CN108584996A - A kind of boron hydride ion rubidium salt compound RbB3H8Synthetic method - Google Patents
A kind of boron hydride ion rubidium salt compound RbB3H8Synthetic method Download PDFInfo
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- CN108584996A CN108584996A CN201810601570.4A CN201810601570A CN108584996A CN 108584996 A CN108584996 A CN 108584996A CN 201810601570 A CN201810601570 A CN 201810601570A CN 108584996 A CN108584996 A CN 108584996A
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- rbb
- rubidium
- salt compound
- boron hydride
- hydride ion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D17/00—Rubidium, caesium or francium compounds
- C01D17/003—Compounds of alkali metals
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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 invention discloses a kind of boron hydride ion rubidium salt compound RbB3H8Synthetic method, belong to the synthesis technical field of hydroboron.Technical scheme of the present invention main points are：A kind of boron hydride ion rubidium salt compound RbB3H8Synthetic method, metal rubidium block is added in reaction vessel under conditions of anhydrous and oxygen-free, then be added borine tetrahydrofuran solution, obtained target product boron hydride ion rubidium salt compound RbB is stirred to react in 0~50 DEG C3H8.The present invention disperses alkali metal without using any medium, is directly reacted with Alkali Metal Rb block, easy to operate, and low toxicity is harmless, securely and reliably, is suitble to large-scale production.
Description
Technical field
The invention belongs to the synthesis technical fields of hydroboron, and in particular to a kind of boron hydride ion rubidium salt compound
RbB3H8Synthetic method.
Background technology
Anion B3H8 -Tool has been widely used, and due to its higher hydrogen content, has very big answer in hydrogen storage field
With foreground, the hydrogen storage material LiB such as synthesized3H8、NaB3H8（J. Am. Chem. Soc. 2018, 140, 6718-
6726）, containing largely negative hydrogen, and have good dissolubility in common organic solvent, therefore can be used as restoring
Agent uses；And it can such as synthesize semi-conducting material MgB as the predecessor for synthesizing other boron-containing compounds2Predecessor Mg
(B3H8)2（Inorg. Chem. 2007, 46, 9060–9066）.
Due to the limitation of synthetic method, M (B3H8)nClass hydroboron is not developed well.Therefore, one is found
Planting easy to operate, safe and non-toxic and low-cost synthetic method is highly desirable.Synthesis M (B at present3H8)nClass hydroboron
Method mainly have：
1, using diborane and alkali metal, mainly sodium amalgam, reaction generates NaB3H8.Toxicity has been used in method very greatly and very
Unsafe mercury, diborane etc., mercury is very big to the harm of human body and inconvenient, and diborane is extremely sensitive to air, inflammable easy
It is quick-fried, and with severe toxicity, operate same abnormally dangerous.
2, iodine aoxidizes sodium borohydride at 100 DEG C.Solvent boiling point needed at a temperature of this is higher, consuming energy, and closes
At B3H8 -Anion contains except the solvent not fallen.
3, the tetrahydrofuran solution of sodium amalgam and borine（THF·BH3）Reaction.Equally exist lacking in the above method 1 and 2
Point.
4, alkali metallic sodium is dispersed on silica gel at 150 DEG C, is then reacted with the tetrahydrofuran of borine.Divide at this temperature
Sodium is dissipated, operation is very inconvenient, and with the presence of very high danger.
5, under conditions of ball milling, alkali metallic sodium is dispersed on inorganic salts, such as NaCl, CaCl2Deng equally existing above-mentioned side
Disadvantage in method 4.
In view of the above synthesis M (B3H8)nThe unfavorable factor of class hydroboron, it is necessary to which designing a kind of building-up process can
It avoids using the high hazardous chemicals of toxicity such as mercury, diborane, and boron hydride ion rubidium salt chemical combination easy to operate, safe and reliable
Object RbB3H8Synthetic method.
Invention content
The technical problem to be solved by the present invention is to provide a kind of easy to operate, safe and reliable and less toxic harmless boron hydrogen the moon from
Sub- rubidium salt compound RbB3H8Synthetic method.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of boron hydride ion rubidium salt compound
RbB3H8Synthetic method, it is characterised in that detailed process is：Metal rubidium block reaction is added under conditions of anhydrous and oxygen-free to hold
In device, the tetrahydrofuran solution of borine is then added, obtained target product boron hydride ion rubidium salinization is stirred to react in 0~50 DEG C
Close object RbB3H8。
Further preferably, the boron hydride ion rubidium salt compound RbB3H8Synthetic method, it is characterised in that specific step
Suddenly it is：In nitrogen glove box, by metal rubidium it is packaged enter schlenk reaction bulbs in, with after plug seal by schlenk reaction bulbs
Nitrogen glove box is removed, the tetrahydrofuran solution THFBH for the borine that molar concentration is 0.5~5mol/L is then added3, wherein
Metal rubidium block and THFBH3Molar ratio be 1:2~1:4, it is stirred to react in 0~50 DEG C until metal rubidium block disappears completely
It loses, is filtered to remove insoluble matter, filtrate, which is concentrated removing solvent, obtains white sticky solid, for several times, then very again with toluene is washed
Sky concentration removes solvent and obtains the pure boron hydride ion rubidium salt compound RbB of white3H8Powder.
Boron hydride ion rubidium salt compound RbB of the present invention3H8Synthetic method in reaction equation be：
2Rb + 4THF·BH3 = RbB3H8 + RbBH4 + 4THF。
Further preferably, the reaction temperature of building-up process is preferably room temperature.
