CN110358103A - Insensitive metal organic frame containing energy of one kind and preparation method thereof - Google Patents
Insensitive metal organic frame containing energy of one kind and preparation method thereof Download PDFInfo
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- CN110358103A CN110358103A CN201910642539.XA CN201910642539A CN110358103A CN 110358103 A CN110358103 A CN 110358103A CN 201910642539 A CN201910642539 A CN 201910642539A CN 110358103 A CN110358103 A CN 110358103A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 53
- 239000002184 metal Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000003446 ligand Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000725 suspension Substances 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 14
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical class [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000005352 clarification Methods 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Chemical compound [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 14
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 7
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical group [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 7
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 7
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 7
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 8
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- 230000035945 sensitivity Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 239000012621 metal-organic framework Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 3
- POCJOGNVFHPZNS-ZJUUUORDSA-N (6S,7R)-2-azaspiro[5.5]undecan-7-ol Chemical group O[C@@H]1CCCC[C@]11CNCCC1 POCJOGNVFHPZNS-ZJUUUORDSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- -1 5'-amino-1H, 1'H- [3,3'-bi (1,2,4-triazol)] -5-yl Chemical group 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- BSPUVYFGURDFHE-UHFFFAOYSA-N Nitramine Natural products CC1C(O)CCC2CCCNC12 BSPUVYFGURDFHE-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 229910001942 caesium oxide Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 159000000006 cesium salts Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- POCJOGNVFHPZNS-UHFFFAOYSA-N isonitramine Natural products OC1CCCCC11CNCCC1 POCJOGNVFHPZNS-UHFFFAOYSA-N 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 239000013384 organic framework Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B41/00—Compositions containing a nitrated metallo-organic compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
Abstract
It is [Cs (ABTNA) H the invention discloses a kind of chemical formula2O]nIt is insensitive containing can metal organic frame and preparation method thereof, the following steps are included: step 1: a certain amount of deionized water being taken to set in a round bottom flask, by a certain amount of 3- amino -3'- nitramino -5,5'- connection -1,2,4- triazole is suspended in deionized water and is stirred, and it is spare to become finely dispersed ligand suspension；Step 2: weighing the metal cesium salt of certain mass in beaker, a certain amount of deionized water is added, be configured to certain density metal cesiated salt solution, and it is stirred until it is spare as clarification metal cesiated salt solution；Step 3: after ligand suspension prepared by above-mentioned steps 1 is heated to certain temperature, the metal cesiated salt solution that step 2 configures is slowly added dropwise into ligand suspension, reaction temperature is kept for a period of time after being added dropwise to complete, the product crystal of generation is filtered, dries and obtain sterling by then natural cooling.
Description
Technical field
The present invention relates to composite material containing energy technical field, more particularly to a kind of insensitive metal containing energy is organic
Frame and preparation method thereof.
Background technique
Pyrotechnics is usually made of the oxidant and combustible that mix, has heat-producing chemical reaction.Most of all,
Redox reaction must be exothermic, self-support and be independent under certain conditions.Combustible metal powder is usually in cigarette
Play the role of combustible material in fire.Oxidant causes the oxidizing fire of combustible and generates light and heat, by dividing at high temperature
It solves oxygen and plays a role in pyrotechnics, there are commonly chlorate, perchlorate, nitrate.In order to increase the intensity of medicament, prolong
The color of the burning velocity of slow pyrotechnics, abundant pyrotechnic compound, usually uses a small amount of additive, such as epoxy resin, dextrin.
Colored flames are mainly derived from alkali metal, alkaline-earth metal or the transition metal that combustible material contains and chlorine donor (such as polychlorostyrene
Ethylene PVC, perchlorate etc.) metal chloride is formed under the high temperature conditions.Because combustible containing chlorine in combustion with gold
Belong to atom and generate useful collision, generates chemical reaction and form diatomic molecule, metallic element undergoes useful in visible light region
Electron transition to generating color.
Currently, used pyrotechnics colorant is mainly inorganic base metal and alkali salt, they have inorganic salts
The very easy moisture absorption of general properties, while perchlorate therein, villaumite and nitrate are all water pollutants, while they are right
The health of the mankind also has great injury.Therefore, develop novel metallochrome it is very necessary and be badly in need of.
Summary of the invention
The purpose of the present invention is to provide a kind of insensitive metal organic frames containing energy and preparation method thereof, and the present invention utilizes
It is insensitive containing can rich nitrogen compound 3- amino -3'- nitramino -5,5'- join -1,2,4- triazoles, from different metal cesium salts into
Row reaction prepares novel no moisture absorption metal-organic framework material containing energy, is potential pyrotechnics colorant class material, symbol
Close the insensitive energetic material of insensitive energetic material requirement.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of insensitive metal organic frame containing energy, chemical formula is [Cs (ABTNA) H2O]n, ABTNA is 3- ammonia in formula
The anion ligand of base -3'- nitramino -5,5'- connection -1,2,4- triazole.
