CN106744693A - The safe extracting method of ammonium perchlorate in a kind of solid cloud detonator - Google Patents
The safe extracting method of ammonium perchlorate in a kind of solid cloud detonator Download PDFInfo
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- CN106744693A CN106744693A CN201611044755.7A CN201611044755A CN106744693A CN 106744693 A CN106744693 A CN 106744693A CN 201611044755 A CN201611044755 A CN 201611044755A CN 106744693 A CN106744693 A CN 106744693A
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- ammonium perchlorate
- cloud detonator
- solid
- extracting method
- 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
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- 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)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to the secure processing techniques field of solid energetic material, specifically disclose a kind of safe extracting method of ammonium perchlorate in solid cloud detonator, including the pulverulent solids cloud detonator containing ammonium perchlorate is well mixed with a certain amount of water, surfactant, wherein the consumption of the surfactant is the 1%~4% of the solid cloud detonator weight；In room temperature, ultrasonic extraction is carried out to the mixed liquor with ultrosonic extractor, ammonium perchlorate is extracted in the aqueous solution；The surfactant is sodium sulfonate anion surfactant.The inventive method can in normal temperature reclaims solid cloud detonator ammonium perchlorate, extraction time substantially shortened, and extraction efficiency is significantly improved, with recovery rate higher, safe operation, it is easy to control and implemented.
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 directed to liquid-solid composite cloud detonator not
Develop enough, liquid solid-state cloud detonator has density contrast between certain mobility, each component larger, is loaded in body, in fortune
Easily occur centroid motion, influence path accuracy and explosion property stabilization during defeated and storage.Solid cloud detonator is with solid-state
Confection is loaded in warhead, forms the two-phase 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, common metal in solid cloud detonator
Powder, such as aluminium powder.It is, in order to adjust the susceptibility of mixture, to make it smoothly detonation that sensitizer is added in solid cloud detonator, and
And make detonation property stabilization 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, it is necessary to carry out safe and environment-friendly recycling.Ammonium perchlorate is soluble in water, can be with
Water dissolves 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 has using boiled process to reclaim the ammonium perchlorate in solid energetic material, and final recovery rate is 85%
Between~90%, but its water temperature is higher, it is necessary to be heated 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 dissolves are carried out to solid cloud detonator with cavitation-anion surfactant, can be in lower temperature reclaims solid cloud detonator
Ammonium perchlorate, extraction time is substantially shortened, and extraction efficiency is significantly improved, with recovery rate higher, safe operation, it is easy to control
And implementation.
In order to solve the above technical problems, 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 be well mixed 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, in room temperature, ultrasonic extraction is carried out to the mixed liquor with ultrosonic extractor, ammonium perchlorate is extracted to water-soluble
In liquid；
The surfactant is sodium sulfonate anion surfactant.
Anion surfactant is divided into carboxylate, sulfonate, sulfuric acid and the major class of phosphate ester salt four, sulphur from structure
Sour sodium anion surfactant belongs to sulfonate anionic surfactant, and it includes aliphatic alcohol polyoxyethylene sulfonate again
Surfactant, aryl or fatty alcohol ethers sulfosalt surfactant, aliphatic acid (ester) sulfosalt surfactant, alkylbenzene
Sulfosalt surfactant etc..
Preferably neopelex or diisooctyl succinate sodium sulfonate anion surfactant of the invention.
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, to obtain preferable recovery rate, the ultrasonic 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 ultrasonic extraction time is in 3, S2
35~50min.
The power that ultrosonic extractor carries out ultrasonic extraction to the mixed liquor in S2 is 300~800W, supersonic frequency
Rate is 28KHz.
Optionally, the S2 carries out ultrasonic extraction in room temperature.
It is using the beneficial effect produced by above-mentioned technical proposal：The inventive method anion surfactant and super
Sound wave extracts ammonium perchlorate, the mechanical effect having using ultrasonic wave, cavitation effect and fuel factor, by increasing medium molecule
Movement velocity, the penetration power of increase medium cause solid to extract ammonium perchlorate in solid cloud detonator especially with cavitation effect
The rupture to the clad and three dimensional network structure of 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 normal 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 recovery rate can be improved further up to 98%, behaviour
Make safety, it is simple and easy to apply.
Brief description of the drawings
Fig. 1 is the process chart of ammonium perchlorate extraction in the inventive method embodiment.
Specific embodiment
It is ammonium perchlorate in solution prior art solid cloud detonator（AP）Extraction efficiency is low, Extracting temperature is high, security is low
Etc. technical problem, the invention discloses a kind of safe extracting method of ammonium perchlorate in solid cloud detonator, using cavitation-anion
Surfactant carries out water dissolves to solid cloud detonator, can normal temperature reclaim solid cloud detonator in ammonium perchlorate, extraction time
Substantially shorten, extraction efficiency is significantly improved, with recovery rate higher, safe operation, it is easy to control and implementation.
