CN117263197A - Boron hydrogen compound ammonium salt NH 4 B 9 H 14 Is synthesized by the method of (2) - Google Patents
Boron hydrogen compound ammonium salt NH 4 B 9 H 14 Is synthesized by the method of (2) Download PDFInfo
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- CN117263197A CN117263197A CN202311292993.XA CN202311292993A CN117263197A CN 117263197 A CN117263197 A CN 117263197A CN 202311292993 A CN202311292993 A CN 202311292993A CN 117263197 A CN117263197 A CN 117263197A
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- ammonium salt
- boron hydride
- hydrogen
- hydride ammonium
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 33
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 10
- -1 Boron hydrogen compound ammonium salt Chemical class 0.000 title claims description 12
- 229910052796 boron Inorganic materials 0.000 title claims description 8
- WZMUUWMLOCZETI-UHFFFAOYSA-N azane;borane Chemical compound B.N WZMUUWMLOCZETI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007787 solid Substances 0.000 claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000001308 synthesis method Methods 0.000 claims abstract description 13
- 239000011232 storage material Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 231100000053 low toxicity Toxicity 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- JJXBITPDOUWVAI-UHFFFAOYSA-N Bc1ccc(F)c(F)c1F Chemical compound Bc1ccc(F)c(F)c1F JJXBITPDOUWVAI-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- UORVGPXVDQYIDP-BJUDXGSMSA-N borane Chemical class [10BH3] UORVGPXVDQYIDP-BJUDXGSMSA-N 0.000 description 1
- 229910010277 boron hydride Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
-
- 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
- C01B35/02—Boron; Borides
- C01B35/026—Higher boron hydrides, i.e. containing at least three boron atoms
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
Abstract
The invention discloses a boron hydride ammonium salt NH 4 B 9 H 14 The synthesis method comprises the following specific processes: under anhydrous and anaerobic condition, KB is used 9 H 14 And NH 4 Cl is used as a reaction raw material, liquid ammonia is used as a solvent, and the pure target product boron hydride ammonium salt NH is prepared through stirring reaction at the temperature of-70 to-40 DEG C 4 B 9 H 14 . By testing the boron hydride ammonium salt NH 4 B 9 H 14 Is capable of thermally decomposing to release hydrogen, indicating that the boron hydride ammonium salt NH 4 B 9 H 14 Can be used as a potential solid hydrogen storage material. The invention has simple operation, low toxicity, no harm, safety, reliability and low cost, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of synthesis of boron hydrogen compounds, and in particular relates to a boron hydrogen compound ammonium salt NH 4 B 9 H 14 Is a synthetic method of (a).
Background
Anion B having polyhedral structure 9 H 14 - Great attention has been paid to researchers because of their wide use. For example, the corresponding alkali metal salt thereof can be used as a solid electrolyte, andexhibits good ion conductivity. Thus, alkali metal salts of this type MB 9 H 14 The boron hydride compound has a very good application prospect, and provides a feasible scheme for solving the defect of low safety performance of the liquid electrolyte battery. For another example, the corresponding ammonium salt NH 4 B 9 H 14 Is a solid hydrogen storage material with very good application prospect, and is combined with NH 4 B 3 H 8 Similar to%Inorg. Chem.2011, 50, 3738-3742). However, with MB 9 H 14 In contrast, boron hydride ammonium salt NH 4 B 9 H 14 The synthesis methods of (2) are less recently reported and generally have the following disadvantages in the previous synthesis methods: 1) Most synthesis methods involve the use of diborane, which is a flammable and explosive toxic gas, and the use process is very prone to safety problems; 2) Besides diborane, expensive reagents such as trifluorophenyl borane are generally used, and the use of the reagents leads to a significant increase in the synthesis cost and is not beneficial to large-scale synthesis; 3) The synthesis process needs relatively high temperature (150-220 ℃), the temperature range is obviously higher than the temperature of the general chemical reaction, the energy consumption is large, and the environment-friendly synthesis concept is not met; 4) The reaction process is not easy to control due to the required conditions, so that various other borane compounds are mixed in the generated product, the difficulty is increased for the subsequent separation and purification, and the yield is low.
Due to the limitation of the synthesis method, the boron hydride ammonium salt NH 4 B 9 H 14 Is not well developed. Therefore, there is a need to design a boron hydride ammonium salt NH which has controllable synthesis process, simple operation, low cost, safety and reliability 4 B 9 H 14 Lays a foundation for the corresponding research of the method. The raw material KB used in the present invention 9 H 14 The product was synthesized based on the prior patent technology of this group (ZL 202210334139.4).
Disclosure of Invention
The invention solves the technical problem of providing a synthetic processBoron hydride ammonium salt NH with simple control and operation, safety and reliability and low cost 4 B 9 H 14 By testing the corresponding heat analysis hydrogen performance, the result shows that the boron hydrogen compound ammonium salt NH 4 B 9 H 14 Has excellent hydrogen storage performance.
