CN107055562A - A kind of preparation method of the high-purity diboron trioxides of powdery 5N - Google Patents
A kind of preparation method of the high-purity diboron trioxides of powdery 5N Download PDFInfo
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- CN107055562A CN107055562A CN201710340144.5A CN201710340144A CN107055562A CN 107055562 A CN107055562 A CN 107055562A CN 201710340144 A CN201710340144 A CN 201710340144A CN 107055562 A CN107055562 A CN 107055562A
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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
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1027—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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 present invention relates to a kind of preparation method of the high-purity diboron trioxides of powdery 5N, its step is：(1) hydrolyze：In 50 milliliters of clean platinum crucibles, 20 grams of high-purity boracic acid trimethyls are added, 5 grams of pure water of lower dropwise addition are then stirred for, continue to stir 5 minutes after adding, hydrolysis is completed；(2) finished product：Platinum crucible containing reactant is moved into clean quartz ampoule, quartz ampoule is put into tube furnace, under vacuum, 100 DEG C are warming up to be kept for 2 hours, platinum crucible is taken out to stir the diboron trioxide in platinum crucible with clean teflon rod, diboron trioxide is set to be uniformly heated in crucible, platinum crucible is moved into quartz ampoule again again, 200 DEG C are continuously heating under vacuum to be kept for 2 hours, it is subsequently cooled to room temperature, platinum crucible is taken out, is stored in drier, obtains the high-purity diboron trioxide of finished product powdery.
Description
Technical field
The invention belongs to chemical reagent field, especially a kind of preparation method of the high-purity diboron trioxides of powdery 5N.
Background technology
High-purity diboron trioxide typically has two kinds of outward appearances, a kind of vitreous fragment, another white powder.This Shen
Please in the high-purity diboron trioxides of 5N mentioned refer to the diboron trioxide product that purity is equal to or more than 99.999%.Powdery is high-purity
There is document report the preparation of diboron trioxide more, it is generally speaking similar.Mainly first by boric acid, repeatedly recrystallization is carried repeatedly
After pure, then gradually it is dehydrated and obtains under the conditions of certain Temperature Vacuum.For many years practice have shown that the high-purity diboron trioxide of this kind of powdery
Preparation method there are problems that.First, boric acid is big by recrystallization purification consumption of raw materials repeatedly, and yield is low, work time cost
Height, is influenceed boric acid quality unstable by operator's technical merit；Secondly, during boric acid vacuum dehydration, temperature control requirement is tighter
Lattice, the too low dehydration of temperature is slow time-consuming, and the slightly higher boric acid molten bonding dehydration of temperature is incomplete.
The content of the invention
It is an object of the invention to overcome prior art deficiency there is provided a kind of steady quality, the high powdery 5N of yield is high-purity
The preparation method of diboron trioxide.
The technical solution adopted by the present invention is：
A kind of preparation method of the high-purity diboron trioxides of powdery 5N, its step is：
(1) hydrolyze：In 50 milliliters of clean platinum crucibles, 20 grams of high-purity boracic acid trimethyls are added, lower dropwise addition is then stirred for
5 grams of pure water, continue to stir 5 minutes, hydrolysis is completed after adding；
(2) finished product：Platinum crucible containing reactant is moved into clean quartz ampoule, quartz ampoule is put into tube furnace, true
Under empty condition, it is warming up to 100 DEG C and is kept for 2 hours, takes out the clean teflon rod of platinum crucible three oxygen in platinum crucible
Change two boron to stir, diboron trioxide is uniformly heated in crucible, then platinum crucible is moved into quartz ampoule again, very
200 DEG C are continuously heating under sky to be kept for 2 hours, room temperature is subsequently cooled to, and are taken out platinum crucible, are stored in drier, obtain finished product
The high-purity diboron trioxide of powdery.
Moreover, step (1) in, the high-purity boracic acid trimethyl and pure water weight ratio are 4:1.
Moreover, step (1) in, the purity of the high-purity boracic acid trimethyl is 99.999%, prepared by purification before the reaction.
