CN106348262A - Preparation method of BN (boron nitride) - Google Patents
Preparation method of BN (boron nitride) Download PDFInfo
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- CN106348262A CN106348262A CN201611043020.2A CN201611043020A CN106348262A CN 106348262 A CN106348262 A CN 106348262A CN 201611043020 A CN201611043020 A CN 201611043020A CN 106348262 A CN106348262 A CN 106348262A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
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Abstract
The invention relates to the technical field of functional materials, in particular to a preparation method of BN (boron nitride). The preparation method of the BN comprises the steps that (1) an colorless acicular crystal, i.e., B-trichloroborazine is obtained; (2) the prepared B-trichloroborazine crystal and isopropylamine are used for performing ammonolysis reaction to obtain triamine-based borazine, wherein an earlier stage of the reaction is performed in a low-temperature bath ice water mixture, and a later stage of the reaction is performed at room temperature; (3) polyborazine containing xylene is prepared; the xylene is completely volatilized; white powdery solid is obtained; (4) a dried polyborazine precursor is ground into a powdery shape and is put into a silica boat; the silica boat is put into a tubular furnace; before heating, nitrogen gas is introduced into the tubular furnace; the tubular furnace is heated; heat insulation is performed; then, the tubular furnace is naturally cooled to room temperature, and thus the nitridized BN can be obtained. The prepared BN is of a flaky structure; the structure between sheets is compact; the BN crystal is mainly a trimetric system.
Description
Technical field
The present invention relates to technical field of function materials is and in particular to a kind of preparation method of boron nitride.
Background technology
Development situation of high-performance inorganic fibers has become one of key areas of modern material scientific research.Boron nitride (bn) fiber has concurrently
The multiple premium properties that bn material and fibrous material have.Bn fiber has that intensity is high, density is low, corrosion-resistant, wave
Strong the features such as, at aspects such as nuclear industry, electronics and composites, there is good application prospect.Pottery with bn fiber as reinforcing agent
Porcelain based composites show excellent wave transparent load-carrying properties in key positions such as aerospace antenna houses, thus bn fiber
Research becomes one of focus of new ceramics fiber art.Between each atom of bn, connecting key is covalent bond, has higher atom
Bond strength, therefore bn also have high temperature resistant, heat shock resistance good characteristic, and its intensity and hardness decline very at high temperature
Few.
The preparation method of bn is varied, and Shen Chunying of Nanjing University of Technology etc. is reacted with tripolycyanamide, using boric acid
Bn whisker is obtained eventually；Yuan Songdong of Hubei University Of Technology etc. also utilizes boric acid bn hexagonal to be obtained with tripolycyanamide, and to system
The specific surface area of bn hexagonal obtaining is analyzed with pore-size distribution；Roc etc. adopts organic precursor method to be obtained forever for Deng Cheng, thunder
Bn fiber, prepared fibre property is preferable, but experiment condition requires harshness.The application adopts organic precursor method in experiment bar
Part is obtained the organic precursor of bn, by nitrogen treatment, prepared bn rhomboidal crystal under conditions of comparing mitigation.
Content of the invention
It is contemplated that proposing a kind of preparation method of boron nitride.
Technical program of the present invention lies in:
The preparation method of boron nitride, comprises the steps:
(1) ammonium chloride powder is added in there-necked flask, be subsequently adding xylene solvent, be stirred vigorously so that ammonium chloride powder
Form suspension in organic solvent, be passed through nitrogen, the air in discharger and moisture；It is passed through three after being heated to 80 ~ 100 DEG C
Boron chloride gas, condensing reflux；Finally the xylene solution of the trichlorine obtaining borazine is passed through nitrogen, low-temperature heat, incites somebody to action
Dimethylbenzene in reaction system vapors away, and the colourless acicular crystal obtaining is trichlorine borazine；
(2) carry out ammonolysis reaction using prepared trichlorine borazine crystal and 2-aminopropane. and triamine alkylborazine, reaction are obtained
Leading portion is carried out in low temperature bath mixture of ice and water, and back segment is carried out at room temperature；
(3) xylene solution of triamine alkylborazine is put in there-necked flask, heat up under nitrogen protection and be heated to 100～
200 DEG C, carry out polyreaction, obtain freezing colloidal solid, the as polyborazine containing dimethylbenzene, dimethylbenzene is vapored away completely
For white powdery solids；
(4) the polyborazine precursor of drying is ground into powder, puts in people's quartz boat, quartz boat is put in tube furnace,
Before heating, tube furnace is passed through nitrogen, to diamond heating, is incubated, then allows tube furnace naturally cool to room temperature, you can to obtain
Bn through nitridation.