A kind of preparation method preparing the above-mentioned insensitive metal organic frame containing energy, comprising the following steps:
Step 1: the preparation of ligand suspension
A certain amount of deionized water is taken to set in a round bottom flask, by a certain amount of 3- amino -3'- nitramino -5,5'- connection -
1,2,4- triazole is suspended in deionized water and is stirred, and it is spare to become uniform ligand suspension；
Step 2: the configuration of metal cesiated salt solution
The metal cesium salt of certain mass is weighed in beaker, a certain amount of deionized water is added, is configured to certain density
Metal cesiated salt solution, and it is stirred until it is spare as clarification metal cesiated salt solution；
Step 3: [Cs (ABTNA) H of the metal organic frame containing energy2O]nPreparation
After ligand suspension prepared by above-mentioned steps 1 is heated to certain temperature, metal cesiated salt solution that step 2 is configured
It is slowly added dropwise into ligand suspension, reaction temperature is kept for a period of time after being added dropwise to complete, then natural cooling, by the production of generation
Product crystal is filtered, dries and obtains sterling.
Specifically, in some embodiments, in the step 2, metal cesium salt is cesium carbonate or cesium hydroxide or chlorination
Caesium or cesium nitrate.
More preferably technical solution is, in the step 2, the concentration of metal cesiated salt solution is 0.1mol/L-
0.2mol/L。
More preferably technical solution is, in the step 2,3- amino -3'- nitramino -5,5'- in ligand suspension
The molar ratio of cesium ion is 1:1 in the anion ligand and metal cesiated salt solution of connection -1,2,4- triazole.
More preferably technical solution is, in the step 3, the temperature of reaction is 30-80 DEG C.
Ligand 3- amino -3'- nitramino -5,5'-, which joins -1,2,4- triazoles (HABTNA), has nitramine group, group tool
There is an acid hydrogen ion, easily and such as metal carbonate and hydroxide metathesis reaction occurs for alkaline matter.Utilize reaction original
Reason, we generate water respectively using the hydroxide and carbonate of caesium and carbon dioxide overflows, so that reacting to target product side
To progress, therefore the available cesium ion that is based on contains energy metal-organic framework material.Utilize the reaction principle, preparation metal containing energy
Organic framework materials, it is simple and easy to get without carrying out hydro-thermal reaction, it is swift in response, is conducive to later period amplification application.
Compared with the prior art, the invention has the beneficial effects that:
Insensitive [Cs (ABTNA) H of the metal organic frame containing energy prepared by the method for the present invention2O]nWith good
Safety and the performance containing energy, have good thermal stability, meet the insensitive energetic material of insensitive energetic material requirement, simultaneously
Possess excellent free-running property, can be used as the composition of pyrotechnic compound, propellant and explosive, impact sensitivity 80J, friction sensitivity is
360N.Pyrotechnics colorant field with good application prospect.Preparation method process flow of the invention is simple, operation side
Just, reaction condition is mild, and safety is good, and product quality is high.
Detailed description of the invention
Fig. 1 is the mono-crystalline structures figure of [Cs (ABTNA) H2O] n；
Fig. 2 is the TG-DSC curve of [Cs (ABTNA) H2O] n.
Specific embodiment
The present invention will be further described with reference to the examples below, and described embodiment is only present invention a part
Embodiment is not whole embodiment.Based on the embodiments of the present invention, those skilled in the art are not making
Other embodiments used obtained, belong to protection scope of the present invention under the premise of creative work.
Embodiment 1
Step 1: the preparation of ligand HABTNA suspension
It takes the deionized water of 10ml to be placed in 50ml round-bottomed flask, the HABTNA of 0.211g (1mmol) is suspended in this
In ionized water and strong stirring 30 minutes is carried out, it is spare to become uniform ligand suspension.
Step 2: the configuration of cesium carbonate solution
The cesium carbonate of 1.629g (0.5mmol) is weighed in 25ml beaker, the deionized water of 10ml is added, is configured to
The cesium carbonate solution of 0.1mol/L, and it be sufficiently stirred until it is spare as clear cesium carbonate solution.
Step 3: [Cs (ABTNA) H of the metal organic frame containing energy2O]nPreparation
After ligand suspension prepared by above-mentioned steps 1 is heated to 80 DEG C, the 0.1mol/L cesium carbonate that step 2 is configured is molten
Liquid is slowly added dropwise into ligand suspension, keeps reaction temperature 30 minutes after being added dropwise to complete, then natural cooling, by the production of generation
Product crystal is filtered, dries and obtains sterling.
