CN106586968A - Safe extracting method of ammonium perchlorate in solid FAE (Fuel Air Explosive) - Google Patents
Safe extracting method of ammonium perchlorate in solid FAE (Fuel Air Explosive) Download PDFInfo
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- CN106586968A CN106586968A CN201611045345.4A CN201611045345A CN106586968A CN 106586968 A CN106586968 A CN 106586968A CN 201611045345 A CN201611045345 A CN 201611045345A CN 106586968 A CN106586968 A CN 106586968A
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- Prior art keywords
- ammonium perchlorate
- solid
- extracting method
- cloud detonator
- surfactant
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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
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/16—Perchloric acid
- C01B11/18—Perchlorates
- C01B11/185—Ammonium perchlorate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to the technical field of safe treatment of solid energetic materials, and particularly discloses an extracting method of ammonium perchlorate in solid FAE (Fuel Air Explosive). The extracting method comprises the following steps: uniformly mixing a powdery solid FAE containing the ammonium perchlorate with a certain amount of water and surfactant, wherein the dosage of the surfactant is 1 to 4 percent of the weight of the solid FAE; carrying out ultrasonic extraction on mixed liquid by using an ultrasonic extraction device under room temperature, wherein the ammonium perchlorate is extracted into a water solution, and the surfactant is a brominated quaternary ammonium cationic surfactant. According to the extracting method disclosed by the invention, the ammonium perchlorate in the solid FAE can be recycled under normal temperature, the extracting time is remarkably shortened, the extracting efficiency is remarkably increased, a higher extracting rate is obtained, the operation is safe, and control and implementation are easy.
Description
Technical field
The present invention relates to the secure processing techniques field of solid energetic material.
Background technology
Ammonium perchlorate is a kind of conventional oxidant, is had a wide range of applications in numerous energetic materials, in national defense industry
For producing the explosive wastewaters such as propellant, agent, hail suppression agent etc. are engraved in civilian production.Ammonium perchlorate property is active, with reducing agent, inflammable
The mixing such as thing and metal dust can explode.
Solid cloud detonator is a kind of high explosive rich in fuel, and solid cloud detonator is to be directed to liquid-solid composite cloud detonator not
Develop enough, liquid solid-state cloud detonator has certain mobility, and density contrast is larger between each component, in filling in body, in fortune
Easily there is centroid motion during defeated and storage, affect path accuracy and explosion property stable.Solid cloud detonator is with solid-state
Confection is filled in warhead, defines the biphase fuel-air explosive of solid phase, gas phase, its mechanism of action and explosion property
Keep constant, but precision and stability is improved, and is easy to produce, transports, stores, and is following widely used primary armament
One of.
Solid cloud detonator is mainly made up of oxidant, fuel agent, sensitizer, deterrent etc..Ammonium perchlorate（AP）It is solid
The oxidant commonly used in cloud detonator, proportion is 5～15%.Fuel agent is again reducing agent in solid cloud detonator, common metal
Powder, such as aluminium powder.Sensitizer is added to be, in order to adjust the sensitivity of mixture, to make it smoothly detonation in solid cloud detonator, and
And make detonation property stable etc..Oxidant, fuel agent, sensitizer etc. are coated by deterrent in solid cloud detonator, quick-fried to reduce cloud
The mechanical sensitivity of agent, improves stability.
The storage of solid cloud detonator is expired, needs to carry out safe and environment-friendly recycling.Ammonium perchlorate is soluble in water, can be with
Water dissolution recovery is carried out to it.Ammonium perchlorate is due to by the cladding such as deterrent paraffin, HTPB in solid cloud detonator, it is not easy to by water
Directly dissolve.
Prior art have using boiled process to reclaim solid energetic material in ammonium perchlorate, final extraction ratio is 85%
Between～90%, but its water temperature is higher, requires heat to 80 DEG C or so, for solid cloud detonator, processing safety compared with
Differ from, and the method extraction time generally needs more than a few hours, extraction efficiency is low.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of safe extracting method of ammonium perchlorate in solid cloud detonator, adopts
Water dissolution is carried out to solid cloud detonator with cavitation-cationic surfactant, can be reclaimed in solid cloud detonator in lower temperature
Ammonium perchlorate, extraction time substantially shortens, and extraction efficiency is significantly improved, with higher extraction ratio, safe operation, it is easy to control
And enforcement.
