CN104098105A - Purification method for boron trichloride - Google Patents
Purification method for boron trichloride Download PDFInfo
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- CN104098105A CN104098105A CN201410356447.2A CN201410356447A CN104098105A CN 104098105 A CN104098105 A CN 104098105A CN 201410356447 A CN201410356447 A CN 201410356447A CN 104098105 A CN104098105 A CN 104098105A
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- boron trichloride
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Abstract
The invention belongs to the technical field of chemical engineering and relates to a purification method for boron trichlorid. The purification method comprises the following steps: a heating tape at the temperature of 35 DEG C is adopted to heat a boron trichloride raw material steel bottle and the temperature is controlled at 25 DEG C- 35 DEG C; boron trichloride raw materials with chlorine gas content greater than 1 ppm are heated and fully vaporized and the gas flow rate of the boron trichloride is controlled at 10 L/ min; micro-scale chlorine gas contained in the boron trichloride gas and boron carbide chlorine gas react with boron carbide at high-temperature through a boron carbide reaction layer which is 5 cm in diameter, 50 cm in height and 850 DEG C in temperature; after the reaction, the gas is cooled by a cryogenic box at the temperature of -20 DEG C and collected into product bottles. The purification method has the benefits that as the high-temperature boron carbide reaction layer is adopted by the technology, the raw materials and the boron carbide are subjected to deep contact reaction to enable the chlorine gas impurity content in the boron trichloride is reduced to less than 1 ppm.
Description
Technical field
The invention belongs to chemical technology field, specifically a kind of purification process of boron trichloride.
Background technology
Owing to using chlorine to react in boron trichloride production technique, so often contain micro-chlorine in boron trichloride product.And in the practical application of electronic grade high-purity boron trichloride, chlorine is a kind of detrimental impurity, the requirement of chlorine content is generally less than to 1ppm.For the requirement that touches the mark, also there is choice for use rectifying tower to carry out rectification and purification, but because chlorine has certain solubility in boron trichloride, simply use rectification and purification to be difficult to reach purification requirement.
Summary of the invention
In view of the defect that prior art exists, the object of this invention is to provide a kind of technique of removing micro-chlorine in boron trichloride, can make the excessive chlorine containing in boron trichloride be reduced to 1ppm once, make its index reach the requirement of electronics and high-purity boron trichloride.
Technical scheme of the present invention is: a kind of purification process of boron trichloride, steps of the method are: with the heating zones of 35 DEG C, boron trichloride raw material steel cylinder is heated, temperature is controlled between 25 DEG C ~ 35 DEG C, the boron trichloride heating raw materials that chlorine content is greater than to 1ppm is fully vaporized, control boron trichloride gas flow velocity 10L/min, be 5cm by diameter, height 50cm, temperature is the norbide responding layer of 850 DEG C, the micro-chlorine and the norbide chlorine that in boron trichloride gas, contain are at high temperature reacted with norbide, reacted gas is cooling via-20 DEG C of cryostates, collect in product bottle.
Reaction equation is:
6Cl
2 + B
4C
4BCl
3 + C。
Beneficial effect of the present invention is: this process using high temperature cabonization boron responding layer, raw material passes through the degree of depth contact reacts with norbide, and chlorine foreign matter content in boron trichloride is reduced to below 1ppm.
Brief description of the drawings
Fig. 1 is process flow diagram of the present invention.
In figure: 1, heating zone, 2, steel cylinder, 3 norbide responding layers, 4, product bottle, 5, cryostat.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in detail.
Embodiment 1:
With the heating zones of 35 DEG C 1, boron trichloride raw material steel cylinder 2 is heated between 25 DEG C ~ 35 DEG C, boron trichloride is fully vaporized, control boron trichloride gas flow velocity 10L/min, be 5cm by diameter, height 50cm, temperature is the norbide responding layer 3 of 850 DEG C, and reacted gas is cooling via-20 DEG C of cryostates 5, collects in product bottle 4.
Before and after purifying, chlorine content balance is as follows:
Embodiment 2:
Operational condition is with embodiment 1, and before and after purifying, chlorine content balance is as follows:
Embodiment 3:
Operational condition is with embodiment 1, and before and after purifying, chlorine content balance is as follows:
In above-mentioned example, although chlorine content difference (being the order of magnitude raises) in the front boron trichloride of purifying, under equal conditions, by after norbide responding layer, chlorine foreign matter content all can be down to below 1ppm, has fully proved validity of the present invention.
