CN109956455A - A kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants - Google Patents
A kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants Download PDFInfo
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- CN109956455A CN109956455A CN201910397750.XA CN201910397750A CN109956455A CN 109956455 A CN109956455 A CN 109956455A CN 201910397750 A CN201910397750 A CN 201910397750A CN 109956455 A CN109956455 A CN 109956455A
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- propellant
- ammonium perchlorate
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of methods that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants, are related to scrapping propellant component recovery technology field.Steps are as follows: (1) propellant is broken；(2) propellant is placed in water: dehydrated alcohol: petroleum ether volume ratio be 1:1:1 mixed solution in impregnate swelling 10 ~ for 24 hours, 33 ~ 48 DEG C of temperature；(3) it after being swollen, filters, distilled water is added into propellant, the mass ratio of propellant and distilled water is 1:10 ~ 15, and the neopelex for accounting for 1 ~ 1.5wt% of distilled water is added, and 1 ~ 3h is extracted in stirring, then 1 ~ 3h of soak extraction is finally placed in 1 ~ 3h of extraction in 720W ~ 960W ultrasonic wave；48 DEG C of water temperature in extraction process；(4) it after extracting, filters, merges to after swelling with the filtrate obtained after extraction, evaporative crystallization after secondary filter obtains ammonium perchlorate.With this method, the recovery rate of ammonium perchlorate is high, extracts quickly, and safety and environmental protection is at low cost, and is common agents and instrument needed for this method, and operating method is simple and easy, is suitble to large-scale application.
Description
Technical field
The present invention relates to propellant component recovery technology field is scrapped, especially a kind of ultrasound assisted extraction scraps four constituent elements
The method of ammonium perchlorate in HTPB propellant.
Background technique
Ammonium perchlorate is a kind of common 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.Its property is active, with reducing agent, combustibles and gold
Belonging to the mixing such as powder can explode.It is soluble easily in water, water dissolution recycling can be carried out to it.
Solid propellant occupies status of crucial importance in military field, and the power source as engine is remarkably improved
Weapon survival ability and operational exertion ability.In all kinds of solid propellants, four constituent element HTPB propellants are easy to get with its raw material,
Have a safety feature, good mechanical performance the advantages that, be used widely on playing arrow and space industry.But due to the military service of weapon
Expire, production factors not up to standard and internal aging etc., annual military power's waste solid propellant to be treated is up to ten thousand tons.
Since waste solid propellant is still energetic material, there is burning, blast characteristics, while its safety reduces, it is with higher
Risk.Therefore, it is necessary to carry out effective, safety to waste solid propellant, timely handle.Wherein, waste solid is promoted
Agent component carries out recycling and reusing, is one of current most green effective processing mode.
In four constituent element HTPB propellant formulation systems, oxidant ammonium perchlorate is main constituent, accounts for propellant mass
Score is about 60%~70%.Ammonium perchlorate in four constituent element HTPB propellants is plasticized agent, HTPB (end hydroxy butadiene)
Deng close cladding, hydrone is difficult to enter dissolution.In the data found, solid energetic material is recycled using boiled process
In ammonium perchlorate.Have the disadvantage that recovery rate is low first is that water is very poor to the swellability of propellant, second is that Extracting temperature mistake
Height, majority reach 70-80 DEG C, and extraction effect is general；Third is that using tetrahydrofuran, toluene and CHCl3Equal highly volatiles, toxicity is very
By force, unstable chemcial property, is easy photochemical substance, and even carcinogenic substance is very big to health damage.And use CHCl3
The swelling ratio of swelling is up to 70% or so, and swelling effect is general.How a large amount of, low cost is simultaneously extracted to safety and environmental protection and is scrapped
Ammonium perchlorate in four constituent element HTPB propellants is the key points and difficulties of research.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of ultrasound assisted extractions to scrap height in four constituent element HTPB propellants
The method of ammonium chlorate, this method realize the safe and efficient extraction of ammonium perchlorate in four constituent element HTPB propellants.With this method,
The recovery rate of ammonium perchlorate is high, extracts quickly, safety and environmental protection is at low cost, and is common agents and instrument needed for this method
Device, operating method is simple and easy, is suitble to large-scale application.
