CN111423292A - Metal azide graphene compound and preparation method thereof - Google Patents
Metal azide graphene compound and preparation method thereof Download PDFInfo
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- CN111423292A CN111423292A CN201911406276.9A CN201911406276A CN111423292A CN 111423292 A CN111423292 A CN 111423292A CN 201911406276 A CN201911406276 A CN 201911406276A CN 111423292 A CN111423292 A CN 111423292A
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- azide
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B35/00—Compositions containing a metal azide
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0008—Compounding the ingredient
Abstract
The invention discloses a metal azide graphene compound and a preparation method thereof. Soluble metal salt, nano metal powder or nano metal oxide are used as raw materials, graphene oxide is used as a conductive carbon material additive, polyvinyl alcohol and the like are used as binders, and the nano metal azide graphene in any shape is prepared. The azide is prepared by putting a plurality of uniformly mixed materials in moulds with different shapes, and carrying out freeze drying, high-temperature carbonization and in-situ azide reaction. Compared with the traditional azide, the azide graphene initiating explosive obtained by the invention has the advantages that the particle size can reach hundreds of nanometers, the electrostatic sensitivity can be reduced due to the existence of conductive materials such as graphene, and the azide graphene initiating explosive can be designed into different shapes and is matched with the charging mode of a micro-initiation system.
Description
The technical field is as follows: the invention relates to a metal azide graphene compound and a preparation method thereof, and belongs to the technical field of energetic materials.
Background
With the development of weapon systems such as novel ammunition, fuze and the like towards miniaturization and intellectualization, the traditional initiation system cannot meet the current requirements due to large charge volume, large charge amount, large initiation voltage and the like. The miniaturization and practical application of MEMS (Micro-Electro-Mechanical systems) initiating explosive devices become one of the main directions for the development of initiation systems, and are accompanied by the miniaturization of charge systems and the change of charge modes. In recent years, nanoscale initiating explosive attracts attention of researchers due to excellent performances such as high specific surface area, many active sites, and fast energy release speed. Therefore, in order to meet the requirement of the development of the MEMS initiation system, the development of a high-energy, insensitive and nanoscale initiating explosive matched with the MEMS device and the development of a charging mode matched with a tiny initiating explosive device are urgently needed.
To date, common primary explosive materials include: mercury, tetrazene, lead stevensonate, lead azide, and some designed and synthesized high-energy compounds containing nitro groups, among others. In recent years, researchers have designed and synthesized a large amount of high nitrogen compounds and are expected to be applied to the field of initiating explosive, but many factors such as complexity of synthesis, low safety performance and inability of mass production have not been put into practical use. Among many kinds of initiating explosive, lead azide is widely studied and applied due to its excellent initiation performance. The copper azide and the silver azide which are both metal azide also have good initiation capability. Azides such as lead azide, silver azide and copper azide have become the most promising initiating explosive for use in small initiating devices in recent years. However, the azide has extremely high electrostatic sensitivity, and has great safety hazard in practical application. Therefore, many researchers have been doping conductive carbon materials such as carbon nanotubes, activated carbon, etc. by various methods, thereby reducing the electrostatic sensitivity. The reasonable modification method is designed, and the three metal azide modified products with moderate static sensitivity and strong initiation capability are prepared, so that the method has important significance. Graphene is undoubtedly a more ideal framework material than a specific carbon material and a carbon nanotube because of its excellent properties such as excellent conductivity, large specific surface area, and the like.
The invention aims to provide a method for preparing uniformly dispersed metal azide graphene composites with different shapes by using soluble metal salts containing copper, lead, silver and the like, nano metal or nano metal oxide as raw materials, graphene oxide and the like as frame materials, polyvinyl alcohol as a binder and performing shaping processing, freeze drying, carbonization and in-situ azidation.