The temperature of described condensing reflux is 0～5 DEG C, and the response time is 10～20 h.
Described be heated to 80 ~ 100 DEG C after be passed through boron trichloride gas again.
Described reaction leading portion 5 ~ 5.5 h is carried out in low temperature bath mixture of ice and water, and back segment 13 ~ 15 h enters at room temperature
OK.
The time of described polyreaction is 10 ~ 20 h.
The temperature of described diamond heating is 1000 ~ 1200 DEG C, and temperature retention time is l ~ 1.5h.
The method have technical effect that:
The present invention synthesizes the organic precursor polymer of bn by relatively mild method, with boron trichloride gas and ammonium chloride diformazan
Benzene mixed serum reacts under the protection of nitrogen, forms water white bn crystal.Bn is laminated structure, structure between piece and piece
Closely, bn crystal is mainly orthorhombic system, and crystal contains b, n, c element.Polyborazine dissolves in dmf and dmso solution, explanation
Polyborazine can be with wet spinning.
Specific embodiment
Embodiment 1
The preparation method of boron nitride, comprises the steps:
(1) ammonium chloride powder is added in there-necked flask, be subsequently adding xylene solvent, be stirred vigorously so that ammonium chloride powder
Form suspension in organic solvent, be passed through nitrogen, the air in discharger and moisture；It is passed through three after being heated to 80 ~ 100 DEG C
Boron chloride gas, condensing reflux；Finally the xylene solution of the trichlorine obtaining borazine is passed through nitrogen, low-temperature heat, incites somebody to action
Dimethylbenzene in reaction system vapors away, and the colourless acicular crystal obtaining is trichlorine borazine；
(2) carry out ammonolysis reaction using prepared trichlorine borazine crystal and 2-aminopropane. and triamine alkylborazine, reaction are obtained
Leading portion is carried out in low temperature bath mixture of ice and water, and back segment is carried out at room temperature；
(3) xylene solution of triamine alkylborazine is put in there-necked flask, heat up under nitrogen protection and be heated to 100～
200 DEG C, carry out polyreaction, obtain freezing colloidal solid, the as polyborazine containing dimethylbenzene, dimethylbenzene is vapored away completely
For white powdery solids；
(4) the polyborazine precursor of drying is ground into powder, puts in people's quartz boat, quartz boat is put in tube furnace,
Before heating, tube furnace is passed through nitrogen, to diamond heating, is incubated, then allows tube furnace naturally cool to room temperature, you can to obtain
Bn through nitridation.
Embodiment 2
On the basis of embodiment 1, the temperature of described condensing reflux is 0～5 DEG C, and the response time is 10～20 h.Described
It is passed through boron trichloride gas again after being heated to 80 ~ 100 DEG C.Described reaction leading portion 5 ~ 5.5 h is in low temperature bath mixture of ice and water
Carry out, back segment 13 ~ 15 h is carried out at room temperature.The time of described polyreaction is 10 ~ 20 h.Described diamond heating
Temperature is 1000 ~ 1200 DEG C, and temperature retention time likes that you are l ~ 1.5h.
