Co. Ltd. | Method for preparing boron nitride |
| EP0544570A1 (en) * | 1991-11-28 | 1993-06-02 | Elf Atochem S.A. | Process for the preparation of boron nitride and the obtaind boron nitride |
| CN103395752A (en) * | 2013-08-09 | 2013-11-20 | 哈尔滨工业大学（威海） | Preparation method for boron nitride micron solid ball |
| CN106348262A (en) * | 2016-11-24 | 2017-01-25 | 陕西聚洁瀚化工有限公司 | Preparation method of BN (boron nitride) |
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