CN103864034A - Method and device for synthesizing copper azide - Google Patents
Method and device for synthesizing copper azide Download PDFInfo
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- CN103864034A CN103864034A CN201410095705.6A CN201410095705A CN103864034A CN 103864034 A CN103864034 A CN 103864034A CN 201410095705 A CN201410095705 A CN 201410095705A CN 103864034 A CN103864034 A CN 103864034A
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Abstract
The invention discloses a method and a device for synthesizing copper azide, in order to solve the problem of high danger in synthesis of copper azide and provide a new technology and a new technique for preparation of a novel green initiating explosive. A reaction device comprises an azoimide generation device, an azidation device and a tail gas absorption device. The method and the device for synthesizing the copper azide initiating explosive have the following remarkable advantages: (1) since explosion happens very easily once azoimide gas is in contact with grease, water and the like, and the whole device is all formed by means of connecting glassware through ground openings without rubber tubes and grease type substances such as vaseline, the safety of reaction is guaranteed fundamentally; (2) the azoimide gas is fed in from the lower part and discharged out from the upper part, thereby fully reacting with porous copper; (3) an anti-explosion ball is smart is structure design and samples can be conveniently placed in and taken out; (4) the gas absorption device with an anti-back-suction ball is capable of effectively preventing the azoimide gas from escaping.
Description
Technical field
The present invention relates to a kind of synthetic method of green priming explosive, be specifically related to a kind of method for the synthesis of copper azide and device.
Background technology
Now widely used priming explosive key ingredient is leaded sensitive compound, such as lead azoimide, lead styphnate etc., and they are harmful and affect HUMAN HEALTH on environment.Cu is very little to the harm of environment, meets the requirement of environment protection with conventional leaded medicament in copper replacement priming system.But, because the mechanical sensitivity of copper azide is more taller than lead azoimide, almost one touch fried, dangerous large in preparation, use procedure, limited its research and application.How both having utilized the friendly feature of copper and environment, and can take into account again Loading Materials for Initiating Explosive Devices security requirement, is a problem demanding prompt solution.
(the By Valarie Pelletier such as By Valarie Pelletier, Sayan Bhattacharyya, Isabel Knoke, Farhad Forohar, Magdy Bichay, and Yury Gogotsi.Copper Azide Confined Inside Templated Carbon Nanotubes[J]. Adv. Funct. Mater, 2010,20:3168 – 3174.) in carbon nanotube, prepare copper azide nanoparticle, because the good conductivity of carbon nanotube, so improve the security of preparation process.(the Fang Zhang such as Fang Zhang, Yanlan Wang, Yingwei Bai, Rui Zhang.Preparation and characterization of copper azide nanowire array[J]. Materials Letters, 89 (2012) 176 – 179.) utilize alumina formwork legal system for NANO CRYSTAL COPPER WIRE, then prepared copper azide nano wire through azide.In above-mentioned research, all adopt the azido reaction of hydrazoic acid gas and Nanometer Copper or copper oxide particle, because hydrazoic acid gas is poisonous, formed metal azide with the metal vigorous reaction such as copper, iron, nickel, and contact and can blast with the material such as water, grease.In bibliographical information few in number, also there is no corresponding compound experiment device, therefore, the synthesizer that design safety is high is the key of azide process.
Summary of the invention
The object of the present invention is to provide a kind of method for the synthesis of copper azide and device, dangerous high problem while synthesizing to solving copper azide, for the preparation of novel green priming explosive provides novel process and new technology.
