CN111422855A - Foam graphene-based metal azide compound and preparation method thereof - Google Patents
Foam graphene-based metal azide compound and preparation method thereof Download PDFInfo
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- CN111422855A CN111422855A CN201911412079.8A CN201911412079A CN111422855A CN 111422855 A CN111422855 A CN 111422855A CN 201911412079 A CN201911412079 A CN 201911412079A CN 111422855 A CN111422855 A CN 111422855A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/08—Hydrazoic acid; Azides; Halogen azides
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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
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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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Abstract
The invention provides a foam graphene-based metal azide compound and a preparation method thereof. Soluble metal salt, nano metal powder or nano metal oxide are used as raw materials, and graphene is used as a conductive carbon material carrier to prepare the foam graphene-based metal azide composite. The azide is a metal azide initiating explosive material which takes foam graphene as a base and is prepared by uniformly dispersing nano metal/metal oxide in graphene oxide solution and carrying out high-temperature hydrothermal reduction reaction, freeze drying and in-situ azide reaction. Compared with the traditional azide, the particle size of the foam graphene-based azide initiating explosive can reach hundreds of nanometers, and the existence of the graphene conductive material can greatly reduce the electrostatic sensitivity and greatly improve the safety of the foam graphene-based azide initiating explosive.
Description
Technical Field
The invention relates to a foam graphene-based metal azide compound and a preparation method thereof, and belongs to the technical field of energetic materials.
Background
The initiating explosive is an initial energy substance which is very sensitive to external action and is widely applied to initiating systems such as detonators, fuses and the like. With the development of a micro-type initiating system, the traditional initiating explosive cannot meet the characteristic requirements of low input and high output, and the development and synthesis of the initiating explosive suitable for the micro-type initiating system are particularly challenging. Lead azide is widely used due to its high initiation ability, but its ignition ability is poor, and it needs to be added with an ignition charge for use. The ignition capability of the carbon material can be improved by the nanoscale carbon material and the heat-conducting carbon material, so that the performance of the lead azide can be modified by adding the nanoscale carbon material, and the lead azide can meet the requirement of a micro-detonation system. Copper azide and silver azide, which are azides, also have the same problem, and modification studies are required. For example, yanli et al prepared a carbon-based copper azide composite with a copper-containing organic framework material and a copper-containing gel as precursors, and both achieved a certain desensitizing effect due to the presence of the high-molecular carbonized activated carbon material and the uniform distribution of copper azide in the porous framework. However, graphene is a more desirable framework material than a specific carbon material because of its excellent properties such as excellent conductivity, large specific surface area, and the like. In addition, with the development of nano materials, the nanoscale initiating explosive attracts researchers' attention due to its excellent properties such as high specific surface area, many active sites, and fast energy release rate. Therefore, the design of the modified initiating explosive which is uniformly distributed in the foam graphene and used for synthesizing the nanoscale metal azide initiating explosive has important significance for promoting the development of a micro initiating system.
The invention aims to provide a nanoscale azide composite material uniformly dispersed in a foamed graphene framework, which is prepared by taking soluble metal salt, nano metal or metal oxide as a raw material and graphene oxide as a conductive additive through high-temperature hydrothermal reaction, freeze drying and in-situ azidation.
Disclosure of Invention
The invention aims to provide a method for preparing a foam graphene-based metal azide composite by taking soluble metal salt, nano metal or nano metal oxide as a precursor material and graphene oxide as a conductive additive through steps of high-temperature hydrothermal reaction, freeze drying, in-situ reaction and the like. The raw materials with different nano-scales can regulate and control the particle size of azide particles, and the conductive material graphene also reduces the electrostatic sensitivity of azide and improves the safety performance of the azide.
The technical scheme of the invention is as follows:
the invention provides a preparation method of a foam graphene-based metal azide compound, which 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, carrying out ultrasonic treatment for 30min, and cooling for 1 h; repeating the ultrasonic and cooling processes for 3 times;
adding soluble metal salt, nano metal or nano metal oxide, performing ultrasonic treatment and fully stirring for 2 hours, placing the stirred solution in a hydrothermal reaction kettle, and performing hydrothermal reaction for 12 hours in a constant-temperature drying oven at 180 ℃ to obtain composite gel; 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%;
thirdly, placing the composite gel obtained in the second step in liquid nitrogen for freeze drying to obtain a dried product, and then heating the dried product under an anaerobic condition, wherein the reaction temperature is controlled to be 300-1000 ℃, the protective air flow rate is controlled to be 10-30 m L/min, and the reaction time is 10-60 min, so as 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 foam graphene-based metal azide 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 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 graphene oxide is 20 wt%.
In a preferred embodiment, the anaerobic condition comprises introducing an inert gas, a reducing gas or a nitrogen gas.
