CN101817537A - Method for preparing pure boron - Google Patents
Method for preparing pure boron Download PDFInfo
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- CN101817537A CN101817537A CN200910117561A CN200910117561A CN101817537A CN 101817537 A CN101817537 A CN 101817537A CN 200910117561 A CN200910117561 A CN 200910117561A CN 200910117561 A CN200910117561 A CN 200910117561A CN 101817537 A CN101817537 A CN 101817537A
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Abstract
The invention discloses a method for preparing pure boron, which comprises the following steps of: weighing corresponding powdery materials in a weight ratio of B2O3 to Mg of 1 to 2-3; performing ball milling and mixing on the materials for 8 to 16 hours; putting the mixture in a mould and compacting the mixture under the pressure of between 10 and 60 MPa; putting ignition powder on the surface of the mixture; then reacting the mixture in a high pressure kettle; blowing the high pressure kettle with argon gas at room temperature so as to discharge the air therein; discharging the air again when the temperature of the container is raised to 180 DEG C; introducing the argon gas of 1 to 6MPa into the container and continuing to raise the temperature of the container; raising the temperature in the container to about 260 DEG C to perform reaction on the ignition powder and release a large amount of heat so as to initiate the reaction between the reaction materials; and finally cooling the reaction product along with the furnace under the protection of the argon gas to room temperature so as to prepare the boron-containing material, wherein the boron content is more than 90 to 98 percent and the particle size is 0.1 to 10 mu m.
Description
Technical field
The present invention relates to the preparation technology of boron.
Background technology
Pure boron has been widely used in industries such as chemical industry, medicine, light industry, weaving, metallurgy, building materials, defence and military, the top science, agricultural, becoming one of important component of insulating material, temperature-resistant material, high-abrasive material, fire retardant material, structured material, also is the important trace element fertilizer of agricultural.Wherein, it is big that amorphous boron powder has specific surface area, and the combustion heat value advantages of higher comes into one's own in many fields such as preparation of military affairs, aerospace, automobile and advanced material.Development boron fine chemistry industry is the task of top priority of boron industry.But existing magnesiothermic reduction prepared technology exists cost height, problem that purity is low.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of pure boron.
The present invention is a kind of preparation method of pure boron, the steps include: B
2O
3Press 1: 2～3 mass ratio with Mg, take by weighing corresponding powder material, carrying out ball milling mixed 8～16 hours, place mould also with compacting under the pressure of 10～60MPa mixed material, put detonator on its surface, in autoclave, react then, at room temperature with argon purge autoclave eliminating air wherein, again exhaust when vessel temp rises to 180 ℃ by the time, the argon gas that passes into then 1～6MPa continues the rising vessel temp; Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thereby the reaction of initiation reaction storeroom cools to room temperature with the furnace and makes the boracic material under argon shield, and boron content is greater than 90～98%, granularity 0.1～10 μ m.
The present invention adopts the single step reaction legal system that spreads certainly under the protective atmosphere to get high purity, ultra-fine boron powder, shortened the warm up time of reacting; improved the yield of reaction conversion rate and boron powder; reduced the MgB compound and generated ratio, the boron powder of Sheng Chenging has reached desired granularity simultaneously.Production Flow Chart of the present invention is simple, and energy consumption is low, availablely low-cost obtains highly purified amorphous pure boron powder, and pollutes for a short time, is suitable for suitability for industrialized production.
Embodiment
The present invention is a kind of preparation method of pure boron, the steps include: B
2O
3Press 1: 2～3 mass ratio with Mg, take by weighing corresponding powder material, carrying out ball milling mixed 8～16 hours, place mould also with compacting under the pressure of 10～60MPa mixed material, put detonator on its surface, in autoclave, react then, at room temperature with argon purge autoclave eliminating air wherein, again exhaust when vessel temp rises to 180 ℃ by the time, the argon gas that passes into then 1～6MPa continues the rising vessel temp; Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thereby the reaction of initiation reaction storeroom cools to room temperature with the furnace and makes the boracic material under argon shield, and boron content is greater than 90～98%, granularity 0.1～10 μ m.
The boracic material of preparation is leached through the hydrochloric acid of 8～11.6mol/L concentration, the sodium hydroxide solution of 1～2mol/L, the hydrochloric acid of 8～11.6mol/L, will be after each the leaching through distilled water wash.
Embodiment 1:
B
2O
3With the mass ratio of Mg by 1: 3, take by weighing corresponding powder material, carrying out ball milling mixed 8～16 hours, mixed material is placed mould and uses compacting under the pressure of 60MPa, put detonator on its surface, in autoclave, react then, at room temperature with argon purge autoclave eliminating air wherein, again exhaust when vessel temp rises to 180 ℃ by the time, the argon gas that passes into then 6MPa continues the rising vessel temp; Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thereby the reaction of initiation reaction storeroom cools to room temperature with the furnace and makes the boracic material under argon shield, and boron content is 92.54%, and granularity is 10 μ m.The boracic material of preparation is leached through the hydrochloric acid of 8～11.6mol/L concentration, the sodium hydroxide solution of 1～2mol/L, the hydrochloric acid of 8～11.6mol/L, will be after each the leaching through distilled water wash.
Embodiment 2:
B
2O
3With the mass ratio of Mg by 1: 2.5, take by weighing corresponding powder material, carrying out ball milling mixed 12 hours, mixed material is placed mould and uses compacting under the pressure of 30MPa, put detonator on its surface, in autoclave, react then, at room temperature with argon purge autoclave eliminating air wherein, again exhaust when vessel temp rises to 180 ℃ by the time, the argon gas that passes into then 3MPa continues the rising vessel temp; Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thereby the reaction of initiation reaction storeroom cools to room temperature with the furnace and makes the boracic material under argon shield, and boron content is 93.61%, and granularity is 6 μ m.The boracic material of preparation is leached through the hydrochloric acid of 8～11.6mol/L concentration, the sodium hydroxide solution of 1～2mol/L, the hydrochloric acid of 8～11.6mol/L, will be after each the leaching through distilled water wash.
