CN109879294A - It is a kind of using B, N, Cl element as the preparation method of new polymers (NH2BHCl) x of skeleton - Google Patents
It is a kind of using B, N, Cl element as the preparation method of new polymers (NH2BHCl) x of skeleton Download PDFInfo
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- CN109879294A CN109879294A CN201910137556.8A CN201910137556A CN109879294A CN 109879294 A CN109879294 A CN 109879294A CN 201910137556 A CN201910137556 A CN 201910137556A CN 109879294 A CN109879294 A CN 109879294A
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Abstract
The invention discloses a kind of using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xPreparation method, detailed process are as follows: by pure NH under conditions of anhydrous and oxygen-free3BH3Cl is added in reaction vessel, adds ether dissolution, in 0~30 DEG C of dropwise addition ether solution of hydrogen chloride HClEt2O, is stirred to react 2h then at 0~30 DEG C, then drains solvent, and dry target product (NH is obtained after being drained again with n-hexane washed product2BHCl)xPowder.Operation of the present invention is simple, is easily purified, and securely and reliably, is suitble to large-scale production.
Description
Technical field
The invention belongs to the synthesis technical fields of boron-nitrogen compound, and in particular to a kind of using B, N, Cl element as the new of skeleton
Type polymer (NH2BHCl)xPreparation method.
Background technique
The poly- nitrogen boron fiber of height has the good characteristics such as high temperature resistant, resistant to chemical etching, and dielectric properties are excellent, insulation
Property good and thermal conductivity it is good, have certain hydrogen storage ability, have in the sophisticated technologies such as Aeronautics and Astronautics, electric power, electronics field and widely answer
Use prospect.
In recent ten years, domestic and foreign scholars have carried out numerous studies, are prepared for the polyborazine of diversified forms.But synthesis side
Method never obtains improving development well, and synthetic method is complicated and synthetic route is longer, causes in recent years to such chemical combination
The progress of object is little.Therefore finding a kind of convenient preparation method is just highly desirable.Synthesis boron nitrogen class high polymer now
Main method have following two: 1, using heavy metal catalyst ruthenium, rhodium, palladium etc. catalysis borine decompose, such method generation
Valence is high, low yield, and most catalyst have toxicity, and environment is unfriendly, is not suitable for high-volume and synthesizes；2, high temperature (> 100 DEG C)
High pressure (> 2MPa) environment decomposes borine, and such method cost is high, and experiment condition is harsh, and product is not easily recycled after test, dangerous
Coefficient is big, is not suitable for high-volume and synthesizes.
In view of the unfavorable factor of the above synthesis boron nitrogen high polymer, and most boron nitrogen high polymers do not have other members in addition to boron nitrogen hydrogen
Element participates in, and causes property between various high polymers not have too many differences, has no and be obviously improved.It is therefore necessary to design a kind of synthesized
Journey can be avoided the hazardous chemical high using toxicity such as heavy metal catalysts, and in easy to operate, safe and reliable product simultaneously
Contain the synthetic method that can promote product overall performance of other elements again.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of low in cost, easy to operate, safe and reliable and less toxic harmless
Using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xPreparation method.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of using B, N, Cl element as the novel of skeleton
Polymer (NH2BHCl)xPreparation method, it is characterised in that detailed process are as follows: will be pure under conditions of anhydrous and oxygen-free
NH3BH3Cl is added in reaction vessel, adds ether dissolution, in 0~30 DEG C of dropwise addition ether solution of hydrogen chloride HClEt2O,
It is stirred to react 2h then at 0~30 DEG C, then drains solvent, dry target is obtained after being drained again with n-hexane washed product
Product (NH2BHCl)xPowder.
Preferably, the NH3BH2Cl and HClEt2The molar ratio of O is 1:0.5~1.5.
Preferably, the NH3BH2Cl and HClEt2The molar ratio of O is 1:1.
