CN106586967B - 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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- CN106586967B CN106586967B CN201611044352.2A CN201611044352A CN106586967B CN 106586967 B CN106586967 B CN 106586967B CN 201611044352 A CN201611044352 A CN 201611044352A CN 106586967 B CN106586967 B CN 106586967B
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- ammonium perchlorate
- cloud detonator
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- extracting method
- solid cloud
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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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
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- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to the secure processing techniques field of solid energetic material, specifically disclose a kind of 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 TWEEN Series nonionic surface active agent.The inventive method can in normal temperature reclaims solid cloud detonator ammonium perchlorate, extraction time substantially shortened, and extraction efficiency is significantly improved, with higher recovery rate, 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 to be 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 occurs centroid motion during defeated and storage, influence path accuracy and explosion property are stable.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, is transported, stores, 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 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, it is necessary to carry out safe and environment-friendly recycling.Ammonium perchlorate is soluble in water, can be with
Water dissolving recovery is carried out to it.Ammonium perchlorate by deterrent paraffin, HTPB etc. due to being coated 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
Difference, and this method extraction time usually require 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, adopt
Water dissolving is carried out to solid cloud detonator with cavitation-nonionic surfactant, can be in lower temperature reclaims solid cloud detonator
Ammonium perchlorate, extraction time is substantially shortened, and extraction efficiency is significantly improved, with higher recovery rate, 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, 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；
S2, with ultrosonic extractor ultrasonic extraction is carried out to the mixed liquor, ammonium perchlorate is extracted to the aqueous solution
In；
The surfactant is TWEEN Series nonionic surface active agent.
Tween, also known as polysorbate, are nonionic surface active agent, are a series of portion of polyoxyethylene sorbitans
Divide fatty acid ester, it is nontoxic, nonirritant.The ester that TWEEN Series are formed by sorbierite from different higher fatty acids, conventional bag
Polysorbate60 is included for monostearate, Tween 80 is monoleate, polysorbas20 is monolaurate, and polysorbate40 is that single palmitic acid is (soft
Resin acid) ester.One kind in the preferred above TWEEN Series of surfactant described in the inventive method.In addition, tween 21, tween
61st, polysorbate65 etc. can be applied to the present invention.
As the preferred embodiment of the technical program, in the S1, the mass ratio of solid cloud detonator and water is 1:2~4.
Further, it is not less than 20min to obtain the ultrasonic extraction time in preferable recovery rate, S2.
It is further preferred that in the S1, the mass ratio of solid cloud detonator and water is 1: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 is carried with surfactant and ultrasonic wave
Ammonium perchlorate is taken, mechanical effect, cavitation effect and the fuel factor having using ultrasonic wave, by the motion speed for increasing medium molecule
Degree, the penetration power of increase medium cause solid cloud quick-fried 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 and high chlorine in agent
The contact of sour ammonium, can realize the ammonium perchlorate in normal temperature reclaims solid cloud detonator, and extraction time substantially shortens, contracted by a few hours
Dozens of minutes is as short as, extraction efficiency is significantly improved, while ammonium perchlorate recovery rate can be improved further up to 98%, safe operation,
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.
Embodiment
To solve ammonium perchlorate in 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-nonionic
Surfactant to solid cloud detonator carry out water dissolving, can normal temperature reclaim solid cloud detonator in ammonium perchlorate, extraction time
Substantially shorten, extraction efficiency is significantly improved, with higher recovery rate, safe operation, it is easy to control and implementation.
Embodiment 1-21 is named to be described in further detail the inventive method.
The SW-1024S standard lists groove ultrasound that each embodiment is produced using Qingdao Vista electric purification equipment Co., Ltd
Ripple cleaning machine shakes as ultrosonic extractor, its working method the bottom of for, and ultrasonic peak power is up to 1200W, supersonic frequency
28KHz。
Solid cloud detonator sample used in 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, is specially：A certain amount of solid cloud detonator is weighed as quartz
Grind alms bowl in, be included in a small amount of distilled water and be ground to uniform fine powder, be placed in 50ml conical flasks, add surfactant and
Be put into after distilled water in the ultrasonic water bath groove of aforementioned ultrasonic extraction element, under different time extract extract after solution filtering,
Titration test is carried out, ammonium perchlorate recovery rate is calculated.
The content of ammonium perchlorate is tested using formol titration in solution after extraction, and formaldehyde after ammonium perchlorate reaction with generating
H+, the content for extracting ammonium perchlorate is calculated with that can be quantified 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.
Surfactant is Tween 80 wherein used in embodiment 1-9, and surfactant used in embodiment 10-18 is tween
20, embodiment 1-3,9-12 ultrosonic extractor sets ultrasonic power to be 300W, embodiment 4-6,13-15 ultrasonic wave extraction dress
Ultrasonic power is installed for 500W, embodiment 7-9,16-18 ultrosonic extractor sets ultrasonic power to be 800W.