To solve above-mentioned technical problem, the technical solution used in the present invention is：
The safe extracting method of ammonium perchlorate in a kind of solid cloud detonator, including
S1, will mix homogeneously with a certain amount of water, surfactant containing the pulverulent solids cloud detonator of ammonium perchlorate, wherein described
The consumption of surfactant is the 1%～4% of the solid cloud detonator weight；
S2, supersound extraction is carried out to the mixed liquor with ultrosonic extractor, ammonium perchlorate is extracted in aqueous solution；
The surfactant is quaternary ammonium bromide cationic surfactants.
Quaternary cationicses, are by ammonium cation [NH4+] four hydrogen atoms entirely by organic group replace and
Into a kind of cationic surface active agent, formula is as follows：
There is 1-3 to be Long carbon chain in its 4 alkyl, remaining carbon number is 1-2.Quaternary ammonium bromide cationic surfactants
X is Br in the formula.
The preferred tetrabutyl ammonium bromide of surfactant described in the inventive method or cetyl trimethylammonium bromide.
Used as the preferred embodiment of the technical program, in the S1, solid cloud detonator is 1 with the mass ratio of water:2～4.
Further, it is to obtain preferable extraction ratio, the supersound extraction time is not less than 20min in S2.
It is further preferred that in the S1, solid cloud detonator is 1 with the mass ratio of water:The supersound extraction time is in 3, S2
35～50min.
In S2 ultrosonic extractor the mixed liquor is carried out supersound extraction power be 300～800W, supersonic frequency
Rate is 28KHz.
Optionally, the S2 carries out supersound extraction in room temperature.
It is using the beneficial effect produced by above-mentioned technical proposal：The inventive method cationic surfactant and super
Sound wave extracts ammonium perchlorate, the mechanical effect having using ultrasound wave, cavitation effect and heat effect, by increasing medium molecule
Movement velocity, the penetration power of increase medium to extract solid cloud detonator in ammonium perchlorate, cause solid especially with cavitation effect
The clad and the rupture of three dimensional network structure to ammonium perchlorate such as deterrent paraffin, HTPB, is effectively increased water in body cloud detonator
Contact with ammonium perchlorate, can realize the ammonium perchlorate in room temperature reclaims solid cloud detonator, and extraction time substantially shortens, by counting
Hour foreshortens to dozens of minutes, and extraction efficiency is significantly improved, while ammonium perchlorate extraction ratio can be improved further up to 98%, grasps
Make safety, it is simple.
Description of the drawings
Fig. 1 is the process chart that ammonium perchlorate is extracted in the inventive method embodiment.
Specific embodiment
Ammonium perchlorate in solve prior art solid cloud detonator（AP）Extraction efficiency is low, Extracting temperature is high, safety is low
Etc. technical problem, the invention discloses in a kind of solid cloud detonator ammonium perchlorate safe extracting method, using cavitation-cation
Surfactant carries out water dissolution to solid cloud detonator, can room temperature reclaim solid cloud detonator in ammonium perchlorate, extraction time
Substantially shorten, extraction efficiency is significantly improved, with higher extraction ratio, safe operation, it is easy to control and enforcement.
Name embodiment 1-21 to be described in further detail the inventive method.
Each embodiment is ultrasonic using the SW-1024S standards single cavity of Qingdao Vista electric purification equipment company limited production
Ripple cleaning machine used as ultrosonic extractor, the bottom of for shake by its working method, and ultrasonic peak power is up to 1200W, supersonic frequency
28KHz。
Solid cloud detonator sample used by each embodiment is certain type solid cloud detonator product, deterrent component include paraffin,
HTPB（End hydroxy butadiene）.