In order to solve the above technical problems, the technical solution used in the present invention is: a kind of ultrasound assisted extraction scraps four groups
The method of ammonium perchlorate in first HTPB propellant, comprising the following steps:
(1) be crushed: it is broken to carry out safety to four constituent element HTPB propellants；
(2) be swollen: propellant is placed in water: dehydrated alcohol: impregnating in the mixed solution that the volume ratio of petroleum ether is 1:1:1 molten
Swollen 10~for 24 hours, mixed solution temperature is 33~48 DEG C；
(3) it extracts: after swelling, filtering, after washes clean, be added distilled water into propellant, propellant and distilled water
Mass ratio is 1:10~15, is added and accounts for the neopelex surface-active that distilled water mass fraction is 1%~1.5%
1~3h is extracted in agent, stirring, then 1~3h of soak extraction, is finally placed in ultrasonic wave 1~3h of extraction under power 720W~960W；
Water temperature is 48 DEG C in entire extraction process；
(4) it after extracting, filters, after washes clean, is closed to the filtrate obtained after resulting filtrate and extraction is filtered after swelling
And evaporative crystallization is carried out after secondary filter, obtain ammonium perchlorate.
Preferably, it after step (1) carries out safe be crushed to four constituent element HTPB propellants, is also cleaned: to propellant
Middle addition petroleum ether impregnates, ultrasonic cleaning.
Preferably, in step (2), propellant is placed in water: dehydrated alcohol: the volume ratio of petroleum ether is the mixing of 1:1:1
Swelling 10h is impregnated in solution, mixed solution temperature is 48 DEG C.
Preferably, in step (2), the grams of propellant and a ml ratio for mixed solution are 1:18.
Preferably, in step (3), after swelling, filter, after washes clean, be added distilled water into propellant, propellant with
The mass ratio of distilled water is 1:10, is added and accounts for the neopelex surfactant that distilled water mass fraction is 1%, stirs
It mixes and extracts 1h, then 2~3h of soak extraction, is finally placed in ultrasonic wave and extracts 1h under power 960W；Water in entire extraction process
Temperature is 48 DEG C.
Preferably, it in step (3), after swelling, filters, the propellant grain after being washed with distilled water clean swelling.
Preferably, it in step (4), after extraction, filters, the propellant grain after being washed with distilled water clean extract.
Reaction principle of the invention: the mixed solution of water, dehydrated alcohol and petroleum ether is swollen propellant, greatly
Increase the volume of propellant so that clad no longer tight ammonium perchlorate, be hydrone enter dissolution perchloric acid
Ammonium provides channel.The vibration that ultrasonic wave generates, generates cavitation, and then formation sound miniflow, spray and shock wave etc. in a liquid
Strong sonic-effect is answered, and then greatly improves the area and speed of leaching.The hydrophilic effect of neopelex surfactant
Should make hydrone more rapidly with ammonium perchlorate contact lysis.
The beneficial effects of adopting the technical scheme are that
(1) the method for the present invention realizes the safe and efficient extraction of ammonium perchlorate in four constituent element HTPB propellants.With we
Method, the recovery rate of ammonium perchlorate is high, extracts quickly, and safety and environmental protection is at low cost, and needed for this method be common agents and
Instrument, operating method is simple and easy, is suitble to large-scale application.
(2) present invention is swollen propellant using the mixed solution of water, dehydrated alcohol and petroleum ether, swelling effect ratio
Existing method is more preferable, and swelling ratio is minimum up to 106%, solves the problems, such as to promote solvent swell hardly possible, and solvent for use toxicity is low,
Stability is good.
(3) present invention improves extraction rate using ultrasonic wave added, reduces the temperature of extraction, the sound miniflow of ultrasonic wave is utilized
It is acted on spray.
(4) present invention is added neopelex surfactant and utilizes the technology of ultrasonic wave under 48 DEG C of water temperatures
Means, extract the ammonium perchlorate in propellant, 2~3h of soaking time, and recovery rate can reach 97.05% or more, solve water temperature
Excessively high problem, and recovery rate improves many.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments；
Fig. 1 be in the embodiment of the present invention 1 HTPB propellant in water: dehydrated alcohol: the swelling ratio of petroleum ether in the mixed solvent
Curve graph.