Disclosure of Invention
The invention aims to provide a method for preparing a metal azide graphene composite by using cheap metal salts containing copper, lead, silver and the like, nano metal or nano metal oxide as precursor materials through the steps of adhesive shaping processing, freeze drying, carbonization, in-situ reaction and the like. On one hand, the particle size of metal azide particles can be regulated and controlled by raw materials with different nano-scales, and the electrostatic sensitivity of the metal azide is reduced by preparing the added conductive material. On the other hand, the prepared nanoscale metal azide graphene composite can be prepared into various shapes such as spheres, cylindrical graphs and cuboids with controllable diameters according to different shaping molds, and can be directly processed and formed to be matched with the structural charge of a device of a micro-detonation system.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of a metal azide graphene compound, which comprises the following specific steps:
step one, taking water as a reaction medium, adding graphene oxide, and carrying out ultrasonic treatment for 1 h;
adding soluble metal salt, nano metal or metal oxide, performing ultrasonic treatment and fully stirring for 2 hours, continuously adding the binder, and stirring for 6 hours to dissolve and uniformly disperse the binder; the content of the graphene oxide is 5-30 wt% calculated by taking the total amount of the soluble metal salt, the nano metal or the nano metal oxide and the graphene oxide as 100 wt%;
step three, placing the uniformly dispersed solution in the step two in shaping molds of different shapes, placing the molds in liquid nitrogen for freeze drying, carbonizing the freeze-dried product under an anaerobic condition, controlling the reaction temperature to be 300-1000 ℃, controlling the flow rate of protective gas to be 10-30 m L/min, and controlling the reaction time to be 60-120 min to obtain a reacted product;
and step four, placing sodium azide and stearic acid in a gas generator, controlling the reaction temperature to be 100-150 ℃, introducing the azido acid generated by the reaction into a one-way vent pipe filled with the product obtained after the reaction in the step three, and controlling the reaction time to be more than 24 hours to obtain the metal azide graphene composite.
In a preferred embodiment, the soluble metal salt includes copper nitrate, copper acetate, lead nitrate, lead acetate, and silver nitrate.
In a preferred technical scheme, the nano metal powder comprises nano copper powder, nano lead powder and nano silver powder.
In a preferred technical scheme, the nano metal oxide comprises nano copper oxide, nano silver oxide and nano lead oxide.
In a preferred technical scheme, the binder comprises polyvinyl alcohol, polyvinylpyrrolidone and polyacrylamide.
In a preferred technical scheme, the content of the graphene oxide is 5 wt% -15 wt%.
In a preferred technical scheme, the content of the graphene oxide is 15 wt% -30 wt%.
In a preferred technical scheme, the content of the binder is 1 to 50 weight percent.
In a preferred embodiment, the anaerobic condition comprises introducing nitrogen, inert gas or reducing gas.
The invention also provides application of the metal azide graphene composite, which is characterized in that the metal azide graphene composite is used as an initiating explosive.
The principle of the invention is as follows: the preparation method comprises the steps of selecting water-soluble metal salt, nano metal or nano metal oxide, graphene oxide and other conductive materials, shaping by polyvinyl alcohol and other binders, and freeze-drying to form a precursor material, wherein the material is safe and easy to prepare. And controlling the reaction time and temperature of the carbonization and azide processes to prepare the metal azide graphene composite. The invention aims to provide a method for preparing nanoscale azide initiating explosive with lower electrostatic sensitivity in any shape by gas-solid reaction with simple process and wide raw material sources.
The invention has the following beneficial effects:
the preparation process of the metal azide graphene compound is simple and easy to implement, high in yield, capable of being prepared into any shape, and applied to a micro initiating device to solve the problem of charging of micro initiating explosive devices;
due to the addition of conductive materials such as graphene, the azide graphene composite is lower in electrostatic sensitivity and higher in safety. The azide graphene composite can regulate and control the size of azide particles according to the particle size of the raw material nano copper. The azide graphene composite is a modified variety.