Different solid-liquid ratios are respectively adopted in embodiment 19-21, and surfactant uses Tween 80, and remaining detail parameters is as follows
Table 7.
With the increase of solid-liquid ratio, AP recovery rate is improved.Although aqueous solvent is cheap and easy to get, solvent increase is unfavorable
In AP crystallizations, power consumption increase, too little solvent can then cause dissolving insufficient, and can cause suction filtration loss increase.Consider energy-conservation
Efficient condition, chooses 1:3 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 tween system of ammonium perchlorate
Row nonionic surface active agent amount ranges are 1%~4%, and extraction time is 30~50min.It is quick-fried by this scheme separation solid cloud
Ammonium perchlorate in agent, recovery rate is up to more than 91%.
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, some improvement can be also carried out to the present invention, these improvement are also fallen into
In the protection domain of the claims in the present invention.
Claims (8)
1. the safe extracting method of ammonium perchlorate in a kind of solid cloud detonator, it is characterised in that：Including
S1, the pulverulent solids cloud detonator containing ammonium perchlorate is well mixed with a certain amount of water, surfactant, wherein described
The consumption of surfactant is the 1%~4% of the solid cloud detonator weight；
S2, with ultrosonic extractor ultrasonic extraction is carried out to the mixed liquor at normal temperatures, ammonium perchlorate is extracted to water
In solution；
The surfactant is TWEEN Series nonionic surface active agent.
2. the safe extracting method of ammonium perchlorate in solid cloud detonator according to claim 1, it is characterised in that the S1
In, the mass ratio of solid cloud detonator and water is 1:2~4.
3. the safe extracting method of ammonium perchlorate in solid cloud detonator according to claim 2, it is characterised in that the S1
In, the mass ratio of solid cloud detonator and water is 1:3.
4. the safe extracting method of ammonium perchlorate in the solid cloud detonator according to claim 1 or 3, it is characterised in that S2
The middle ultrasonic extraction time is not less than 20min.
5. the safe extracting method of ammonium perchlorate in solid cloud detonator according to claim 4, it is characterised in that surpass in S2
Sound extraction time is 35~50min.
6. the safe extracting method of ammonium perchlorate in solid cloud detonator according to claim 5, it is characterised in that surpass in S2
The power that sound wave extraction element carries out ultrasonic extraction to the mixed liquor is 300~800W, and supersonic frequency is 28KHz.
7. the safe extracting method of ammonium perchlorate in solid cloud detonator according to claim 1, it is characterised in that the table
Face activating agent is one kind in polysorbas20, polysorbate40, polysorbate60, Tween 80.
8. the safe extracting method of ammonium perchlorate in solid cloud detonator according to claim 1, it is characterised in that the S2
Ultrasonic extraction is carried out in room temperature.
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| CN201611044352.2A CN106586967B (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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| CN106586967B true CN106586967B (en) | 2017-10-10 |
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| CN108722000B (en) * | 2018-05-25 | 2020-09-29 | 中国人民解放军63908部队 | Application of dodecyl trimethyl ammonium bromide in solid-liquid cloud blasting agent component separation and method |
| CN110078025B (en) * | 2019-05-14 | 2020-10-23 | 中国人民解放军32181部队 | Method for extracting ammonium perchlorate in scrapped HTPB propellant under assistance of microwave-surfactant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4854982A (en) * | 1989-01-31 | 1989-08-08 | The United States Of America As Represented By The Secretary Of The Army | Method to dimilitarize extract, and recover ammonium perchlorate from composite propellants using liquid ammonia |
| CN102372747A (en) * | 2010-08-23 | 2012-03-14 | 北京化工大学 | Method for recovering ferrocene derivatives and ammonium perchlorate from composite solid propellant |
| CN105317585A (en) * | 2014-07-22 | 2016-02-10 | 湖北航天化学技术研究所 | In-situ AP extracting device for small-sized composite solid rocket motor grain |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8585840B2 (en) * | 2003-08-29 | 2013-11-19 | G.D.O., Inc. | Recovery of the energetic component from plastic bonded explosives |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4854982A (en) * | 1989-01-31 | 1989-08-08 | The United States Of America As Represented By The Secretary Of The Army | Method to dimilitarize extract, and recover ammonium perchlorate from composite propellants using liquid ammonia |
| CN102372747A (en) * | 2010-08-23 | 2012-03-14 | 北京化工大学 | Method for recovering ferrocene derivatives and ammonium perchlorate from composite solid propellant |
| CN105317585A (en) * | 2014-07-22 | 2016-02-10 | 湖北航天化学技术研究所 | In-situ AP extracting device for small-sized composite solid rocket motor grain |
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