Preferably, described using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xPreparation method, feature
It is specific steps are as follows: in nitrogen glove box, by 65.5mg chloro ammonia borine NH3BH2Cl is packed into 100mL Schlenk reaction
In bottle, Schlenk reaction flask is removed into glove box with after plug seal, adds the 25mL ether by water removal of distilling, flow back
Then the diethyl ether solution HClEt for the HCl that 10mL molar concentration is 1mol/L is added in stirring in draught cupboard2O, wherein
NH3BH2Cl and HClEt2The molar ratio of O is 1:1, is stirred to react 2h in 20 DEG C, drains solvent, washs three with n-hexane
It is drained again after secondary and obtains dry target product (NH2BHCl)xPowder.
It is of the present invention using B, N, Cl element as the new polymers (NH of skeleton2BHCl) anti-in the preparation method of x
Answer equation are as follows:
Compared with the prior art, the invention has the following beneficial effects: operation of the present invention is simple, it is easily purified, securely and reliably,
It is suitble to large-scale production.
Detailed description of the invention
Fig. 1 is that embodiment 1 is obtained using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xIn ether11B liquid core magnetic chart.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, by 65.5mg chloro ammonia borine NH3BH2Cl
It is fitted into 100mL Schlenk reaction flask, Schlenk reaction flask is removed into glove box with after plug seal, is added by steaming
It evaporates, the 25mL ether stirring for the water removal that flows back, the ether for the HCl that 10mL molar concentration is 1mol/L is then added in draught cupboard
Solution H ClEt2O, wherein NH3BH2Cl and HClEt2The molar ratio of O is 1:1, is stirred to react 2h in 20 DEG C, drains molten
Agent drains again after being washed three times with n-hexane and obtains dry target product (NH2BHCl)xPowder.
Embodiment 2
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, by 65.5mg chloro ammonia borine NH3BH2Cl
It is fitted into 100mL Schlenk reaction flask, Schlenk reaction flask is removed into glove box with after plug seal, is added by steaming
It evaporates, the 25mL ether stirring for the water removal that flows back, the ether for the HCl that 10mL molar concentration is 1mol/L is then added in draught cupboard
Solution H ClEt2O, wherein NH3BH2Cl and HClEt2The molar ratio of O is 1:1, is stirred to react 2h in 23 DEG C, drains molten
Agent drains again after washing five times with n-hexane and obtains dry target product (NH2BHCl)xPowder.
Embodiment 3
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, by 131mg chloro ammonia borine NH3BH2Cl dress
Enter in 100mL Schlenk reaction flask, with after plug seal by Schlenk reaction flask remove glove box, add by distillation,
The 30mL ether stirring of reflux water removal, is then added the diethyl ether solution for the HCl that 10mL molar concentration is 1mol/L in draught cupboard
HCl·Et2O, wherein NH3BH2Cl and HClEt2The molar ratio of O is 2:1, is stirred to react 2h in 25 DEG C, drains solvent,
It is drained again after being washed three times with n-hexane and obtains dry target product (NH2BHCl)xPowder.
Embodiment 4
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, by 65.5mg chloro ammonia borine NH3BH2Cl
It is fitted into 100mL Schlenk reaction flask, Schlenk reaction flask is removed into glove box with after plug seal, is added by steaming
It evaporates, the 25mL ether stirring for the water removal that flows back, the ether for the HCl that 15mL molar concentration is 1mol/L is then added in draught cupboard
Solution H ClEt2O, wherein NH3BH2Cl and HClEt2The molar ratio of O is 1:1.5, is stirred to react 1h in 23 DEG C, drains
Solvent is drained again after washing five times with n-hexane and obtains dry target product (NH2BHCl)xPowder.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (4)
1. a kind of using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xPreparation method, it is characterised in that specific mistake
Journey are as follows: by pure NH under conditions of anhydrous and oxygen-free3BH3Cl is added in reaction vessel, adds ether dissolution, in 0~30
DEG C be added dropwise ether solution of hydrogen chloride HClEt2O is stirred to react 2h then at 0~30 DEG C, then drains solvent, washed with n-hexane
Product obtains dry target product (NH after draining again2BHCl)xPowder.