Realizing technical scheme of the present invention is:
A kind of device for the synthesis of copper azide, described device comprises hydrazoic acid generating unit, azide device and device for absorbing tail gas, described hydrazoic acid generating unit comprises heat-collecting magnetic stirring device, reactor, square elbow, drying tube, " S " type glass bend pipe and nitrogen gas generating device, described azide device comprises explosion-proof ball, , described nitrogen gas generating device, reactor, square elbow, drying tube, " S " type glass bend pipe, explosion-proof ball, described explosion-proof ball is the globosity of both ends open, there is respectively Link Port top and bottom, upper interface diameter is larger, be convenient to placement and the taking-up of sample, lower interface diameter is less, and an inner segment distance is stretched in explosion-proof ball bottom, this structure can be placed on copper sheet between intermediate glass post and explosion-proof ball, play the effect of fixing copper sheet.Described nitrogen gas generating device, reactor, square elbow, drying tube, " S " type glass bend pipe, explosion-proof ball, device for absorbing tail gas are connected successively, and described reactor is fixed in heat-collecting magnetic stirring device.
Wherein, described heat-collecting magnetic stirring utensil has temperature regulator and oil bath pan function, and reactor is there-necked flask, and thermometer is connected to there-necked flask by a ground glass stopper.
Described explosion-proof ball is the globosity of both ends open, there is respectively Link Port top and bottom, upper interface diameter is larger, be convenient to placement and the taking-up of sample, lower interface diameter is less, and explosion-proof ball bottom joint stretches into an inner segment distance, stretch into inner Glass tubing tube wall place and have aperture, this structure can prevent that sample bottom air-flow is excessive, and sample is placed unstable problem, makes the abundant contact reacts of sample and gas simultaneously.
Described nitrogen gas generating device is nitrogengas cylinder.
Described reactor, square elbow, drying tube, " S " type glass bend pipe, explosion-proof ball, anti-suck ball, beaker all adopt glass material, and the sealing between interface is all designed to glass ground joint and connects sealing.
Said apparatus is used for synthesizing copper azide, and concrete steps are as follows:
(1) in three-necked flask, add sodiumazide and stearic acid, in drying tube, add siccative, then in explosion-proof ball, add the previously prepared good Porous Cu sample with micro-nano structure, prepare alkaline solution and pour in beaker, connect whole device;
(2) open nitrogengas cylinder air valve and pass into nitrogen with speed slowly, discharge the inner air of whole device and foreign gas, and the resistance to air loss of verifying attachment;
(3) temperature reaction, produces HN in reaction process
3, after isothermal reaction for some time, close nitrogen valve, make the HN producing
3fully react with Porous Cu;
(4) reaction is opened nitrogen valve after finishing again, slowly passes into nitrogen flooding except residue HN
3make the alkali lye in beaker fully absorb, sell quick-fried, open ventilation installation, decompression is taken out copper azide sample after ventilating from explosion-proof ball;
(5) residual solid in three-necked flask is first processed with chlorine bleach liquor, the liquid and waste slag produced individual curing of doing.
Wherein, in step (1), sodiumazide and stearic mass ratio are 1:5.5, Porous Cu quality 10mg.
In step (3), temperature reaction temperature keeps 130 ~ 140 DEG C.Above-mentioned reaction all should be carried out under stink cupboard and safeguard procedures.
The present invention compared with prior art its remarkable advantage is: described reaction unit is made up of hydrazoic acid gas generating unit, azido reaction container, device for absorbing tail gas and pipe connecting.Adopt the synthetic copper azide priming explosive of the present invention to have following remarkable advantage: (1) reaction safety is high.Whole reaction unit is glass material, and is in airtight system; (2) hydrazoic acid gas adopts the form of bottom in and top out, can make hydrazoic acid fully react with Porous Cu; (3) explosion-proof ball structure design is ingenious, and sample is placed with taking-up easy to operate; (4) can effectively prevent hydrazoic acid effusion with the device for absorbing tail gas of anti-suck ball.
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Brief description of the drawings
The experimental installation structural representation of the synthetic copper azide of Fig. 1 the present invention.
The structural representation of explosion-proof ball in Fig. 2 apparatus of the present invention (a-front view, b-side-view, c-vertical view).
The XRD phenogram of Fig. 3 the present invention Porous Cu used.
The XRD phenogram of the synthetic copper azide of Fig. 4 the present invention.