The invention adopts the following technical proposal to solve the technical problems that the boron hydride ammonium salt NH 4 B 9 H 14 The synthesis method is characterized by comprising the following specific steps: under anhydrous and anaerobic condition, KB is used 9 H 14 And NH 4 Cl is used as a reaction raw material, liquid ammonia is used as a solvent, and the pure target product boron hydride ammonium salt NH is prepared through stirring reaction at the temperature of-70 to-40 DEG C 4 B 9 H 14 。
Further preferably, the boron hydride ammonium salt NH 4 B 9 H 14 The synthesis method is characterized by comprising the following specific steps: KB was then placed in a nitrogen glove box 9 H 14 And NH 4 Cl is filled into a schlenk reaction bottle according to the mol ratio of 1:1, a plug is used for sealing, the schlenk reaction bottle is removed from a glove box, liquid ammonia is used as a solvent, stirring reaction is carried out for 2-10 h at the temperature of-70 to-40 ℃, liquid ammonia is naturally volatilized at normal temperature to obtain a white solid, anhydrous acetonitrile is added for extraction, filtrate is concentrated to remove the solvent to obtain the white solid after filtration, the solid is washed by normal hexane, and a white solid product boron hydrogen compound ammonium salt NH with the purity close to 100% is obtained by pumping the solid 4 B 9 H 14 。
It is further preferred that the reaction temperature during the synthesis is-50℃and the reaction time is 4 hours.
The invention relates to boron hydride ammonium salt NH 4 B 9 H 14 The reaction equation in the synthesis method is:
KB 9 H 14 + NH 4 Cl = NH 4 B 9 H 14 +KCl。
the invention relates to boron hydride ammonium salt NH 4 B 9 H 14 Can be used as a solid hydrogen storage material, the boron hydride ammonium salt NH 4 B 9 H 14 Thermally decomposing at 100-120 ℃ to release hydrogen, wherein the amount of released hydrogen is boron hydride ammonium salt NH 4 B 9 H 14 7-9% of the weight of the hydrogen storage material can meet the requirements of releasing hydrogen and the hydrogen release amount of the hydrogen storage material under mild conditions.
Compared with the prior art, the invention has the following advantages and beneficial effects: the invention has simple operation, low toxicity, no harm, safety, reliability and low cost, is suitable for large-scale production, and lays a foundation for application research. Subsequently, we tested the NH 4 B 9 H 14 The thermal decomposition performance of the compound and the fact that the released gas is hydrogen gas are confirmed by mass spectrum show that the compound can be used as a potential solid hydrogen storage material.
Drawings
FIG. 1 is a boron hydride ammonium salt NH synthesized in example 1 4 B 9 H 14 In deuterated DMSO 11 B and 11 B{ 1 h } liquid nuclear magnetic diagram, and the target product prepared by the diagram is pure NH 4 B 9 H 14 。
FIG. 2 is a boron hydride ammonium salt NH synthesized in example 1 4 B 9 H 14 Thermal decomposition performance diagram, from which the boron hydride ammonium salt NH can be seen 4 B 9 H 14 The thermal decomposition starts at 110 ℃ to release hydrogen, and the amount of the released hydrogen is about the NH of the boron hydrogen compound ammonium salt 4 B 9 H 14 8% of the weight of the boron hydride ammonium salt NH can meet the requirements of hydrogen release and hydrogen release amount of the hydrogen storage material under mild conditions 4 B 9 H 14 Can be used as a potential solid hydrogen storage material.
Detailed Description
The above-described matters of the present invention will be described in further detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within the scope of the present invention.
Examples
All operations were performed under nitrogen atmosphere. In a glove box, 50mL of the mixture was fed with magnetonInto a lenk flask was charged 0.304g KB 9 H 14 And 0.107g NH 4 Cl, after sealing with a stopper, the schlenk flask was removed from the glove box, followed by 15mL of liquid ammonia as solvent, and the reaction was stirred at-70℃for 10h. And naturally volatilizing liquid ammonia at normal temperature to obtain a white solid, adding anhydrous acetonitrile for extraction, filtering, and concentrating the filtrate to remove the solvent to obtain the white solid. Washing the solid with n-hexane, and pumping the solid to obtain white solid product boron hydride ammonium salt NH 4 B 9 H 14 The calculated yield is 60% and the purity of the nuclear magnetic resonance is close to 100%.
Examples
All operations were performed under nitrogen atmosphere. In a glove box, 0.304g KB was added to a 50mL schlenk flask containing a magneton 9 H 14 And 0.107g NH 4 Cl, after sealing with a stopper, the schlenk flask was removed from the glove box, followed by 15mL of liquid ammonia as solvent, and the reaction was stirred at-60℃for 8h. And naturally volatilizing liquid ammonia at normal temperature to obtain a white solid, adding anhydrous acetonitrile for extraction, filtering, and concentrating the filtrate to remove the solvent to obtain the white solid. Washing the solid with n-hexane, and pumping the solid to obtain white solid product boron hydride ammonium salt NH 4 B 9 H 14 The calculated yield was 62% and the purity of the nuclear magnetic detection was close to 100%.