In another aspect, the present invention provides a foam graphene-based metal azide composite, which is characterized in that: the foam graphene-based metal azide composite is prepared by any one of the preparation methods of the foam graphene-based metal azide composite.
In a preferred embodiment, the foam graphene-based metal azide composite includes a foam graphene-based copper azide composite, a foam graphene-based lead azide composite, and a foam graphene-based silver azide composite.
The invention also provides a foam graphene-based metal azide compound, which is characterized in that the foam graphene-based metal azide compound 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 powder or nano metal oxide as a precursor material, carrying out high-temperature hydrothermal reaction on graphene oxide to form graphene gel, and freeze-drying to form the porous precursor material with large surface area. By controlling the time of the in-situ azide reaction, the foam graphene-based metal azide compound (shown in figure 1) is prepared. The invention provides a compound taking foam graphene as a framework and loading nano azide and a preparation method thereof.
The invention has the following beneficial effects:
the foam graphene-based azide compound can regulate and control the size of azide particles according to the particle size of the nano metal of the raw material; due to the addition of the graphene conductive material, the foam graphene-based azide composite is lower in electrostatic sensitivity and higher in safety. The foam graphene-based azide compound is an azide modified variety.
Drawings
FIG. 1 is an SEM image of a foam graphene-based azide composite prepared by the method.
Detailed Description
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1: raw materials: cupric acetate [ (CH)3COO)2Cu·H2O]Sodium azide (NaN)3) Graphene Oxide (GO), 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 constant-temperature drying box, a hydrothermal reaction kettle, 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 0.24g copper acetate into a standby solution A, performing ultrasonic treatment and fully stirring for 2h until the solution is uniformly dispersed, placing the uniformly dispersed solution in a hydrothermal reaction kettle, performing hydrothermal reaction for 12h in a constant-temperature drying oven at 180 ℃, filtering and washing to obtain a copper acetate and graphene compound, placing the compound in liquid nitrogen, performing freeze drying on the frozen solid to obtain foamed graphene/copper acetate standby A, performing high-temperature thermal decomposition on a dried cylindrical sample under an anaerobic condition, controlling the reaction temperature at 600 ℃, controlling the protective gas flow rate at 10m L/min, controlling the reaction time at 30min, placing a carbonized product in a ventilation device through which gas generated by co-heat of sodium azide and stearic acid passes to obtain a copper azide @ graphene finished product, wherein the raw material ratio of the azide gas generation device (molar ratio) is (mol ratio)Er) is NaN3:CH3(CH2)16COOH is 1:1, the reaction temperature is 120 ℃, and the reaction time is 36 h.
Example 2: raw materials: copper nanopowder (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 constant-temperature drying box, a hydrothermal reaction kettle, a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
Measuring 13m L water, adding 60mg graphene oxide, performing ultrasonic treatment for 1h, weighing 0.4g of nano copper powder, adding 2m L water, performing ultrasonic stirring for 30min, slowly dropping graphene oxide solution into nano copper dispersion liquid under stirring, sufficiently stirring to uniformly disperse the graphene oxide solution, placing the uniformly dispersed solution into a hydrothermal reaction kettle, performing hydrothermal reaction for 12h in a constant-temperature drying oven at 180 ℃, obtaining compound gel of graphene oxide, copper and oxides thereof, placing the compound into liquid nitrogen, performing freeze drying on the frozen solid to obtain cylindrical foam graphene/copper and oxides thereof for later use, heating a dried cylindrical sample under anaerobic condition, controlling reaction temperature at 600 ℃, controlling protective gas flow at 10m L/min, controlling reaction time at 30min, completely converting cuprous oxide into copper, placing the heated product into a ventilation device through which gas containing sodium azide and stearic acid co-generates heat, and obtaining a copper azide graphene finished product, wherein the raw material ratio (molar) of an acid 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: 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 constant-temperature drying box, a hydrothermal reaction kettle, a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
13m of L mg of water are metered in, and 40mg of oxidizing agent are addedThe method comprises the steps of carrying out ultrasonic treatment on graphene for 1h, weighing 0.4g of nano lead oxide, adding the nano lead oxide into 2m L of water, carrying out ultrasonic stirring for 30min, slowly dropping a graphene oxide solution into a stirred nano lead oxide dispersion liquid, fully stirring to uniformly disperse the solution, placing the uniformly dispersed solution into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 12h in a constant-temperature drying box at 180 ℃, obtaining a compound gel of graphene oxide, lead oxide and oxides thereof, placing the compound into liquid nitrogen, carrying out freeze drying on the frozen solid to obtain cylindrical foamed graphene/lead oxide for later use, placing the foamed graphene/lead oxide into a ventilation device through which gas generated by sodium azide and stearic acid in a common heat passes, obtaining a lead azide @ graphene finished product, wherein the raw material feeding ratio (mol) of an acid gas generating 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: 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 constant-temperature drying box, a hydrothermal reaction kettle, 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 0.24g lead acetate into a standby solution A, performing ultrasonic treatment and fully stirring for 2h until the solution is uniformly dispersed, placing the uniformly dispersed solution in a hydrothermal reaction kettle, performing hydrothermal reaction for 12h in a constant-temperature drying oven at 180 ℃, filtering and washing to obtain a lead acetate and graphene compound, placing the compound in liquid nitrogen, performing freeze drying on the frozen solid to obtain foamed graphene/lead acetate standby solution A, performing high-temperature thermal decomposition on the dried cylindrical sample under the anaerobic condition, controlling the reaction temperature at 600 ℃, controlling the protective gas flow rate at 10m L/min, controlling the reaction time at 30min, placing the carbonized product in a ventilation device through which gas generated by the co-heat of sodium azide and stearic acid passes to obtain a lead azide @ graphene finished product, wherein the raw material ratio (mol) of an azide acid 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: nano silver oxide (Ag)2O), 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 constant-temperature drying box, a hydrothermal reaction kettle, a freeze dryer, a tube furnace, a round-bottom flask and a water bath kettle.