Embodiment
The following examples can make the present invention of those skilled in the art comprehend.
A kind of for the synthetic method of copper azide and device, as shown in Figure 1, described reaction unit comprises heat-collecting magnetic stirring device 1, three-necked flask 2, thermometer 3, square elbow 4, drying tube 5, " S " type glass bend pipe 6, explosion-proof ball 7, anti-suck ball 8, beaker 9 and nitrogengas cylinder 10.Described heat-collecting magnetic stirring device 1 has temperature and regulates and control function, simultaneously with oil bath pan; Described thermometer 3 is connected to three-necked flask 2 by a ground glass stopper; In described drying tube 5, siccative is housed; As shown in Figure 2, there is respectively Link Port described explosion-proof ball 7 top and bottom, upper interface 71 diameters are larger, the placement of the sample of being convenient to and taking-up, certain distance in explosion-proof ball is stretched in lower interface 72 one end, the Glass tubing tube wall place that stretches into explosion-proof ball inside has aperture 73, is convenient to the stable placement of sample and hydrazoic acid gas is fully reacted with Porous Cu; In described beaker 9, fill alkaline solution, reclaim unnecessary hydrazoic acid gas; In described reaction unit, all containers and pipe connecting all adopt glass material, and the sealing between interface can not be used grease, are all designed to glass ground joint and connect sealing; Described reaction need be carried out under protection at stink cupboard with effectively.
For the synthetic method of copper azide and a device, described reaction unit comprises heat-collecting magnetic stirring device 1, three-necked flask 2, thermometer (3), square elbow 4, drying tube 5, " S " type glass bend pipe 6, explosion-proof ball 7, anti-suck ball 8, beaker 9 and nitrogengas cylinder 10.In described heat-collecting magnetic stirring device 1 oil bath pan, adopt organic silicone oil; In described drying tube 5, Calcium Chloride Powder Anhydrous siccative is housed; In described beaker 9, fill KOH solution, reclaim unnecessary hydrazoic acid gas; Described reaction need be carried out under protection at stink cupboard with effectively.Copper azide building-up process of the present invention is:
(1) 250mL three-necked round bottom flask is fixed in oil bath pan with iron stand, in oil bath pan, adds the organic silicone oil of 2/3rds volumes, in three-necked flask, add rotor, sodiumazide (0.5g) and stearic acid (2.75g), in drying tube, add Calcium Chloride Powder Anhydrous and stop up two ends with cotton, then in 100mL explosion-proof ball, add the Porous Cu sample 10mg anticipating, (preparation of described Porous Cu is according to document " Hebing Zhang, Yinghua Ye, Ruiqi Shen, Chengbo Ru, and Yan. HuEffect of Bubble Behavior on the Morphology of Foamed PorousCopper Prepared via Electrodeposition[J]. Journal of the Electrochemical Society, 2013, prepared by the method for 160 (10): D441-D445. " reporting), 1.0gKOH is made into 300ml solution to be poured in 500mL beaker, for absorption reaction residual gas, anti-suck ball (100mL) connects by diagram, whole device is placed in stink cupboard,
(2) open heat-collecting magnetic stirring device, make oil bath pan be warming up to 130-140 DEG C, now starting has HN
3gas generates, and detects the stopping property between each interface with moistening litmus paper, and whether observation litmus paper color changes, if change, stop immediately heating and slowly blow out residual air with nitrogen, again checking resistance to air loss, just can carry out next step experiment until meet the requirements.As litmus paper color does not change, use nitrogen gas stream very slowly to import explosion-proof ball via drying tube from the lower interface of explosion-proof ball;
(3) under 130-140 DEG C of condition, through reaction in two hours, close nitrogen valve, stop nitrogen gas stream and pass into, make the HN producing
3in explosion-proof ball, fully react with Porous Cu;
(4) continue heated and stirred after 5 hours, stop oil bath heating, then make its reaction keep at normal temperatures i.e. reaction after 19 hours to finish;
(5) again open nitrogen valve, slowly pass into residual gas in nitrogen blowing out device, be transported in the beaker that fills KOH solution remaining HN through the upper interface of the explosion-proof ball drying tube of flowing through
3gas and KOH solution reaction, anti-suck ball can prevent the solution suck-back in beaker;
(6) open ventilation installation, after decompression is ventilated, remove experimental installation, take out compound good copper azide sample in explosion-proof ball, wherein cuprous containing a small amount of azide;
(7) residual solid in three-necked flask is first processed with chlorine bleach liquor, the liquid and waste slag produced individual curing of doing.