Claims (6)
1. boron nitride preparation method it is characterised in that: comprise the steps:
(1) ammonium chloride powder is added in there-necked flask, be subsequently adding xylene solvent, be stirred vigorously so that ammonium chloride powder
Form suspension in organic solvent, be passed through nitrogen, the air in discharger and moisture；It is passed through three after being heated to 80 ~ 100 DEG C
Boron chloride gas, condensing reflux；Finally the xylene solution of the trichlorine obtaining borazine is passed through nitrogen, low-temperature heat, incites somebody to action
Dimethylbenzene in reaction system vapors away, and the colourless acicular crystal obtaining is trichlorine borazine；
(2) carry out ammonolysis reaction using prepared trichlorine borazine crystal and 2-aminopropane. and triamine alkylborazine, reaction are obtained
Leading portion is carried out in low temperature bath mixture of ice and water, and back segment is carried out at room temperature；
(3) xylene solution of triamine alkylborazine is put in there-necked flask, heat up under nitrogen protection and be heated to 100～
200 DEG C, carry out polyreaction, obtain freezing colloidal solid, the as polyborazine containing dimethylbenzene, dimethylbenzene is vapored away completely
For white powdery solids；
(4) the polyborazine precursor of drying is ground into powder, puts in people's quartz boat, quartz boat is put in tube furnace,
Before heating, tube furnace is passed through nitrogen, to diamond heating, is incubated, then allows tube furnace naturally cool to room temperature, you can to obtain
Bn through nitridation.
2. boron nitride according to claim 1 preparation method it is characterised in that: the temperature of described condensing reflux be 0
～5 DEG C, the response time is 10～20 h.
3. boron nitride according to claim 1 preparation method it is characterised in that: described be heated to 80 ~ 100 DEG C after again
It is passed through boron trichloride gas.
4. boron nitride according to claim 1 preparation method it is characterised in that: described reaction leading portion 5 ~ 5.5 h exists
Carry out in low temperature bath mixture of ice and water, back segment 13 ~ 15 h is carried out at room temperature.
5. boron nitride according to claim 1 preparation method it is characterised in that: the time of described polyreaction be 10
~20 h.
6. boron nitride according to claim 1 preparation method it is characterised in that: the temperature of described diamond heating is
1000 ~ 1200 DEG C, temperature retention time is l ~ 1.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611043020.2A CN106348262A (en) | 2016-11-24 | 2016-11-24 | Preparation method of BN (boron nitride) |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611043020.2A CN106348262A (en) | 2016-11-24 | 2016-11-24 | Preparation method of BN (boron nitride) |
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| CN106348262A true CN106348262A (en) | 2017-01-25 |
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| CN201611043020.2A Pending CN106348262A (en) | 2016-11-24 | 2016-11-24 | Preparation method of BN (boron nitride) |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375094A (en) * | 2020-11-25 | 2021-02-19 | 中国人民解放军国防科技大学 | Catalyst-free high-yield synthesis method and device for trichloroborazine |
| CN113697782A (en) * | 2021-10-28 | 2021-11-26 | 北京玻钢院复合材料有限公司 | Inorganic boron nitride powder with low reactivity and preparation method thereof |
| CN114890393A (en) * | 2022-03-24 | 2022-08-12 | 中国人民解放军国防科技大学 | Low-temperature preparation method of BN microspheres |
-
2016
- 2016-11-24 CN CN201611043020.2A patent/CN106348262A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375094A (en) * | 2020-11-25 | 2021-02-19 | 中国人民解放军国防科技大学 | Catalyst-free high-yield synthesis method and device for trichloroborazine |
| CN113697782A (en) * | 2021-10-28 | 2021-11-26 | 北京玻钢院复合材料有限公司 | Inorganic boron nitride powder with low reactivity and preparation method thereof |
| CN114890393A (en) * | 2022-03-24 | 2022-08-12 | 中国人民解放军国防科技大学 | Low-temperature preparation method of BN microspheres |
| CN114890393B (en) * | 2022-03-24 | 2023-08-22 | 中国人民解放军国防科技大学 | Low-temperature preparation method of BN microsphere |
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Application publication date: 20170125 |
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