Examples
All operations were performed under nitrogen atmosphere. In a glove box, 0.304g KB was added to a 50mL schlenk flask containing a magneton 9 H 14 And 0.107g NH 4 Cl, after sealing with a stopper, the schlenk flask was removed from the glove box, followed by 15mL of liquid ammonia as solvent, and the reaction was stirred at-50℃for 4h. And naturally volatilizing liquid ammonia at normal temperature to obtain a white solid, adding anhydrous acetonitrile for extraction, filtering, and concentrating the filtrate to remove the solvent to obtain the white solid. Washing the solid with n-hexane, and pumping the solid to obtain white solid product boron hydride ammonium salt NH 4 B 9 H 14 The yield was calculated to be 78% and the purity was close to 100% by nuclear magnetic detection.
Examples
All operations were performed under nitrogen atmosphere. In a glove boxInto a 50mL schlenk flask containing a magneton, 0.304g KB was added 9 H 14 And 0.107g NH 4 Cl, after sealing with a stopper, the schlenk flask was removed from the glove box, followed by 15mL of liquid ammonia as solvent, and the reaction was stirred at-40℃for 2h. And naturally volatilizing liquid ammonia at normal temperature to obtain a white solid, adding anhydrous acetonitrile for extraction, filtering, and concentrating the filtrate to remove the solvent to obtain the white solid. Washing the solid with n-hexane, and pumping the solid to obtain white solid product boron hydride ammonium salt NH 4 B 9 H 14 The calculated yield was 63% and the purity of the nuclear magnetic detection was close to 100%.
While the basic principles, principal features and advantages of the present invention have been described in the foregoing examples, it will be appreciated by those skilled in the art that the present invention is not limited by the foregoing examples, but is merely illustrative of the principles of the invention, and various changes and modifications can be made without departing from the scope of the invention, which is defined by the appended claims.
Claims (5)
1. Boron hydrogen compound ammonium salt NH 4 B 9 H 14 The synthesis method is characterized by comprising the following specific steps: under anhydrous and anaerobic condition, KB is used 9 H 14 And NH 4 Cl is used as a reaction raw material, liquid ammonia is used as a solvent, and the pure target product boron hydride ammonium salt NH is prepared through stirring reaction at the temperature of-70 to-40 DEG C 4 B 9 H 14 。
2. The boron hydride ammonium salt NH according to claim 1 4 B 9 H 14 The synthesis method is characterized by comprising the following specific steps: KB was then placed in a nitrogen glove box 9 H 14 And NH 4 Cl is filled into a schlenk reaction bottle according to the mol ratio of 1:1, a plug is used for sealing, the schlenk reaction bottle is removed from a glove box, liquid ammonia is introduced as a solvent, stirring reaction is carried out for 2-10 h at the temperature of-70 to-40 ℃, liquid ammonia is naturally volatilized at normal temperature to obtain white solid, anhydrous acetonitrile is added for extraction, filtrate is concentrated to remove the solvent after filtration to obtain white solid, and n-hexane is used for preparing the white solidWashing the solid with alkane, and pumping the solid to obtain white solid product boron hydride ammonium salt NH with purity close to 100% 4 B 9 H 14 。
3. The boron hydride ammonium salt NH according to claim 1 or 2 4 B 9 H 14 The synthesis method of (2) is characterized in that: the reaction temperature in the synthesis process is-50 ℃ and the reaction time is 4 hours.
4. The boron hydride ammonium salt NH according to claim 1 or 2 4 B 9 H 14 The synthesis method is characterized in that the reaction equation in the synthesis process is as follows: KB (KB) 9 H 14 + NH 4 Cl = NH 4 B 9 H 14 +KCl。
5. The boron hydride ammonium salt NH according to claim 1 or 2 4 B 9 H 14 The synthesis method of (2) is characterized in that: the boron hydride ammonium salt NH 4 B 9 H 14 Can be used as a solid hydrogen storage material, the boron hydride ammonium salt NH 4 B 9 H 14 Thermally decomposing at 100-120 ℃ to release hydrogen, wherein the amount of released hydrogen is boron hydride ammonium salt NH 4 B 9 H 14 7-9% of the weight of the hydrogen storage material can meet the requirements of releasing hydrogen and the hydrogen release amount of the hydrogen storage material under mild conditions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311292993.XA CN117263197A (en) | 2023-10-08 | 2023-10-08 | Boron hydrogen compound ammonium salt NH 4 B 9 H 14 Is synthesized by the method of (2) |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311292993.XA CN117263197A (en) | 2023-10-08 | 2023-10-08 | Boron hydrogen compound ammonium salt NH 4 B 9 H 14 Is synthesized by the method of (2) |
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| Publication Number | Publication Date |
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| CN117263197A true CN117263197A (en) | 2023-12-22 |
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| CN202311292993.XA Pending CN117263197A (en) | 2023-10-08 | 2023-10-08 | Boron hydrogen compound ammonium salt NH 4 B 9 H 14 Is synthesized by the method of (2) |
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2023
- 2023-10-08 CN CN202311292993.XA patent/CN117263197A/en active Pending
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