2. according to claim 1 using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xPreparation method,
It is characterized in that: the NH3BH2Cl and HClEt2The molar ratio of O is 1:0.5~1.5.
3. according to claim 1 using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xPreparation method,
It is characterized in that: the NH3BH2Cl and HClEt2The molar ratio of O is 1:1.
4. according to claim 1 using B, N, Cl element as the new polymers (NH of skeleton2BHCl)xPreparation method,
It is characterized in that specific steps are as follows: in nitrogen glove box, by 65.5mg chloro ammonia borine NH3BH2Cl is packed into 100mL Schlenk
In reaction flask, Schlenk reaction flask is removed into glove box with after plug seal, adds the 25mL by water removal of distilling, flow back
Then the diethyl ether solution HClEt for the HCl that 10mL molar concentration is 1mol/L is added in ether stirring in draught cupboard2O, wherein
NH3BH2Cl and HClEt2The molar ratio of O is 1:1, is stirred to react 2h in 20 DEG C, drains solvent, washs three with n-hexane
It is drained again after secondary and obtains dry target product (NH2BHCl)xPowder.
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| CN201910137556.8A CN109879294A (en) | 2019-02-25 | 2019-02-25 | It is a kind of using B, N, Cl element as the preparation method of new polymers (NH2BHCl) x of skeleton |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010320A (en) * | 2020-08-12 | 2020-12-01 | 河南师范大学 | Preparation method of B-substituted sodium cyanoborohydride |
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| US5053365A (en) * | 1990-02-28 | 1991-10-01 | The Ohio State University Research Foundation | Method for the low temperature preparation of amorphous boron nitride using alkali metal and haloborazines |
| US5169613A (en) * | 1991-02-06 | 1992-12-08 | The Ohio State University Research Foundation | Method for the preparation of boron nitride using ammonia-monohaloborane |
| FR2958286A1 (en) * | 2010-03-30 | 2011-10-07 | Univ Claude Bernard Lyon | NOVEL PRECURSORS OF THE METALLOBORAZINE TYPE, PROCESS AND MATERIALS OBTAINED FROM SUCH PRECURSORS |
| CN103113397A (en) * | 2013-02-05 | 2013-05-22 | 武汉大学 | Preparation method of amino borane |
| CN104923297A (en) * | 2015-05-14 | 2015-09-23 | 大连理工大学 | Iridium catalyst used for catalyzing ammonia borane hydrolysis hydrogen production process, and preparation method and application thereof |
| EP3081528A1 (en) * | 2015-04-17 | 2016-10-19 | Justus-Liebig-Universität Gießen | Method for release of hydrogen from the adduct of ammonia and borane and use of transition metal free multidentate catalysts for release of hydrogen from the adduct of ammonia and borane |
| CN108586266A (en) * | 2018-06-07 | 2018-09-28 | 东莞市乐远化工科技有限公司 | A kind of dimethyamine borane synthesis technology |
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2019
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| US5053365A (en) * | 1990-02-28 | 1991-10-01 | The Ohio State University Research Foundation | Method for the low temperature preparation of amorphous boron nitride using alkali metal and haloborazines |
| US5169613A (en) * | 1991-02-06 | 1992-12-08 | The Ohio State University Research Foundation | Method for the preparation of boron nitride using ammonia-monohaloborane |
| FR2958286A1 (en) * | 2010-03-30 | 2011-10-07 | Univ Claude Bernard Lyon | NOVEL PRECURSORS OF THE METALLOBORAZINE TYPE, PROCESS AND MATERIALS OBTAINED FROM SUCH PRECURSORS |
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| EP3081528A1 (en) * | 2015-04-17 | 2016-10-19 | Justus-Liebig-Universität Gießen | Method for release of hydrogen from the adduct of ammonia and borane and use of transition metal free multidentate catalysts for release of hydrogen from the adduct of ammonia and borane |
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| CN112010320A (en) * | 2020-08-12 | 2020-12-01 | 河南师范大学 | Preparation method of B-substituted sodium cyanoborohydride |
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