Detailed Description
The invention is achieved by the following examples, but the conditions and results described in the practice do not limit the content or rights of the invention.
Example 1: raw materials: polyvinyl alcohol ([ C ]2H4O]n) Copper acetate [ (CH)3COO)2Cu·H2O]Sodium azide (NaN)3) Graphene oxide, stearic acid (CH)3(CH2)16COOH)。
The main instruments and equipment comprise a magnetic stirrer, a super constant-temperature water bath, a measuring cylinder (5m L), a glass bottle (15 m L), a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
Measuring 15m L water, adding 60mg graphene oxide, performing ultrasonic treatment for 1h, adding 0.4g copper acetate into the solution A, performing ultrasonic treatment and fully stirring for 2h until the solution A is uniformly dispersed, adding 0.3g polyvinyl alcohol, stirring for 6h under the condition of 80 ℃ constant-temperature water bath to dissolve and uniformly disperse the solution A to obtain a solution for later use, pouring the solution into a cylindrical silica gel mold, placing the mold into liquid nitrogen, freezing and then placing the mold into a freeze dryer for drying for 48h, carbonizing the dried cylindrical sample under the anaerobic condition, controlling the reaction temperature to be 800 ℃, controlling the flow rate of protective gas to be 10m L/min, controlling the reaction time to be 30min, placing the carbonized product into a ventilation device through which gas generated by the co-heat of sodium azide and stearic acid passes to obtain a cylindrical copper azide graphene composite finished product, wherein the raw material charge ratio (mol) of the azide gas generation device is NaN3:CH3(CH2)16COOH is 1:1, the reaction temperature is 120 ℃, and the reaction time is 36 h.
Example 2: raw materials: polyvinyl alcohol ([ C ]2H4O]n) Copper acetate [ (C)H3COO)2Cu·H2O]Sodium azide (NaN)3) Graphene oxide, stearic acid (CH)3(CH2)16COOH)。
The main instruments and equipment comprise a magnetic stirrer, a super constant-temperature water bath, a measuring cylinder (5m L), a glass bottle (15 m L), a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
Measuring 15m L water, adding 60mg graphene oxide, performing ultrasonic treatment for 1h, adding 0.4g copper acetate into the solution A, performing ultrasonic treatment and fully stirring for 2h until the solution A is uniformly dispersed, adding 0.3g polyvinyl alcohol, stirring for 6h under the condition of 80 ℃ constant-temperature water bath to dissolve and uniformly disperse the solution A to obtain a solution for later use, dripping the solution into liquid nitrogen by using injectors with different diameters, placing the obtained spherical particles in a freeze dryer for freeze drying for 48h, carbonizing the dried spherical particles under the anaerobic condition, controlling the reaction temperature to be 800 ℃, controlling the flow rate of protective gas to be 10m L/min, controlling the reaction time to be 30min, placing the carbonized product into a ventilating device through which gas generated by sodium azide and stearic acid in a concurrent manner passes to obtain a spherical copper azide graphene composite finished product, wherein the raw material charge ratio (mol) of the azide gas generating device is NaN3:CH3(CH2)16COOH is 1:1, the reaction temperature is 120 ℃, and the reaction time is 36 h.