Fig. 3 is the XRD diffractogram spectrogram of prepared Porous Cu, and known, main component is copper, has the oxidized Red copper oxide that formed of a small amount of copper in the process of preparing Porous Cu.
Fig. 4 is the XRD diffracting spectrum of the copper azide that obtains of embodiment, known, has generated copper azide target product, also has a small amount of azide cuprous, and copper peak is the diffraction peak of base material.
Claims (9)
1. the device for the synthesis of copper azide, it is characterized in that, described device comprises hydrazoic acid generating unit, azide device and device for absorbing tail gas, described hydrazoic acid generating unit comprises heat-collecting magnetic stirring device (1), reactor (2), square elbow (4), drying tube (5), " S " type glass bend pipe (6) and nitrogen gas generating device (10), described azide device comprises explosion-proof ball (7), the globosity that described explosion-proof ball (7) is both ends open, there is respectively Link Port top and bottom, described nitrogen gas generating device (10), reactor (2), square elbow (4), drying tube (5), " S " type glass bend pipe (6), explosion-proof ball (7), device for absorbing tail gas is connected successively, described reactor (2) is fixed in heat-collecting magnetic stirring device (1).
2. reaction unit according to claim 1, is characterized in that: described reactor (2) is that there-necked flask, one of them ground of there-necked flask connect thermometer (3) by glass stopper.
3. reaction unit according to claim 1, is characterized in that: described tail gas collecting device comprises beaker (9) and is placed on the suck-back ball (8) in beaker (9).
4. reaction unit according to claim 1, it is characterized in that: the globosity that described explosion-proof ball (7) is both ends open, there is respectively Link Port top and bottom, upper interface (71) diameter is larger, be convenient to placement and the taking-up of sample, lower interface (72) diameter is less, and explosion-proof ball bottom stretches into an inner segment distance, and the Glass tubing tube wall place that stretches into explosion-proof ball inside has aperture (73).
5. reaction unit according to claim 1, is characterized in that: nitrogen gas generating device (10) is nitrogengas cylinder.
6. reaction unit according to claim 3, it is characterized in that: described reactor (2), square elbow (4), drying tube (5), " S " type glass bend pipe (6), explosion-proof ball (7), anti-suck ball (8), beaker (9) all adopt glass material, the sealing between interface is glass ground joint and connects sealing.
7. for the synthesis of a method for copper azide, it is characterized in that concrete steps are as follows:
(1) in reactor, add sodiumazide and stearic acid, in drying tube, add siccative, then in explosion-proof ball, add the previously prepared good Porous Cu with micro-nano structure, preparing alkaline solution pours in beaker, connect whole device, described device comprises hydrazoic acid generating unit, azide device and device for absorbing tail gas, described hydrazoic acid generating unit comprises heat-collecting magnetic stirring device (1), reactor (2), square elbow (4), drying tube (5), " S " type glass bend pipe (6) and nitrogen gas generating device (10), described azide device comprises explosion-proof ball (7), the globosity that described explosion-proof ball (7) is both ends open, there is respectively Link Port top and bottom, described nitrogen gas generating device (10), reactor (2), square elbow (4), drying tube (5), " S " type glass bend pipe (6), explosion-proof ball (7), device for absorbing tail gas is connected successively, described reactor (2) is fixed in heat-collecting magnetic stirring device (1),
(2) open nitrogen gas generating device and pass into nitrogen with speed slowly, discharge the inner air of whole device and foreign gas, and the resistance to air loss of verifying attachment;
(3) temperature reaction, produces HN in reaction process
3, after isothermal reaction for some time, close nitrogen valve, make the HN producing
3fully react with Porous Cu;
(4) reaction is opened nitrogen valve after finishing again, slowly passes into nitrogen flooding except residue HN
3make the alkali lye in beaker fully absorb, sell quick-fried, open ventilation installation, decompression is taken out copper azide sample after ventilating from explosion-proof ball;
(5) residual solid in three-necked flask is first processed with chlorine bleach liquor, the liquid and waste slag produced individual curing of doing.
