CN110002403A - A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method - Google Patents

A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method Download PDF

Info

Publication number
CN110002403A
CN110002403A CN201910214795.9A CN201910214795A CN110002403A CN 110002403 A CN110002403 A CN 110002403A CN 201910214795 A CN201910214795 A CN 201910214795A CN 110002403 A CN110002403 A CN 110002403A
Authority
CN
China
Prior art keywords
sodium salt
added
synthetic method
boron hydronitrogen
hydronitrogen
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910214795.9A
Other languages
Chinese (zh)
Inventor
陈学年
米童鸽
陈西孟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henan Normal University
Original Assignee
Henan Normal University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henan Normal University filed Critical Henan Normal University
Priority to CN201910214795.9A priority Critical patent/CN110002403A/en
Publication of CN110002403A publication Critical patent/CN110002403A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
    • C01B6/10—Monoborane; Diborane; Addition complexes thereof
    • C01B6/13—Addition complexes of monoborane or diborane, e.g. with phosphine, arsine or hydrazine

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The invention discloses a kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method, belong to the synthesis technical field of boron hydronitrogen.Technical solution of the present invention main points are as follows: under conditions of anhydrous and oxygen-free, ammonia borine and sodium hydride are added in reaction vessel, tetrahydrofuran solvent is added with syringe again, is then stirred to react in 50-65 DEG C, finally obtained target product boron hydronitrogen sodium salt Na [BH3NH2BH3].Operation of the present invention is simple, is easy to purify, and securely and reliably, is suitble to large-scale production.