The present invention has the advantages that compared with prior art：The present invention disperses alkali gold without using any medium
Belong to, directly reacted with alkali metal lump, easy to operate, low toxicity is harmless, securely and reliably, is suitble to large-scale production.
Description of the drawings
Fig. 1 is the boron hydride ion rubidium salt compound RbB that the embodiment of the present invention 1 synthesizes3H8In tetrahydrofuran11B
NMR liquid core magnetic charts, target product obtained is pure RbB as seen from the figure3H8。
Specific implementation mode
The above of the present 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 the above of the present invention belong to this hair
Bright range.
Embodiment 1
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, reacted to the schlenk of the 100mL equipped with magneton
1.71g metal rubidium blocks are added in bottle, schlenk reaction bulbs are removed into nitrogen glove box with after plug seal.Then addition mole
The tetrahydrofuran solution THFBH of the borine of a concentration of 1mol/L3Reaction 5 hours is stirred at room temperature in 40mL.It is filtered to remove
Filtrate is concentrated removing solvent and obtains white sticky solid by insoluble matter, and again with toluene washs solid 3 times, each 20mL, then very
Sky concentration removes solvent and obtains white solid product, the pure RbB of as solvent-free adduction3H8.Obtained RbB3H8It is weighed as
1.00g, it is 79% to calculate yield, and nuclear-magnetism detects its purity close to 100%.
Embodiment 2
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, reacted to the schlenk of the 100mL equipped with magneton
1.71g metal rubidium blocks are added in bottle, schlenk reaction bulbs are removed into nitrogen glove box with after plug seal.Then addition mole
The tetrahydrofuran solution THFBH of the borine of a concentration of 1mol/L380mL is stirred to react 9 hours at 0 DEG C.It is filtered to remove insoluble
Filtrate is concentrated removing solvent and obtains white sticky solid by object, and again with toluene washs solid 3 times, and each 20mL, then vacuum is dense
Contracting removes solvent and obtains white solid product, the pure RbB of as solvent-free adduction3H8.Obtained RbB3H8It is weighed as
1.08g, it is 85% to calculate yield, and nuclear-magnetism detects its purity close to 100%.
Embodiment 3
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, reacted to the schlenk of the 100mL equipped with magneton
1.71g metal rubidium blocks are added in bottle, schlenk reaction bulbs are removed into nitrogen glove box with after plug seal.Then addition mole
The tetrahydrofuran solution THFBH of the borine of a concentration of 0.5mol/L3Reaction 7 hours is stirred at room temperature in 80mL.It crosses and filters out
Insoluble matter is removed, filtrate, which is concentrated removing solvent, obtains white sticky solid, and again with toluene washs solid 3 times, each 20mL, then
It is concentrated in vacuo removing solvent and obtains white solid product, the pure RbB of as solvent-free adduction3H8.Obtained RbB3H8It weighs
For 1.08g, it is 85% to calculate yield, and nuclear-magnetism detects its purity close to 100%.
Embodiment 4
All operations carry out in a nitrogen atmosphere.In nitrogen glove box, reacted to the schlenk of the 100mL equipped with magneton
1.71g metal rubidium blocks are added in bottle, schlenk reaction bulbs are removed into nitrogen glove box with after plug seal.Then addition mole
The tetrahydrofuran solution THFBH of the borine of a concentration of 5mol/L38mL is stirred to react 3 hours at 50 DEG C.It is filtered to remove insoluble
Filtrate is concentrated removing solvent and obtains white sticky solid by object, and again with toluene washs solid 3 times, and each 20mL, then vacuum is dense
Contracting removes solvent and obtains white solid product, the pure RbB of as solvent-free adduction3H8.Obtained RbB3H8It is weighed as
1.03g, it is 82% to calculate yield, and nuclear-magnetism detects its purity close to 100%.
Embodiment above describes the basic principles and main features and advantage of the present invention, and 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 the originals of the present 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 (3)
1. a kind of boron hydride ion rubidium salt compound RbB3H8Synthetic method, it is characterised in that detailed process is：In anhydrous and oxygen-free
Under conditions of metal rubidium block is added in reaction vessel, the tetrahydrofuran solution of borine is then added, it is anti-in 0~50 DEG C of stirring
Target product boron hydride ion rubidium salt compound RbB should be made3H8。
2. boron hydride ion rubidium salt compound RbB according to claim 13H8Synthetic method, it is characterised in that specific step
Suddenly it is：In nitrogen glove box, by metal rubidium it is packaged enter schlenk reaction bulbs in, with after plug seal by schlenk reaction bulbs
Nitrogen glove box is removed, the tetrahydrofuran solution THFBH for the borine that molar concentration is 0.5~5mol/L is then added3, wherein
Metal rubidium block and THFBH3Molar ratio be 1:2~1:4, it is stirred to react in 0~50 DEG C until metal rubidium block disappears completely
It loses, is filtered to remove insoluble matter, filtrate, which is concentrated removing solvent, obtains white sticky solid, for several times, then very again with toluene is washed
Sky concentration removes solvent and obtains the pure boron hydride ion rubidium salt compound RbB of white3H8Powder.
3. boron hydride ion rubidium salt compound RbB according to claim 1 or 23H8Synthetic method, it is characterised in that：It closes
Reaction temperature at process is preferably room temperature.
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| CN201810601570.4A CN108584996A (en) | 2018-06-12 | 2018-06-12 | A kind of boron hydride ion rubidium salt compound RbB3H8Synthetic method |
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| CN201810601570.4A CN108584996A (en) | 2018-06-12 | 2018-06-12 | A kind of boron hydride ion rubidium salt compound RbB3H8Synthetic method |
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Application publication date: 20180928 |