Specific embodiment
Embodiment 1
A kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants, comprising the following steps: right
Four constituent element HTPB propellants carry out safety and are crushed, and broken propellant sample original dimension is 10mm × 5mm × 3mm；5g is pushed away
It is placed in conical flask into agent, petroleum ether is added, impregnated 3 minutes, ultrasonic power is that 720W is cleaned 3 minutes, is cleaned 3 times.Cleaning
5g propellant is placed in water after clean: dehydrated alcohol: the volume ratio of petroleum ether is that swelling is impregnated in the mixed solution 90ml of 1:1:1
For 24 hours, solution temperature is 33 DEG C.It then filters, after the propellant grain after being washed with distilled water clean swelling, distilled water is added,
The mass ratio of propellant and distilled water is 1:10, is added and accounts for the neopelex surface that distilled water mass fraction is 1%
Activating agent, revolving speed is stirs 1h in the constant temperature blender with magnetic force of 500r, and then soak extraction 3h, is finally placed in power in ultrasonic wave
1h is mentioned under 960W, it is 48 DEG C that water temperature is constant in entire extraction process.It after extraction, filters, after being washed with distilled water clean extract
After propellant grain, merges to the filtrate obtained after resulting filtrate and extraction is filtered after swelling, be evaporated after secondary filter
Crystallization, obtains ammonium perchlorate, purity is up to 99.01%.The recovery rate of ammonium perchlorate is 97.26%.
Wherein, HTPB propellant is in water: dehydrated alcohol: the swelling ratio curve graph in petroleum ether mixed solution is as shown in Figure 1.
As shown in Figure 1, HTPB propellant is under water and dehydrated alcohol and the mixed solution of petroleum ether three, to the swelling effect of propellant
Most preferably, 24 hours swelling ratios are minimum up to 106.82%.The swelling rate of propellant in a solvent is incremental there is one
Process then tends towards stability, until reaching swelling equilibrium, does not continue to swelling and increases.And it can be seen that pushing away for same solution
Into solvent swell than size, thickness is maximum, and width takes second place, and length is minimum.Illustrate that the size of propellant is smaller, swelling ratio is bigger.
Embodiment 2
A kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants, comprising the following steps: right
Four constituent element HTPB propellants carry out safety and are crushed, and broken propellant sample size is less than 4mm；10g propellant is placed in taper
In bottle, petroleum ether is added, impregnates 3 minutes, ultrasonic power is that 720W is cleaned 3 minutes, is cleaned 3 times.Clean up rear propellant
Be placed in water: dehydrated alcohol: the volume ratio of petroleum ether is that swelling 10h is impregnated in the mixed solution 180ml of 1:1:1, and solution temperature is
48℃.It then filters, after the propellant grain after being washed with distilled water clean swelling, distilled water, propellant and distilled water is added
Mass ratio be 1:10, be added and account for the neopelex surfactant that distilled water mass fraction is 1%, revolving speed is
1h is stirred in the constant temperature blender with magnetic force of 500r, then 1~3h of soak extraction, be finally placed in ultrasonic wave and extract under power 960W
1h, it is 48 DEG C that water temperature is constant in entire extraction process.It is then filtered by vacuum, the propulsion after being washed with distilled water clean extract
After agent particle, the filtrate obtained after the filtrate filtered after swelling and extraction is merged, evaporative crystallization is carried out after secondary filter,
Obtain ammonium perchlorate.
When considering dosage of surfactant using the influence test of neopelex surfactant concentration, extract
Between, the influence to extraction effect such as temperature, table 1 is sampling test data.
1 sampling test data of table
As shown in Table 1, when surfactant qualities score is 1%, the ultrasonic wave for being 960W using power, soaking time
When 1~3h, the recovery rate of ammonium perchlorate reaches 93.83% or more, and purity is up to 98.81% or more.