Description

A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method
Technical field
The invention belongs to the synthesis technical fields of boron hydronitrogen, and in particular to a kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method.
Background technique
Anion [BH3NH2BH3]-It is suggested for the first time in generation 30 or 40 years in last century.Boronation scholar Stock passes through NH3With B2H6Reaction accidentally synthesized [NH3BH2NH3][BH4].In determination [NH3BH2NH3][BH4] configuration process in, it is a variety of with point Isomers is suggested, comprising: [the NH proposed in 19334]2[B2H4], [NH proposed in 19384][BH3NH2BH3], it mentions within 1956 [(NH out4)(BH2NH2)(BH4)].Confirm by years of researches, final certification NH3With B2H6The product formula of reaction is [NH3BH2NH3][BH4], rather than it is other.But the compound of other structures form also becomes synthesis in later research Emphasis.
Anion [BH has been synthesized for the first time within 20103NH2BH3]-Sodium salt, before this, having synthesized on a large amount of N has alkane Anion [the BH that base replaces3NR2BH3]-, the compound of unsubstituted finds suitable synthetic method not yet.Main cause is The operation of substituted base is relatively easy, and compound is relatively stable, and reaction condition is easy to reach.And without alkyl-substituted chemical combination The synthesis condition for the anhydrous and oxygen-free that object needs is harsher, and experimental implementation is more difficult.Girolami seminar utilizes metallic sodium within 2010 Or Sodamide and ammonia borine have synthesized Na [BH under conditions of reflux3NH2BH3](J.Am.Chem.Soc.2010,132,7254- 7255) synthetic method, but in article mentioned and purification process are relatively complicated, can not obtain pure compound, and need Want room temperature heating and the time of reflux longer.2015, Chen seminar was reacted using aminodiborane and sodium hydride (J.Am.Chem.Soc.2015,137,12406-12414), successfully synthesizes Na [BH3NH2BH3], and obtain its crystal Structure, but the synthesis, purification and the storage that synthesize raw material aminodiborane used have certain difficulty, for synthesis Na in next step [BH3NH2BH3] cause certain difficulty.
In view of Na [BH3NH2BH3] extensive use in fields such as organic reducing, energy storage materials, with current synthetic method Defect, it is necessary to continue research and develop Na [BH3NH2BH3] high-efficiency synthesis method, for after it widely application establish it is solid Basis.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of easy to operate, safe and reliable and efficient boron hydronitrogen Sodium salt Na [BH3NH2BH3] synthetic method.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method, it is characterised in that detailed process are as follows: under conditions of anhydrous and oxygen-free, by ammonia borine and sodium hydride It is added in reaction vessel, then tetrahydrofuran solvent is added with syringe, be then stirred to react in 50-65 DEG C, mesh is finally made Mark product boron hydronitrogen sodium salt Na [BH3NH2BH3]。
Further preferably, the boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method, it is characterised in that it is specific Step are as follows: in nitrogen glove box, ammonia borine and sodium hydride are fitted into schlenk reaction flask, incited somebody to action with after plug seal Schlenk reaction flask removes glove box, solvents tetrahydrofurane then is added with syringe, and wherein ammonia borine and sodium hydride feed intake Molar ratio is 2:1-5:1, and 8-20h is stirred to react in 50-65 DEG C, is added later and the isometric n-hexane of tetrahydrofuran, filtering Precipitating is removed, removing solvent is concentrated in filtrate and obtains pure white solid boron hydronitrogen sodium salt Na [BH3NH2BH3], core Its purity of Magnetic testi is close to 100%.
Boron hydronitrogen sodium salt Na [BH of the present invention3NH2BH3] synthetic method in reaction equation are as follows:
2NH3BH3+ NaH=Na [BH3NH2BH3]+NH3+H2
Compared with the prior art, the invention has the following beneficial effects: operation of the present invention is simple, product is easy to purify, raw material It is easy to get, is suitble to large-scale production.
Detailed description of the invention
Fig. 1 and Fig. 2 is the boron hydronitrogen Na [BH that the embodiment of the present invention 1 synthesizes sodium respectively3NH2BH3] in deuterated acetonitrile In11B NMR with1H NMR nuclear magnetic spectrum, target product obtained is pure Na [BH as seen from the figure3NH2BH3]。
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 under the protection of nitrogen atmosphere.In glove box, to the 100mL's equipped with magneton 0.62g ammonia borine and 0.24g sodium hydride are added in schlenk reaction flask, schlenk reaction flask is removed into hand with after plug seal Casing, and be connected on schlenk line, 30mL tetrahydrofuran solvent then is added with syringe, is stirred to react in 50 DEG C 20h, and constantly stir, 30mL n-hexane is added later into reaction flask, filters to isolate a small amount of precipitating, filtrate is concentrated It removes solvent and obtains white solid powder Na [BH3NH2BH3], obtained Na [BH3NH2BH3] it is weighed as 0.35g, calculate yield It is 52%, nuclear-magnetism detects its purity close to 100%.
Embodiment 2
All operations carry out under the protection of nitrogen atmosphere.In glove box, to the 100mL's equipped with magneton 0.93g ammonia borine and 0.24g sodium hydride are added in schlenk reaction flask, schlenk reaction flask is removed into hand with after plug seal Casing, and be connected on schlenk line, 30mL tetrahydrofuran solvent then is added with syringe, is stirred to react in 55 DEG C 16h, and constantly stir, 30mL n-hexane is added later into reaction flask, filters to isolate a small amount of precipitating, filtrate is concentrated It removes solvent and obtains white solid powder Na [BH3NH2BH3], obtained Na [BH3NH2BH3] it is weighed as 0.37g, calculate yield It is 55%, nuclear-magnetism detects its purity close to 100%.
Embodiment 3
All operations carry out under the protection of nitrogen atmosphere.In glove box, to the 100mL's equipped with magneton 1.24g ammonia borine and 0.24g sodium hydride are added in schlenk reaction flask, schlenk reaction flask is removed into hand with after plug seal Casing, and be connected on schlenk line, 30mL tetrahydrofuran solvent then is added with syringe, is stirred to react in 60 DEG C 12h, and constantly stir, 30mL n-hexane is added later into reaction flask, filters to isolate a small amount of precipitating, filtrate is concentrated It removes solvent and obtains white solid powder Na [BH3NH2BH3], obtained Na [BH3NH2BH3] it is weighed as 0.35g, calculate yield It is 52%, nuclear-magnetism detects its purity close to 100%.
Embodiment 4
All operations carry out under the protection of nitrogen atmosphere.In glove box, to the 100mL's equipped with magneton 1.55g ammonia borine and 0.24g sodium hydride are added in schlenk reaction flask, schlenk reaction flask is removed into hand with after plug seal Casing, and be connected on schlenk line, 30mL tetrahydrofuran solvent then is added with syringe, is stirred to react in 65 DEG C 8h, and constantly stir, 30mL n-hexane is added later into reaction flask, filters to isolate a small amount of precipitating, filtrate is concentrated It removes solvent and obtains white solid powder Na [BH3NH2BH3], obtained Na [BH3NH2BH3] it is weighed as 0.38g, calculate yield It is 56%, nuclear-magnetism detects its purity close to 100%.
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 (2)

1. a kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method, it is characterised in that detailed process are as follows: anhydrous Under conditions of anaerobic, ammonia borine and sodium hydride are added in reaction vessel, then tetrahydrofuran solvent is added with syringe, then It is stirred to react in 50-65 DEG C, finally obtained target product boron hydronitrogen sodium salt Na [BH3NH2BH3]。
2. boron hydronitrogen sodium salt Na [BH according to claim 13NH2BH3] synthetic method, it is characterised in that tool Body step are as follows: in nitrogen glove box, ammonia borine and sodium hydride are fitted into schlenk reaction flask, incited somebody to action with after plug seal Schlenk reaction flask removes glove box, solvents tetrahydrofurane then is added with syringe, and wherein ammonia borine and sodium hydride feed intake Molar ratio is 2:1-5:1, and 8-20h is stirred to react in 50-65 DEG C, is added later and the isometric n-hexane of tetrahydrofuran, filtering Precipitating is removed, removing solvent is concentrated in filtrate and obtains pure white solid boron hydronitrogen sodium salt Na [BH3NH2BH3], core Its purity of Magnetic testi is close to 100%.
CN201910214795.9A 2019-03-20 2019-03-20 A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method Pending CN110002403A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910214795.9A CN110002403A (en) 2019-03-20 2019-03-20 A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910214795.9A CN110002403A (en) 2019-03-20 2019-03-20 A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method