The operating procedure of each embodiment is identical, referring to Fig. 1, specially：A certain amount of solid cloud detonator is weighed as quartz
In grinding alms bowl, count a small amount of distilled water and be ground to uniform fine powder, in being placed in 50ml conical flasks, add Quaternary ammonium bromide sun
During the ultrasonic water bath groove of aforementioned ultrasonic extraction element is put into after ionic surface active agent and distilled water, extract under different time
Solution is filtered, carries out titration test after extraction, calculates ammonium perchlorate extraction ratio.
The content of ammonium perchlorate is tested using formol titration in solution after extraction, is generated after formaldehyde and ammonium perchlorate reaction
H+, with after NaOH solution drop reaction liquid can quantitative Analysis extract the content of ammonium perchlorate, then by solid cloud detonator used
Technical specification calculates the content of ammonium perchlorate in cloud detonator, thus obtains the extraction ratio of ammonium perchlorate.
In each embodiment the control parameter such as dosage of surfactant, extraction time, temperature and extract after solution titration knot
Really and calculate gained ammonium perchlorate extraction ratio see the table below 1-7.Wherein the consumption of surfactant accounts for solid cloud detonator with it
The percent of weight is represented.
Wherein surfactant used by embodiment 1-9 is tetrabutyl ammonium bromide（TBAB）, surface used by embodiment 10-18 is lived
Property agent be cetyl trimethylammonium bromide（CTMAB）, embodiment 1-3,9-12 ultrosonic extractor arrange ultrasonic power be
300W, it is 500W that embodiment 4-6,13-15 ultrosonic extractor arranges ultrasonic power, and embodiment 7-9,16-18 ultrasound wave is carried
It is 800W to take device and arrange ultrasonic power.
Embodiment 19-21 is respectively adopted different solid-liquid ratios, and surfactant adopts CTMAB, remaining detail parameters such as table 7 below.
With the increase of solid-liquid ratio, the extraction ratio of AP is improved.Although aqueous solvent is cheap and easy to get, solvent increase is unfavorable for AP
Crystallization, power consumption increase, too little solvent can then cause dissolving insufficient, and can cause sucking filtration loss increase.Consider efficient energy-saving
Condition, choose 1:3 used as suitable solid-liquid ratio, and AP more can sufficiently be extracted and be conducive to AP to crystallize under the conditions of this.
Contrasted from above example, impact very little of the temperature to extraction ratio, the preferred bromination season for extracting ammonium perchlorate
Ammonium salt cationic surfactant amount ranges are 1%～4%, and extraction time is 30～50min.It is quick-fried solid cloud to be separated by this scheme
Ammonium perchlorate in agent, extraction ratio is up to more than 90%.
The inventive method is described in detail above, using specific case to embodiments of the present invention in the present invention
It is set forth, the explanation of above example is only intended to help and understands the present invention, it is noted that for the skill of the art
For art personnel, under the premise without departing from the principles of the invention, can also some improvement be carried out to the present invention, these improvement also fall into
In the protection domain of the claims in the present invention.
Claims (8)
1. in a kind of solid cloud detonator ammonium perchlorate safe extracting method, it is characterised in that：Including
S1, will mix homogeneously with a certain amount of water, surfactant containing the pulverulent solids cloud detonator of ammonium perchlorate, wherein described
The consumption of surfactant is the 1%～4% of the solid cloud detonator weight；
S2, supersound extraction is carried out to the mixed liquor with ultrosonic extractor, ammonium perchlorate is extracted in aqueous solution；
The surfactant is quaternary ammonium bromide cationic surfactants.
2. in solid cloud detonator according to claim 1 ammonium perchlorate safe extracting method, it is characterised in that the S1
In, solid cloud detonator is 1 with the mass ratio of water:2～4.
3. in solid cloud detonator according to claim 2 ammonium perchlorate safe extracting method, it is characterised in that the S1
In, solid cloud detonator is 1 with the mass ratio of water:3.
4. in the solid cloud detonator according to claim 1 or 3 ammonium perchlorate safe extracting method, it is characterised in that S2
The middle supersound extraction time is not less than 20min.
5. in solid cloud detonator according to claim 4 ammonium perchlorate safe extracting method, it is characterised in that in S2 surpass
Sound extraction time is 35～50min.