Embodiment 1-21 is named to be described in further detail the inventive method.
Each embodiment is ultrasonic using the SW-1024S standard lists groove of Qingdao Vista electric purification equipment Co., Ltd 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 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, be placed in 50ml conical flasks, add anionic surface to live
Property agent and distilled water after be put into the ultrasonic water bath groove of aforementioned ultrasonic extraction element, solution after extracting is extracted under the different time
Filter, carry out titration test, calculate ammonium perchlorate recovery rate.
The content of ammonium perchlorate is tested using formol titration in solution after extraction, is generated after formaldehyde and ammonium perchlorate reaction
H+, the content of ammonium perchlorate is extracted with that can quantify to calculate after NaOH solution drop reaction liquid, then by solid cloud detonator used
Technical indicator calculates the content of ammonium perchlorate in cloud detonator, thus obtains the recovery rate 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 obtained by calculating the recovery rate of ammonium perchlorate see the table below 1-7.Wherein the consumption of surfactant accounts for solid cloud detonator with it
The percentage of weight is represented.
Anion surfactant is neopelex, the moon used by embodiment 10-18 wherein used by embodiment 1-9
Ionic surface active agent is diisooctyl succinate sodium sulfonate, and embodiment 1-3,9-12 ultrosonic extractor sets ultrasonic power
It is 300W, it is 500W, embodiment 7-9,16-18 ultrasonic wave that embodiment 4-6,13-15 ultrosonic extractor sets ultrasonic power
It is 800W that extraction element sets ultrasonic power.
Embodiment 19-21 is respectively adopted different solid-liquid ratios, and surfactant uses neopelex, and remaining is detailed
Thin parameter such as table 7 below.
With the increase of solid-liquid ratio, the recovery rate of AP is improved.Although aqueous solvent is cheap and easy to get, it is unfavorable that solvent increases
In AP crystallizations, power consumption increase, too little solvent can then cause dissolving insufficient, and suction filtration can be caused to lose increase.Consider energy-conservation
Efficient condition, chooses 1:3 used as suitable solid-liquid ratio, and AP more can sufficiently be extracted and be conducive to AP to tie under the conditions of this
It is brilliant.
Contrasted from above example, influence very little of the temperature to recovery rate, preferably extract the sodium sulfonate of ammonium perchlorate
Anion surface active amount ranges are 1%~4%, and extraction time is 30~50min.By in this scheme separation solid cloud detonator
Ammonium perchlorate, recovery rate is up to more than 94%.
The inventive method is described in detail above, application specific case is 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 be well mixed 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, ultrasonic extraction is carried out to the mixed liquor with ultrosonic extractor, ammonium perchlorate is extracted in the aqueous solution；
The surfactant is sodium sulfonate anion surfactant.
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 ultrasonic 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
The power that sound wave extraction element carries out ultrasonic extraction to the mixed liquor is 300~800W, 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 neopelex or diisooctyl succinate sodium sulfonate.
8. in solid cloud detonator according to claim 1 ammonium perchlorate safe extracting method, it is characterised in that the S2
Ultrasonic extraction is carried out in room temperature.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611044755.7A CN106744693A (en) | 2016-11-24 | 2016-11-24 | The safe extracting method of ammonium perchlorate in a kind of solid cloud detonator |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611044755.7A CN106744693A (en) | 2016-11-24 | 2016-11-24 | The safe extracting method of ammonium perchlorate in a kind of solid cloud detonator |
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| CN106744693A true CN106744693A (en) | 2017-05-31 |
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| CN201611044755.7A Pending CN106744693A (en) | 2016-11-24 | 2016-11-24 | The safe extracting method of ammonium perchlorate in a kind of solid cloud detonator |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109956455A (en) * | 2019-05-14 | 2019-07-02 | 中国人民解放军32181部队 | A kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants |
| CN110078025A (en) * | 2019-05-14 | 2019-08-02 | 中国人民解放军32181部队 | The method that microwave-surfactant assisted extraction scraps ammonium perchlorate in HTPB propellant |
Citations (3)
| 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 |
-
2016
- 2016-11-24 CN CN201611044755.7A patent/CN106744693A/en active Pending
Patent Citations (3)
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| T.F. SHI ET AL.: "Research on recovery and utilization of Solid FAE", 《ADVANCES IN ENGINEERING RESEARCH》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109956455A (en) * | 2019-05-14 | 2019-07-02 | 中国人民解放军32181部队 | A kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants |
| CN110078025A (en) * | 2019-05-14 | 2019-08-02 | 中国人民解放军32181部队 | The method that microwave-surfactant assisted extraction scraps ammonium perchlorate in HTPB propellant |
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Application publication date: 20170531 |