8. method according to claim 7, is characterized in that: in step (1), sodiumazide and stearic mass ratio are 1:5.5, Porous Cu quality 10mg.
9. method according to claim 7, is characterized in that: in step (3), temperature reaction temperature keeps 130 ~ 140 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837515A (en) * | 2017-11-29 | 2019-06-04 | 南京理工大学 | Nano combined film containing energy and preparation method thereof |
| CN110040701A (en) * | 2019-05-22 | 2019-07-23 | 北京理工大学 | A kind of preparation method for the high desnity metal azide that loading density arbitrarily regulates and controls |
| CN110078033A (en) * | 2019-05-22 | 2019-08-02 | 北京理工大学 | A kind of preparation method of the high-density copper azide with constraint shell |
| CN110857215A (en) * | 2018-08-22 | 2020-03-03 | 南京理工大学 | Method for preparing low-sensitivity copper azide from composite CNTs and copper nanowires |
| CN110857214A (en) * | 2018-08-22 | 2020-03-03 | 南京理工大学 | Method for preparing low-sensitivity copper azide by compounding rGO and copper nanowire |
| CN111153757A (en) * | 2020-01-06 | 2020-05-15 | 郑州大学 | High-performance copper azide composite primary explosive and preparation method thereof |
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| CN1156122A (en) * | 1996-11-25 | 1997-08-06 | 袁必疆 | Process for producing barium azide |
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Non-Patent Citations (2)
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837515A (en) * | 2017-11-29 | 2019-06-04 | 南京理工大学 | Nano combined film containing energy and preparation method thereof |
| CN109837515B (en) * | 2017-11-29 | 2021-05-04 | 南京理工大学 | Nano composite energetic film and preparation method thereof |
| CN110857215A (en) * | 2018-08-22 | 2020-03-03 | 南京理工大学 | Method for preparing low-sensitivity copper azide from composite CNTs and copper nanowires |
| CN110857214A (en) * | 2018-08-22 | 2020-03-03 | 南京理工大学 | Method for preparing low-sensitivity copper azide by compounding rGO and copper nanowire |
| CN110857215B (en) * | 2018-08-22 | 2023-08-18 | 南京理工大学 | Method for preparing low-sensitivity copper azide by compounding CNTs and copper nanowires |
| CN110857214B (en) * | 2018-08-22 | 2023-08-22 | 南京理工大学 | Method for preparing low-sensitivity copper azide by compounding rGO and copper nanowire |
| CN110040701A (en) * | 2019-05-22 | 2019-07-23 | 北京理工大学 | A kind of preparation method for the high desnity metal azide that loading density arbitrarily regulates and controls |
| CN110078033A (en) * | 2019-05-22 | 2019-08-02 | 北京理工大学 | A kind of preparation method of the high-density copper azide with constraint shell |
| CN111153757A (en) * | 2020-01-06 | 2020-05-15 | 郑州大学 | High-performance copper azide composite primary explosive and preparation method thereof |
| CN111153757B (en) * | 2020-01-06 | 2021-09-21 | 郑州大学 | High-performance copper azide composite primary explosive and preparation method thereof |
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Application publication date: 20140618 |