6. in solid cloud detonator according to claim 5 ammonium perchlorate safe extracting method, it is characterised in that in S2 surpass
It is 300～800W that sound wave extraction element carries out the power of supersound extraction to the mixed liquor, and supersonic frequency is 28KHz.
7. in solid cloud detonator according to claim 1 ammonium perchlorate safe extracting method, it is characterised in that the table
Face activating agent is tetrabutyl ammonium bromide or cetyl trimethylammonium bromide.
8. in solid cloud detonator according to claim 1 ammonium perchlorate safe extracting method, it is characterised in that the S2
Supersound extraction is carried out in room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611045345.4A CN106586968A (en) | 2016-11-24 | 2016-11-24 | Safe extracting method of ammonium perchlorate in solid FAE (Fuel Air Explosive) |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611045345.4A CN106586968A (en) | 2016-11-24 | 2016-11-24 | Safe extracting method of ammonium perchlorate in solid FAE (Fuel Air Explosive) |
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| CN106586968A true CN106586968A (en) | 2017-04-26 |
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| CN201611045345.4A Pending CN106586968A (en) | 2016-11-24 | 2016-11-24 | Safe extracting method of ammonium perchlorate in solid FAE (Fuel Air Explosive) |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558588A (en) * | 2018-05-25 | 2018-09-21 | 中国人民解放军63908部队 | Application and method of the dodecyl pyridinium chloride in the separation of solid-liquid cloud detonator component |
| CN108727198A (en) * | 2018-05-25 | 2018-11-02 | 中国人民解放军63908部队 | Application and method of the cetyl trimethylammonium bromide in the separation of solid-liquid cloud detonator component |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4198209A (en) * | 1978-09-29 | 1980-04-15 | Mcintosh Meldon J | Process for the leaching of AP from propellant |
| US6063960A (en) * | 1997-12-15 | 2000-05-16 | Tpl, Inc. | Recovering nitroamines and reformulation of by-products |
| CN102359899A (en) * | 2011-06-20 | 2012-02-22 | 西安近代化学研究所 | Pretreatment method of polymer bonded explosive sample |
| US20120227877A1 (en) * | 2009-10-07 | 2012-09-13 | G.D.O., Inc | Demilitarization of wax desensitized explosive projectiles |
-
2016
- 2016-11-24 CN CN201611045345.4A patent/CN106586968A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4198209A (en) * | 1978-09-29 | 1980-04-15 | Mcintosh Meldon J | Process for the leaching of AP from propellant |
| US6063960A (en) * | 1997-12-15 | 2000-05-16 | Tpl, Inc. | Recovering nitroamines and reformulation of by-products |
| US20120227877A1 (en) * | 2009-10-07 | 2012-09-13 | G.D.O., Inc | Demilitarization of wax desensitized explosive projectiles |
| CN102359899A (en) * | 2011-06-20 | 2012-02-22 | 西安近代化学研究所 | Pretreatment method of polymer bonded explosive sample |
Non-Patent Citations (1)
| Title |
|---|
| T.F SHI ET AL.: "Research on recovery and utilization of Solid FAE", 《ADVANCES IN ENGINEERING RESEARCH》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558588A (en) * | 2018-05-25 | 2018-09-21 | 中国人民解放军63908部队 | Application and method of the dodecyl pyridinium chloride in the separation of solid-liquid cloud detonator component |
| CN108727198A (en) * | 2018-05-25 | 2018-11-02 | 中国人民解放军63908部队 | Application and method of the cetyl trimethylammonium bromide in the separation of solid-liquid cloud detonator component |
| CN108558588B (en) * | 2018-05-25 | 2020-06-16 | 中国人民解放军63908部队 | Application of dodecyl pyridine chloride in separation of solid-liquid cloud blasting agent components and method |
| CN108727198B (en) * | 2018-05-25 | 2020-09-22 | 中国人民解放军63908部队 | Application of hexadecyl trimethyl ammonium bromide in solid-liquid cloud blasting agent component separation and method |
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Application publication date: 20170426 |