Claims (1)
1. the purification process of a boron trichloride, it is characterized in that, the step of this purification process is: with the heating zones of 35 DEG C (1), boron trichloride raw material steel cylinder (2) is heated, temperature is controlled between 25 DEG C ~ 35 DEG C, the boron trichloride heating raw materials that chlorine content is greater than to 1ppm is fully vaporized, control boron trichloride gas flow velocity 10L/min, be 5cm by diameter, height 50cm, temperature is the norbide responding layer (3) of 850 DEG C, the micro-chlorine and the norbide chlorine that in boron trichloride gas, contain are at high temperature reacted with norbide, reacted gas is that the cryostat (5) of-20 DEG C is cooling via temperature, collect in product bottle (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410356447.2A CN104098105A (en) | 2014-07-25 | 2014-07-25 | Purification method for boron trichloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410356447.2A CN104098105A (en) | 2014-07-25 | 2014-07-25 | Purification method for boron trichloride |
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| Publication Number | Publication Date |
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| CN104098105A true CN104098105A (en) | 2014-10-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410356447.2A Pending CN104098105A (en) | 2014-07-25 | 2014-07-25 | Purification method for boron trichloride |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731481A (en) * | 2014-12-12 | 2016-07-06 | 广东先导稀材股份有限公司 | Method and equipment for purifying boron trichloride |
| CN106957061A (en) * | 2017-05-25 | 2017-07-18 | 江西瑞合精细化工有限公司 | The boron chloride process units and method of a kind of low phosgene content |
| CN108163868A (en) * | 2017-12-29 | 2018-06-15 | 和立气体（上海）有限公司 | A kind of boron chloride purification devices |
| CN108821302A (en) * | 2018-09-05 | 2018-11-16 | 欧中电子材料（重庆）有限公司 | A kind of purification process and device of boron chloride |
| CN109195909A (en) * | 2016-06-23 | 2019-01-11 | 昭和电工株式会社 | The manufacturing method of boron chloride |
| CN112062134A (en) * | 2020-09-21 | 2020-12-11 | 齐齐哈尔大学 | Method for preparing boron trichloride-11 by utilizing solid-phase raw material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010111550A (en) * | 2008-11-07 | 2010-05-20 | Ube Ind Ltd | High-purity boron trichloride and production method thereof |
| CN102557058A (en) * | 2011-12-16 | 2012-07-11 | 天津市泰亨气体有限公司 | Method for preparing high-purity boron trifluoride |
| JP2013144644A (en) * | 2013-04-30 | 2013-07-25 | Ube Industries Ltd | Method for producing high purity boron trichloride |
-
2014
- 2014-07-25 CN CN201410356447.2A patent/CN104098105A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010111550A (en) * | 2008-11-07 | 2010-05-20 | Ube Ind Ltd | High-purity boron trichloride and production method thereof |
| CN102557058A (en) * | 2011-12-16 | 2012-07-11 | 天津市泰亨气体有限公司 | Method for preparing high-purity boron trifluoride |
| JP2013144644A (en) * | 2013-04-30 | 2013-07-25 | Ube Industries Ltd | Method for producing high purity boron trichloride |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731481A (en) * | 2014-12-12 | 2016-07-06 | 广东先导稀材股份有限公司 | Method and equipment for purifying boron trichloride |
| CN105731481B (en) * | 2014-12-12 | 2018-07-06 | 广东先导稀材股份有限公司 | Method and equipment for purifying boron trichloride |
| CN109195909A (en) * | 2016-06-23 | 2019-01-11 | 昭和电工株式会社 | The manufacturing method of boron chloride |
| CN109195909B (en) * | 2016-06-23 | 2022-08-16 | 昭和电工株式会社 | Method for producing boron trichloride |
| CN106957061A (en) * | 2017-05-25 | 2017-07-18 | 江西瑞合精细化工有限公司 | The boron chloride process units and method of a kind of low phosgene content |
| CN108163868A (en) * | 2017-12-29 | 2018-06-15 | 和立气体（上海）有限公司 | A kind of boron chloride purification devices |
| CN108821302A (en) * | 2018-09-05 | 2018-11-16 | 欧中电子材料（重庆）有限公司 | A kind of purification process and device of boron chloride |
| CN112062134A (en) * | 2020-09-21 | 2020-12-11 | 齐齐哈尔大学 | Method for preparing boron trichloride-11 by utilizing solid-phase raw material |
| CN112062134B (en) * | 2020-09-21 | 2023-05-09 | 齐齐哈尔大学 | Method for preparing boron trichloride-11 by using solid-phase raw material |
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Application publication date: 20141015 |