Example 3: raw materials: polyvinyl alcohol ([ C ]2H4O]n) Nano copper (Cu), sodium azide (NaN)3) Graphene oxide, stearic acid (CH)3(CH2)16COOH)。
The main instruments and equipment comprise a magnetic stirrer, a super constant-temperature water bath, a measuring cylinder (5m L), a glass bottle (15 m L), a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
Measuring 15m of L water, adding 60mg of graphene oxide, performing ultrasonic treatment for 1h, adding 0.4g of nano-copper into the solution A for later use, performing ultrasonic treatment and fully stirring for 2h until the nano-copper is uniformly dispersed, adding 0.3g of polyvinyl alcohol, stirring for 6h under the condition of 80 ℃ constant-temperature water bath to dissolve and uniformly disperse the nano-copper to obtain a solution for later use, dripping the solution into liquid nitrogen by using injectors with different diameters, placing the obtained spherical particles in a freeze dryer for freeze drying for 48h, drying, and freeze-dryingCarbonizing the spherical particles under the anaerobic condition, controlling the reaction temperature at 800 ℃, controlling the flow rate of protective gas at 10m L/min, controlling the reaction time at 30min, placing the carbonized product in a ventilating device through which gas passes and which is generated by sodium azide and stearic acid in a concurrent manner, and obtaining a spherical copper azide graphene composite finished product, wherein the raw material charge ratio (mol) of an azide gas generation device is NaN3:CH3(CH2)16COOH is 1:1, the reaction temperature is 120 ℃, and the reaction time is 36 h.
Example 4: raw materials: polyvinyl alcohol ([ C ]2H4O]n) Lead acetate [ (CH)3COO)2Pb·3H2O]Sodium azide (NaN)3) Graphene oxide, stearic acid (CH)3(CH2)16COOH)。
The main instruments and equipment comprise a magnetic stirrer, a super constant-temperature water bath, a measuring cylinder (5m L), a glass bottle (15 m L), a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
Measuring 15m L water, adding 60mg graphene oxide, performing ultrasonic treatment for 1h, adding 0.4g lead acetate into the standby solution A, performing ultrasonic treatment and fully stirring for 2h until the solution A is uniformly dispersed, adding 0.3g polyvinyl alcohol, stirring for 6h under the condition of 80 ℃ constant-temperature water bath to dissolve and uniformly disperse the solution A to obtain a solution for standby, pouring the solution into a cylindrical silica gel mold, placing the mold into liquid nitrogen, freezing and then placing the mold into a freeze dryer for drying for 48h, carbonizing the dried cylindrical sample under the anaerobic condition, controlling the reaction temperature to be 800 ℃, controlling the flow rate of protective gas to be 10m L/min, controlling the reaction time to be 30min, placing the carbonized product into a ventilation device through which gas generated by the co-heat of sodium azide and stearic acid passes to obtain a cylindrical lead azide graphene finished product, wherein the raw material charge ratio (mol) of the azide gas generation device is NaN3:CH3(CH2)16COOH is 1:1, the reaction temperature is 120 ℃, and the reaction time is 36 h.
Example 5: raw materials: polyvinyl alcohol ([ C ]2H4O]n) Nano lead oxide (PbO), sodium azide (NaN)3) Graphene oxide, stearic acid (CH)3(CH2)16COOH)。
The main instruments and equipment comprise a magnetic stirrer, a super constant-temperature water bath, a measuring cylinder (5m L), a glass bottle (15 m L), a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
Measuring 15m L water, adding 60mg graphene oxide, performing ultrasonic treatment for 1h, adding 0.4g nano lead oxide into the standby solution A, performing ultrasonic treatment and fully stirring for 2h until the nano lead oxide is uniformly dispersed, adding 0.3g polyvinyl alcohol, stirring for 6h under the condition of 80 ℃ constant-temperature water bath to dissolve and uniformly disperse the nano lead oxide to obtain a solution for standby, dripping the solution into liquid nitrogen by using injectors with different diameters, placing the obtained spherical particles in a freeze dryer for freeze drying for 48h, carbonizing the dried spherical particles under the anaerobic condition, controlling the reaction temperature to be 800 ℃, controlling the flow rate of protective gas to be 10m L/min, controlling the reaction time to be 30min, placing the carbonized product into a ventilation device through which gas generated by sodium azide and stearic acid co-heating passes to obtain a spherical lead azide graphene composite finished product, wherein the raw material charge ratio (mol) of the azide gas generation device is NaN3:CH3(CH2)16COOH is 1:1, the reaction temperature is 120 ℃, and the reaction time is 36 h.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a metal azide graphene compound is characterized by comprising the following steps: the preparation method comprises the following specific steps:
step one, taking water as a reaction medium, adding graphene oxide, and carrying out ultrasonic treatment for 1 h;
adding soluble metal salt, nano metal or nano metal oxide, performing ultrasonic treatment and fully stirring for 2 hours, continuously adding the binder, and stirring for 6 hours to dissolve and uniformly disperse the binder; the content of the graphene oxide is 5-30 wt% calculated by taking the total amount of the soluble metal salt, the nano metal or the nano metal oxide and the graphene oxide as 100 wt%;
step three, placing the uniformly dispersed solution in the step two in shaping molds of different shapes, placing the molds in liquid nitrogen for freeze drying, carbonizing the freeze-dried product under an anaerobic condition, controlling the reaction temperature to be 300-1000 ℃, controlling the flow rate of protective gas to be 10-30 m L/min, and controlling the reaction time to be 60-120 min to obtain a reacted product;
and step four, placing sodium azide and stearic acid in a gas generator, controlling the reaction temperature to be 100-150 ℃, introducing the azido acid generated by the reaction into a one-way vent pipe filled with the product obtained after the reaction in the step three, and controlling the reaction time to be more than 24 hours to obtain the metal azide graphene composite.
2. The method for preparing a metal azide graphene complex according to claim 1, wherein: the soluble metal salt comprises copper nitrate, copper acetate, lead nitrate, lead acetate and silver nitrate.
3. The method for preparing a metal azide graphene complex according to claim 1, wherein: the nano metal powder comprises nano copper powder, nano lead powder and nano silver powder.
4. The method for preparing a metal azide graphene complex according to claim 1, wherein: the nano metal oxide comprises nano copper oxide, nano silver oxide and nano lead oxide.
5. The method of preparing a metal azide/graphene composite according to claim 1, wherein: the binder comprises polyvinyl alcohol, polyvinylpyrrolidone and polyacrylamide.
6. The method of preparing a metal azide/graphene composite according to claim 1, wherein: the content of the graphene oxide is 5 wt% -15 wt%.
7. The method of preparing a metal azide/graphene composite according to claim 1, wherein: the content of the graphene oxide is 15 wt% -30 wt%.
8. The method of preparing a metal azide/graphene composite according to claim 1, wherein: the anaerobic condition comprises introducing nitrogen, inert gas or reducing gas.
9. A metal azide graphene composite, characterized by: the metal azide graphene composite is prepared by the preparation method of the metal azide graphene composite according to any one of claims 1 to 8.
10. Use of the metal azide graphene complex according to claim 9 as an initiator.
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Cited By (7)
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| CN112899746A (en) * | 2021-02-05 | 2021-06-04 | 南京理工大学 | Method for reducing electrostatic sensitivity of cuprous azide film |
| CN115677439A (en) * | 2021-07-28 | 2023-02-03 | 北京理工大学 | Porous carbon/graphene/azide compound and preparation method thereof |
| CN116081607A (en) * | 2023-04-06 | 2023-05-09 | 中国万宝工程有限公司 | Graphene-based cadmium azide compound and preparation method and application thereof |
| CN116082105A (en) * | 2023-04-07 | 2023-05-09 | 中国万宝工程有限公司 | Copper azide lead azide carbon fiber composite initiating explosive and preparation method thereof |
| CN116082106A (en) * | 2023-04-10 | 2023-05-09 | 中国万宝工程有限公司 | Copper azide organic compound and preparation method and application thereof |
| CN116082107A (en) * | 2023-04-10 | 2023-05-09 | 中国万宝工程有限公司 | Lead azide compound and preparation method and application thereof |
| CN116462560A (en) * | 2023-04-26 | 2023-07-21 | 中国万宝工程有限公司 | Copper azide and cadmium azide carbon fiber composite initiating explosive and preparation method thereof |
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