Moreover, step (1) in, electricity Zu Shuai≤12 megohm of the pure water.
Moreover, step (2) in, be warming up in the tube furnace 100 DEG C keep 2 hours before, be first warming up to 50 DEG C of holdings
Preheated within 1 hour.
Advantage of the present invention and good effect are：
The present invention directly generates high-purity three oxygen to facilitate 99.999% high-purity boracic acid trimethyl of preparation to be hydrolyzed as raw material
Change two boron, heating in vacuum dehydration prepares the technique of high-purity diboron trioxide again after contrasting using boric acid as the repeated multiple times purification of raw material,
Present invention process is simple, easily operation, and man-hour is short, and finished product yield is high, steady quality, and added value of product is high, good in economic efficiency, and
Most importantly, the purity of its reagent manufacture is unable to reach 4N grades, during prepared by chemical reagent, especially in purity
When more than 99.9%, the purity that can improve 0.01% is the presence of very big technological difficulties, and this product, which is mainly used in, partly to be led
Body is manufactured, high optics glass, and the preparation of other boride with high purity compounds etc..
Embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not limit
Qualitatively, it is impossible to which protection scope of the present invention is limited with this.
A kind of preparation method of the high-purity diboron trioxides of powdery 5N, its step is：
(1) hydrolyze：In 50 milliliters of clean platinum crucibles, 20 grams of high-purity boracic acid trimethyls are added, lower dropwise addition is then stirred for
5 grams of pure water, continue to stir 5 minutes, hydrolysis is completed after adding；
(2) finished product：Platinum crucible containing reactant is moved into clean quartz ampoule, quartz ampoule is put into tube furnace, true
Under empty condition, it is warming up to 50 DEG C and keeps preheating for 1 hour, then be warming up to 100 DEG C and kept for 2 hours, takes out that platinum crucible is clean to be gathered
Tetrafluoroethene rod stirs the diboron trioxide in platinum crucible once, diboron trioxide is uniformly heated in crucible, then
Platinum crucible is moved into quartz ampoule again, 200 DEG C are continuously heating under vacuum and is kept for 2 hours, room temperature is subsequently cooled to, platinum is taken out
Crucible, is stored in drier, obtains the high-purity diboron trioxide of finished product powdery.
High-purity boracic acid trimethyl is voluntarily prepared in the present embodiment, and purity is 99.999%, electricity Zu Shuai≤12 of pure water
Megohm.
The quality index and measured result of the high-purity diboron trioxides of 5N provided the following is above-described embodiment：
Test product：The high-purity diboron trioxides of 5N (99.999%) that the present embodiment is provided
Above analyze data shows the high-purity diboron trioxide preparation methods of powdery 5N of the present invention, high-purity three oxidations of 5N being made
Two boron finished products, every quality index meets the requirements.
The Principles of Chemical Engineering of invention are：
With pure water hydrolysis occurs for trimethylborate：2B(OCH3)3+3H2O→B2O3+6CH3OH, generates diboron trioxide
And methanol, the ingredient proportion of trimethylborate and pure water is controlled by above formula, and ensure that trimethylborate somewhat excessively prevents generation
Boric acid.Heating in vacuum methanol removal and a small amount of unreacted trimethylborate, finally obtain powdery diboron trioxide after the completion of reaction
Finished product.
Although the preparation method and preparation process of the present invention have carried out illustration by preferred embodiments, person skilled can
Present invention is not being departed from, methods and techniques described herein is being modified or reconfigured in spirit and scope, is coming real
Now final technology of preparing.In particular, all similar replacements and change for a person skilled in the art
It is it will be apparent that they are considered as being included in spirit of the invention, scope and content.