Publications (1)

Publication Number Publication Date
CN110002403A true CN110002403A (en) 2019-07-12

Family

ID=67167511

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910214795.9A Pending CN110002403A (en) 2019-03-20 2019-03-20 A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method

Country Status (1)

Country Link
CN (1) CN110002403A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113666383A (en) * 2021-08-31 2021-11-19 河南师范大学 Boron-nitrogen-hydrogen compound K [ B ]3H7NH2BH2NH2B3H7]Method of synthesis of

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837953A (en) * 2010-05-12 2010-09-22 四川大学 Novel ammonia borane composite material for hydrolysis hydrogen production
CN108358165A (en) * 2018-03-10 2018-08-03 河南师范大学 A kind of hydroboron sodium salt NaB3H8Preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837953A (en) * 2010-05-12 2010-09-22 四川大学 Novel ammonia borane composite material for hydrolysis hydrogen production
CN108358165A (en) * 2018-03-10 2018-08-03 河南师范大学 A kind of hydroboron sodium salt NaB3H8Preparation method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113666383A (en) * 2021-08-31 2021-11-19 河南师范大学 Boron-nitrogen-hydrogen compound K [ B ]3H7NH2BH2NH2B3H7]Method of synthesis of
CN113666383B (en) * 2021-08-31 2023-08-18 河南师范大学 Boron-nitrogen compound K [ B ] 3 H 7 NH 2 BH 2 NH 2 B 3 H 7 ]Is synthesized by the method of (2)

Similar Documents

Publication Publication Date Title
KR100921212B1 (en) Organometallic complexes as hydrogen storage materials and a method of preparing the same
Lingam et al. A Convenient Synthesis and a NMR Study of the Diammoniate of Diborane
CN110002403A (en) A kind of boron hydronitrogen sodium salt Na [BH3NH2BH3] synthetic method
CN109678169B (en) Novel borane derivative NH3BH2Preparation of I
CN108622857B (en) Preparation method of cyclic boron-nitrogen-hydrogen compound aminodiborane
KR101046281B1 (en) Amine Borane Synthesis
CN108358165B (en) Sodium borohydride salt NaB3H8Preparation method of (1)
CN108483397B (en) Method for synthesizing cyclic boron-nitrogen-hydrogen compound aminodiborane by one-pot method
CN113526466B (en) Boron hydrogen compound potassium salt KB 11 H 14 Is synthesized by the method of (2)
CN108439339B (en) Lithium borohydride LiB3H8Preparation method of (1)
JP5374774B2 (en) Method for producing metal cyclopentadienide
CN109705152A (en) A kind of method that the boron nitrogen chain cyclization reaction of iodine induction prepares cyclic annular boron hydronitrogen
CN113666383B (en) Boron-nitrogen compound K [ B ] 3 H 7 NH 2 BH 2 NH 2 B 3 H 7 ]Is synthesized by the method of (2)
CN110283040B (en) Synthetic method of 3-methyl-D3-benzyl bromide
CN108383809A (en) A kind of hydroboron THFB3H7Preparation method
CN111592559A (en) Method for synthesizing sodium difluorooxalate through one-step method
DE102007024145B3 (en) Molecular hydrogen storage and hydrogen transfer reagents for hydrogenation reactions
CN115181119A (en) Synthesis method of borane compound BN hexa-heterocyclic compound
CN117263197A (en) Boron hydrogen compound ammonium salt NH 4 B 9 H 14 Is synthesized by the method of (2)
CN109879294A (en) It is a kind of using B, N, Cl element as the preparation method of new polymers (NH2BHCl) x of skeleton
CN108912176A (en) A method of POCOP palladium pincer complex is prepared by co-ligand of sulfydryl carborane
TW200624422A (en) Process for production of 2-chloro-4-nitroimidazole
CN108912178A (en) A method of POCOP nickel pincer complex is prepared by co-ligand of sulfydryl carborane
JP2004083534A (en) New metal hydride cluster anion
CN115286648A (en) Synthetic method of five-membered boron nitrogen heterocyclic compound

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190712

WD01 Invention patent application deemed withdrawn after publication