Embodiment 2
Step 1: the preparation of ligand HABTNA suspension
It takes the deionized water of 10ml to be placed in 50ml round-bottomed flask, the HABTNA of 0.211g (1mmol) is suspended in this
In ionized water and strong stirring 30 minutes is carried out, it is spare to become uniform ligand suspension.
Step 2: the configuration of cesium hydroxide solution
The cesium hydroxide of 1.499g (1mmol) is weighed in 25ml beaker, the deionized water of 10ml is added, is configured to
The cesium hydroxide solution of 0.1mol/L, and it be sufficiently stirred until it is spare as clear cesium hydroxide solution.
Step 3: [Cs (ABTNA) H of the metal organic frame containing energy2O]nPreparation
After ligand suspension prepared by above-mentioned steps 1 is heated to 60 DEG C, 0.2mol/L cesium hydroxide that step 2 is configured
Solution is slowly added dropwise into ligand suspension, keeps reaction temperature 60 minutes after being added dropwise to complete, then natural cooling, by generation
Product crystal is filtered, dries and obtains sterling.
Embodiment 3
Step 1: the preparation of ligand HABTNA suspension
It takes the deionized water of 10ml to be placed in 50ml round-bottomed flask, the HABTNA of 0.211g (1mmol) is suspended in this
In ionized water and strong stirring 30 minutes is carried out, it is spare to become uniform ligand suspension.
Step 2: the configuration of cesium chloride solution
The cesium chloride of 1.684g (1mmol) is weighed in 25ml beaker, the deionized water of 10ml is added, is configured to
The cesium chloride solution of 0.2mol/L, and it be sufficiently stirred until it is spare as clear cesium chloride solution.
Step 3: [Cs (ABTNA) H of the metal organic frame containing energy2O]nPreparation
After ligand suspension prepared by above-mentioned steps 1 is heated to 60 DEG C, the 0.2mol/L cesium chloride that step 2 is configured is molten
Liquid is slowly added dropwise into ligand suspension, keeps reaction temperature 60 minutes after being added dropwise to complete, then natural cooling, by the production of generation
Product crystal is filtered, dries and obtains sterling.
Embodiment 4
Step 1: the preparation of ligand HABTNA suspension
It takes the deionized water of 10ml to be placed in 50ml round-bottomed flask, the HABTNA of 0.211g (1mmol) is suspended in this
In ionized water and strong stirring 30 minutes is carried out, it is spare to become uniform ligand suspension.
Step 2: the configuration of cesium nitrate solution
The cesium nitrate of 1.949g (1mmol) is weighed in 25ml beaker, the deionized water of 10ml is added, is configured to
The cesium nitrate solution of 0.2mol/L, and it be sufficiently stirred until it becomes clear cesium nitrate solution for standby.
Step 3: [Cs (ABTNA) H of the metal organic frame containing energy2O]nPreparation
After ligand suspension prepared by above-mentioned steps 1 is heated to 50 DEG C, the 0.2mol/L cesium nitrate that step 2 is configured is molten
Liquid is slowly added dropwise into ligand suspension, keeps reaction temperature 30 minutes after being added dropwise to complete, then natural cooling, by the production of generation
Product crystal is filtered, dries and obtains sterling.
It tests and finds through TG-DSC, in 10 DEG C of min-1With [the Cs (ABTNA) of the metal organic frame containing energy under nitrogen atmosphere
H2O]nAs shown in Figure 1, having good thermal decomposition temperature, thermal decomposition temperature is up to 225 DEG C, sees Fig. 2.Meanwhile security performance
Test shows that in BAM mechanical sensitivity test macro, the compound shows excellent security performance, impact sensitivity be greater than
80J, friction sensitivity are greater than 360N, it was demonstrated that the compound is a kind of insensitive energetic material.
Insensitive [Cs (ABTNA) H of the metal organic frame containing energy prepared through method of the invention2O]nCrystal data see
Table 1:
Table 1 is [Cs (ABTNA) H2O]nCrystal data table
The present invention relates to have with the metal containing energy that 3- amino -3'- nitramino -5,5'- connection -1,2,4- triazole is the ligand containing energy
The preparation method of machine frame frame material, based on 3- amino -3'- nitramino -5,5'- join -1,2,4- triazoles (N- (5'-amino-1H,
1'H- [3,3'-bi (1,2,4-triazol)] -5-yl) nitramine, HABTNA) and metal caesium metal salt containing can metal have
Machine frame frame material [Cs (ABTNA) H2O]nIt is reported for the first time in the present invention.The metal prepared by the method for the present invention containing energy has
Machine frame [Cs (ABTNA) H2O]n, find that it is a kind of with good thermal stability after tested, find that it is a kind of tool after tested
There is good thermal stability, meets the insensitive energetic material of insensitive energetic material requirement, impact sensitivity 80J, friction sensitivity
For 360N.Therefore, in view of the superperformance of the compound, preparation method is very important.The present invention is aiming at the change
Object is closed, the water-soluble liquid-crystalization synthetic route of a reliable, easy suitable amplification is designed and develop.This method is with HABTNA
It is raw material with different metal cesium salt, can be obtained target product by the four step simple operations such as dissolution, heating, mixing and cooling.