Claims (5)
1. a kind of preparation method of the high-purity diboron trioxides of powdery 5N, it is characterised in that：Its step is：
(1) hydrolyze：In 50 milliliters of clean platinum crucibles, 20 grams of high-purity boracic acid trimethyls are added, lower 5 grams of dropwise addition is then stirred for
Pure water, continues to stir 5 minutes, hydrolysis is completed after adding；
(2) finished product：Platinum crucible containing reactant is moved into clean quartz ampoule, quartz ampoule is put into tube furnace, in vacuum bar
Under part, it is warming up to 100 DEG C and is kept for 2 hours, takes out the clean teflon rod of platinum crucible three oxidations two in platinum crucible
Boron is stirred, diboron trioxide is uniformly heated in crucible, then platinum crucible is moved into quartz ampoule again, under vacuum
It is continuously heating to 200 DEG C to be kept for 2 hours, is subsequently cooled to room temperature, takes out platinum crucible, be stored in drier, obtain finished product powdery
High-purity diboron trioxide.
2. the preparation method of the high-purity diboron trioxides of powdery 5N according to claim 1, it is characterised in that：Step (1) in,
The high-purity boracic acid trimethyl is 4 with pure water weight ratio:1.
3. the preparation method of the high-purity diboron trioxides of powdery 5N according to claim 1, it is characterised in that：Step (1) in,
The purity of the high-purity boracic acid trimethyl is 99.999%, prepared by purification before the reaction.
4. the preparation method of the high-purity diboron trioxides of powdery 5N according to claim 1, it is characterised in that：Step (1) in,
Electricity Zu Shuai≤12 megohm of the pure water.
5. the preparation method of the high-purity diboron trioxides of powdery 5N according to claim 1, it is characterised in that：Step (2) in,
Be warming up in the tube furnace 100 DEG C keep 2 hours before, be first warming up to 50 DEG C of holdings and preheated for 1 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710340144.5A CN107055562A (en) | 2017-05-15 | 2017-05-15 | A kind of preparation method of the high-purity diboron trioxides of powdery 5N |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110987716A (en) * | 2019-12-17 | 2020-04-10 | 佛山纬达光电材料股份有限公司 | Method for measuring concentration of boric acid in iodine polarizing film processing tank liquid |
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| JPH01119511A (en) * | 1987-10-30 | 1989-05-11 | Mitsubishi Metal Corp | Production of high-purity boron oxide powder |
| US4908196A (en) * | 1986-07-16 | 1990-03-13 | Societa Chimica Larderello S.P.A. | Boric oxide preparation method |
| TW238292B (en) * | 1990-09-25 | 1995-01-11 | Inst Francais Du Petrole | |
| CN1107120A (en) * | 1993-11-24 | 1995-08-23 | 美国博拉克有限公司 | Production of boric oxide |
| CN1438176A (en) * | 2003-03-17 | 2003-08-27 | 郭水虎 | Method for preparing modified nano boron oxide |
| CN103523793A (en) * | 2013-10-08 | 2014-01-22 | 清远先导材料有限公司 | Method for preparing anhydrous boron oxide |
-
2017
- 2017-05-15 CN CN201710340144.5A patent/CN107055562A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4908196A (en) * | 1986-07-16 | 1990-03-13 | Societa Chimica Larderello S.P.A. | Boric oxide preparation method |
| JPH01119511A (en) * | 1987-10-30 | 1989-05-11 | Mitsubishi Metal Corp | Production of high-purity boron oxide powder |
| TW238292B (en) * | 1990-09-25 | 1995-01-11 | Inst Francais Du Petrole | |
| CN1107120A (en) * | 1993-11-24 | 1995-08-23 | 美国博拉克有限公司 | Production of boric oxide |
| EP0654442B1 (en) * | 1993-11-24 | 1999-07-07 | U.S. Borax Inc. | Production of boric oxide |
| CN1438176A (en) * | 2003-03-17 | 2003-08-27 | 郭水虎 | Method for preparing modified nano boron oxide |
| CN103523793A (en) * | 2013-10-08 | 2014-01-22 | 清远先导材料有限公司 | Method for preparing anhydrous boron oxide |
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| 高远等: "高纯氧化硼的制备", 《无机盐工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110987716A (en) * | 2019-12-17 | 2020-04-10 | 佛山纬达光电材料股份有限公司 | Method for measuring concentration of boric acid in iodine polarizing film processing tank liquid |
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Application publication date: 20170818 |