Embodiment 3
A kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants, comprising the following steps: right
Four constituent element HTPB propellants carry out safety and are crushed, and broken propellant sample size is less than 4mm；5g propellant is placed in conical flask
In, petroleum ether is added, impregnates 3 minutes, ultrasonic power is that 720W is cleaned 3 minutes, is cleaned 3 times.Clean up rear propellant 5g
Be placed in water: dehydrated alcohol: the volume ratio of petroleum ether is that swelling 12h, solution temperature 41 are impregnated in the mixed solution 90ml of 1:1:1
℃.It then filters, after the propellant grain after being washed with distilled water clean swelling, is added distilled water, propellant and distilled water
Mass ratio is 1:15, and 1.5% neopelex surfactant is added, and revolving speed is the constant temperature blender with magnetic force of 500r
Upper stirring 1h, then soak extraction 2h, is finally placed in ultrasonic wave and mentions 1h under power 720W, and water temperature is constant in entire extraction process
It is 48 DEG C.It is then filtered by vacuum, after the propellant grain after being washed with distilled water clean extract, is obtained being filtered after swelling
Filtrate and extraction after obtained filtrate merge, to resulting filtrate is filtered, carry out evaporative crystallization after secondary filter, obtain high chlorine
Sour ammonium.The recovery rate of ammonium perchlorate is 94.42%, and purity is up to 99.21%.
Claims (7)
1. a kind of method that ultrasound assisted extraction scraps ammonium perchlorate in four constituent element HTPB propellants, which is characterized in that including with
Lower step:
(1) be crushed: it is broken to carry out safety to four constituent element HTPB propellants；
(2) be swollen: propellant is placed in water: dehydrated alcohol: the volume ratio of petroleum ether is that swelling 10 is impregnated in the mixed solution of 1:1:1
~ for 24 hours, mixed solution temperature is 33 ~ 48 DEG C；
(3) it extracts: after swelling, filtering, after washes clean, distilled water, the quality of propellant and distilled water are added into propellant
The neopelex surfactant that distilled water mass fraction is 1% ~ 1.5% is accounted for than being added for 1:10 ~ 15, stirring mentions
1 ~ 3h is taken, then 1 ~ 3h of soak extraction, is finally placed in ultrasonic wave 1 ~ 3h of extraction under power 720W ~ 960W；Entire extraction process
Middle water temperature is 48 DEG C；
(4) it after extracting, filters, after washes clean, merges to the filtrate obtained after resulting filtrate and extraction is filtered after swelling, two
Evaporative crystallization is carried out after secondary filtering, obtains ammonium perchlorate.
2. the side that a kind of ultrasound assisted extraction according to claim 1 scraps ammonium perchlorate in four constituent element HTPB propellants
Method, which is characterized in that after step (1) carries out safe be crushed to four constituent element HTPB propellants, also cleaned: into propellant
Petroleum ether is added, impregnates, ultrasonic cleaning.
3. the side that a kind of ultrasound assisted extraction according to claim 1 scraps ammonium perchlorate in four constituent element HTPB propellants
Method, which is characterized in that in step (2), propellant is placed in water: dehydrated alcohol: the volume ratio of petroleum ether is that the mixing of 1:1:1 is molten
Swelling 10h is impregnated in liquid, mixed solution temperature is 48 DEG C.
4. the side that a kind of ultrasound assisted extraction according to claim 1 scraps ammonium perchlorate in four constituent element HTPB propellants
Method, which is characterized in that in step (2), the grams of propellant and a ml ratio for mixed solution are 1:18.
5. the side that a kind of ultrasound assisted extraction according to claim 1 scraps ammonium perchlorate in four constituent element HTPB propellants
Method, which is characterized in that in step (3), after swelling, filter, after washes clean, be added distilled water into propellant, propellant with
The mass ratio of distilled water is 1:10, is added and accounts for the neopelex surfactant that distilled water mass fraction is 1%, stirs
It mixes and extracts 1 h, then 2 ~ 3h of soak extraction, is finally placed in ultrasonic wave and extracts 1h under power 960W；Water in entire extraction process
Temperature is 48 DEG C.
6. the side that a kind of ultrasound assisted extraction according to claim 1 scraps ammonium perchlorate in four constituent element HTPB propellants
Method, which is characterized in that in step (3), after swelling, filter, the propellant grain after being washed with distilled water clean swelling.
7. the side that a kind of ultrasound assisted extraction according to claim 1 scraps ammonium perchlorate in four constituent element HTPB propellants
Method, which is characterized in that in step (4), after extraction, filter, the propellant grain after being washed with distilled water clean extract.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620253A (en) * | 2020-05-06 | 2021-11-09 | 南京理工大学 | Preparation method of expanded ammonium perchlorate |
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