The route completes insensitive [Cs (ABTNA) H of the metal-organic framework material containing energy for the first time2O]nPreparation, and used raw material letter
It is singly easy to get, preparation method organic solvent-free uses, environmentally protective.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of insensitive metal organic frame containing energy, which is characterized in that its chemical formula is [Cs (ABTNA) H2O]n, in formula
ABTNA is the anion ligand of 3- amino -3'- nitramino -5,5'- connection -1,2,4- triazole.
2. the preparation method of the insensitive metal organic frame containing energy described in claim 1, which is characterized in that including following step
It is rapid:
Step 1: the preparation of ligand suspension
It takes a certain amount of deionized water to set in a round bottom flask, a certain amount of 3- amino -3'- nitramino -5,5'- is joined -1,2,
4- triazole is suspended in deionized water and is stirred, and it is spare to become finely dispersed ligand suspension；
Step 2: the configuration of metal cesiated salt solution
The metal cesium salt of certain mass is weighed in beaker, a certain amount of deionized water is added, is configured to certain density metal
Cesiated salt solution, and it is stirred until it is spare as clarification metal cesiated salt solution；
Step 3: [Cs (ABTNA) H of the metal organic frame containing energy2O]nPreparation
After ligand suspension prepared by above-mentioned steps 1 is heated to certain temperature, the metal cesiated salt solution that step 2 is configured is slow
It is added dropwise in ligand suspension, keeps reaction temperature for a period of time after being added dropwise to complete, then natural cooling, the product of generation is brilliant
Body is filtered, dries and obtains sterling [Cs (ABTNA) H2O]n。
3. the preparation method of the insensitive metal organic frame containing energy according to claim 2, which is characterized in that in the step
In rapid 2, metal cesium salt is cesium carbonate or cesium hydroxide or cesium chloride or cesium nitrate.
4. the preparation method of the insensitive metal organic frame containing energy according to claim 2, which is characterized in that in the step
In rapid 2, the concentration of metal cesiated salt solution is 0.1mol/L-0.2mol/L.
5. the preparation method of the insensitive metal organic frame containing energy according to claim 2, which is characterized in that in the step
In rapid 2, the anion ligand and metal cesium salt of -1,2,4- triazoles of 3- amino -3'- nitramino -5,5'- connection are molten in ligand suspension
The molar ratio of cesium ion is 1:1 in liquid.
6. the preparation method of the insensitive metal organic frame containing energy according to claim 2, which is characterized in that in the step
In rapid 3, the temperature of reaction is 30-80 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111875459A (en) * | 2018-09-26 | 2020-11-03 | 西安航科等离子体科技有限公司 | Pyrotechnic agent containing cesium nitrate salt and preparation method thereof |
| CN111875461A (en) * | 2018-10-13 | 2020-11-03 | 西安航科等离子体科技有限公司 | Medicament formula and preparation method of ultrahigh-energy broadband electromagnetic pulse weapon |
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| CN106883423A (en) * | 2017-02-28 | 2017-06-23 | 中国工程物理研究院化工材料研究所 | Alkali metal organic frame containing energy and preparation method thereof |
| CN109096215A (en) * | 2018-10-12 | 2018-12-28 | 中国工程物理研究院化工材料研究所 | Rich nitrogen energetic material 3- amino -3 '-nitramino -5,5 '-connection -1,2,4- triazole and preparation method thereof |
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| CN106883423A (en) * | 2017-02-28 | 2017-06-23 | 中国工程物理研究院化工材料研究所 | Alkali metal organic frame containing energy and preparation method thereof |
| CN109096215A (en) * | 2018-10-12 | 2018-12-28 | 中国工程物理研究院化工材料研究所 | Rich nitrogen energetic material 3- amino -3 '-nitramino -5,5 '-connection -1,2,4- triazole and preparation method thereof |
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| 王霆威，李燕，陈东，张祺，朱顺官: "3⁃氨基⁃3′⁃硝胺基⁃5，5′⁃联⁃1H⁃1，2，4⁃三唑的合成与表征", 《含能材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111875459A (en) * | 2018-09-26 | 2020-11-03 | 西安航科等离子体科技有限公司 | Pyrotechnic agent containing cesium nitrate salt and preparation method thereof |
| CN111875461A (en) * | 2018-10-13 | 2020-11-03 | 西安航科等离子体科技有限公司 | Medicament formula and preparation method of ultrahigh-energy broadband electromagnetic pulse weapon |
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