Measuring 13m L water, adding 60mg graphene oxide, performing ultrasonic treatment for 1h, weighing 0.4g nano silver oxide, adding 2m L water, performing ultrasonic stirring for 30min, slowly dropping a graphene oxide solution into a stirred nano silver oxide dispersion liquid, sufficiently stirring to uniformly disperse the solution, placing the uniformly dispersed solution into a hydrothermal reaction kettle, performing hydrothermal reaction for 12h in a constant-temperature drying box at 180 ℃, obtaining a composite gel of graphene oxide, silver oxide and an oxide thereof, placing the composite in liquid nitrogen, performing freeze drying on a frozen solid to obtain cylindrical foamed graphene/silver oxide for later use, placing the foamed graphene/silver oxide into a ventilation device through which gas generated by co-heat of sodium azide and stearic acid passes to obtain a finished product of silver azide graphene, wherein the raw material 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.
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 foam graphene-based metal azide 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, carrying out ultrasonic treatment for 30min, and cooling for 1 h; repeating the ultrasonic and cooling processes for 3 times;
adding soluble metal salt, nano metal or nano metal oxide, performing ultrasonic treatment and fully stirring for 2 hours, placing the stirred solution in a hydrothermal reaction kettle, and performing hydrothermal reaction for 12 hours in a constant-temperature drying oven at 180 ℃ to obtain composite gel; 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%;
thirdly, placing the composite gel obtained in the second step in liquid nitrogen for freeze drying to obtain a dried product, and then heating the dried product under an anaerobic condition, wherein the reaction temperature is controlled to be 300-1000 ℃, the protective air flow rate is controlled to be 10-30 m L/min, and the reaction time is 10-60 min, so as 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 foam graphene-based metal azide composite.
2. The method of preparing a foam graphene-based metal azide composite according to claim 1, wherein: the soluble metal salt comprises copper nitrate, copper acetate, lead nitrate, lead acetate and silver nitrate.
3. The method of preparing a foam graphene-based metal azide composite according to claim 1, wherein: the nano metal powder comprises nano copper powder, nano lead powder and nano silver powder.
4. The method of preparing a foam graphene-based metal azide composite 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 foam graphene-based metal azide composite according to claim 1, wherein: the content of the graphene oxide is 5 wt% -15 wt%.
6. The method of preparing a foam graphene-based metal azide composite according to claim 1, wherein: the content of the graphene oxide is 15 wt% -30 wt%.
7. The method of preparing a foam graphene-based metal azide composite according to claim 1, wherein: the anaerobic condition comprises the introduction of inert gas, reducing gas or nitrogen.
8. A foam graphene-based metal azide composite, characterized by: the foam graphene-based metal azide composite is prepared by the preparation method of the foam graphene-based metal azide composite according to any one of claims 1 to 7.
9. The foam graphene-based metal azide composite according to claim 8, wherein: the foam graphene-based metal azide compound comprises a foam graphene-based copper azide compound, a foam graphene-based lead azide compound and a foam graphene-based silver azide compound.
10. Use of the foam graphene-based metal azide composite according to claim 8 or 9 as an initiator.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| CN117613250A (en) * | 2024-01-24 | 2024-02-27 | 帕瓦(长沙)新能源科技有限公司 | Three-dimensional conductive lead-carbon composite material, preparation method thereof, negative electrode and lead-acid battery |
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| 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 |
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