Embodiment 3:
B
2O
3With the mass ratio of Mg by 1: 2, take by weighing corresponding powder material, carrying out ball milling mixed 16 hours, mixed material is placed mould and uses compacting under the pressure of 50MPa, put detonator on its surface, in autoclave, react then, at room temperature with argon purge autoclave eliminating air wherein, again exhaust when vessel temp rises to 180 ℃ by the time, the argon gas that passes into then 2MPa continues the rising vessel temp; Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thereby the reaction of initiation reaction storeroom cools to room temperature with the furnace and makes the boracic material under argon shield, and boron content is 97.26%, and granularity is 0.1 μ m.The boracic material of preparation is leached through the hydrochloric acid of 8～11.6mol/L concentration, the sodium hydroxide solution of 1～2mol/L, the hydrochloric acid of 8～11.6mol/L, will be after each the leaching through distilled water wash.
Claims (2)
1. the preparation method of a pure boron the steps include: B
2O
3Press 1: 2～3 mass ratio with Mg, take by weighing corresponding powder material, carrying out ball milling mixed 8～16 hours, place mould also with compacting under the pressure of 10～60MPa mixed material, put detonator on its surface, in autoclave, react then, at room temperature with argon purge autoclave eliminating air wherein, again exhaust when vessel temp rises to 180 ℃ by the time, the argon gas that passes into then 1～6MPa continues the rising vessel temp; Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thereby the reaction of initiation reaction storeroom cools to room temperature with the furnace and makes the boracic material under argon shield, and boron content is greater than 90～98%, granularity 0.1～10 μ m.
2. according to the preparation method of the described pure boron of claim 1, it is characterized in that: the boracic material of preparation is leached through the hydrochloric acid of 8～11.6mol/L concentration, the sodium hydroxide solution of 1～2mol/L, the hydrochloric acid of 8～11.6mol/L, will be after each the leaching through distilled water wash.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910117561A CN101817537A (en) | 2009-11-02 | 2009-11-02 | Method for preparing pure boron |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910117561A CN101817537A (en) | 2009-11-02 | 2009-11-02 | Method for preparing pure boron |
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|---|---|
| CN101817537A true CN101817537A (en) | 2010-09-01 |
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|---|---|---|---|
| CN200910117561A Pending CN101817537A (en) | 2009-11-02 | 2009-11-02 | Method for preparing pure boron |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211777A (en) * | 2011-03-05 | 2011-10-12 | 兰州理工大学 | Method for preparing pure boron |
| CN104944464A (en) * | 2015-06-26 | 2015-09-30 | 武汉大学 | Method for preparing nanometer SnO2 through self-propagation high-temperature synthesizing technology |
| CN106492940A (en) * | 2016-12-01 | 2017-03-15 | 东北大学 | A kind of mechanical activation improves the technique that boron concentrate soaks boron rate |
| CN107285328A (en) * | 2017-07-31 | 2017-10-24 | 北京矿冶研究总院 | Boron powder surface purification method |
| CN108149072A (en) * | 2018-02-05 | 2018-06-12 | 南通鑫祥锌业有限公司 | A kind of zinc foil material and preparation process |
| CN108687354A (en) * | 2018-05-04 | 2018-10-23 | 北京理工大学 | A kind of preparation method of high activity Ti/2B nano-powders |
| CN109336127A (en) * | 2018-11-30 | 2019-02-15 | 深圳大学 | A kind of boron alkene and preparation method thereof |
| CN111072041A (en) * | 2019-12-24 | 2020-04-28 | 燕山大学 | Method for rapidly preparing two-dimensional boron alkene |
-
2009
- 2009-11-02 CN CN200910117561A patent/CN101817537A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211777A (en) * | 2011-03-05 | 2011-10-12 | 兰州理工大学 | Method for preparing pure boron |
| CN104944464A (en) * | 2015-06-26 | 2015-09-30 | 武汉大学 | Method for preparing nanometer SnO2 through self-propagation high-temperature synthesizing technology |
| CN106492940A (en) * | 2016-12-01 | 2017-03-15 | 东北大学 | A kind of mechanical activation improves the technique that boron concentrate soaks boron rate |
| CN106492940B (en) * | 2016-12-01 | 2018-06-26 | 东北大学 | The technique that a kind of mechanical activation improves boron concentrate leaching boron rate |
| CN107285328A (en) * | 2017-07-31 | 2017-10-24 | 北京矿冶研究总院 | Boron powder surface purification method |
| CN107285328B (en) * | 2017-07-31 | 2019-11-05 | 北京矿冶研究总院 | Boron powder surface purification method |
| CN108149072A (en) * | 2018-02-05 | 2018-06-12 | 南通鑫祥锌业有限公司 | A kind of zinc foil material and preparation process |
| CN108687354A (en) * | 2018-05-04 | 2018-10-23 | 北京理工大学 | A kind of preparation method of high activity Ti/2B nano-powders |
| CN109336127A (en) * | 2018-11-30 | 2019-02-15 | 深圳大学 | A kind of boron alkene and preparation method thereof |
| CN111072041A (en) * | 2019-12-24 | 2020-04-28 | 燕山大学 | Method for rapidly preparing two-dimensional boron alkene |
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Open date: 20100901 |