CN107098867A - A kind of method for extracting hexogen in solid cloud detonator - Google Patents
A kind of method for extracting hexogen in solid cloud detonator Download PDFInfo
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- CN107098867A CN107098867A CN201710262093.9A CN201710262093A CN107098867A CN 107098867 A CN107098867 A CN 107098867A CN 201710262093 A CN201710262093 A CN 201710262093A CN 107098867 A CN107098867 A CN 107098867A
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- hexogen
- leaching
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- extracting
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/04—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D251/06—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with hetero atoms directly attached to ring nitrogen atoms
Abstract
The invention discloses a kind of method for extracting hexogen in solid cloud detonator, it is related to energetic material technical field, comprises the following steps：The extraction experimental technique of hexogen in cloud detonator is determined, the technique is supersonic leaching crystallisation；It is experimental factor to choose ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number of times using orthogonal test method, and evaluation index is used as using recovery rate；Test combinations are determined according to the orthogonal arrage that the value of each factor chooses five factors and five levels, and carry out extraction experiment；Analyzed using synthesis necessary technology extracting test data, choose optimal factor group technology；Carry out repeating experimental verification with the combination of optimal factor, determine optimised process, few with the used time, operating method is simple and easy to apply, the characteristics of recovery rate is high.
Description
Technical field
The invention belongs to energetic material technical field, and in particular to a kind of method of hexogen in extraction solid cloud detonator.
Background technology
Hexogen（RDX）Also known as cyclonite, it is a kind of conventional high explosive, there is extensive in numerous energetic materials
Using.It is used for the explosives such as terraced black aluminium, civilian production detonator, primacord and making priming glue etc. in national defense industry.Its chemistry
Property is stable, and power is extremely strong, is a kind of splendid explosive of combination property.
Hexogen in solid cloud detonator is by paraffin, end hydroxy butadiene（HTPB）Deng cladding, it is not easy to by organic molten
Agent is directly dissolved, and causes the increasing for extracting difficulty.In the data found, reclaim solid using organic solvent technique and contain energy
Hexogen in material, recovery rate is generally relatively low, and highest recovery rate is 90%.
The content of the invention
The technical problem to be solved in the present invention is that there is provided one kind extraction solid cloud detonator for above-mentioned the deficiencies in the prior art
The method of middle hexogen, solves to extract the problem of difficulty is big, recovery rate is universal relatively low, with the used time is few, operating method is simply easy
Row, the characteristics of recovery rate is high.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of method for extracting hexogen in solid cloud detonator, comprises the following steps：
（1）The extraction experimental technique of RDX in cloud detonator is determined, the technique is supersonic leaching crystallisation；
（2）It is experiment to choose ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number of times using orthogonal test method
Factor, evaluation index is used as using recovery rate；
（3）The orthogonal arrage of five factors and five levels is chosen according to the value of each factor（L25（56））Test combinations are determined, and are carried
Take experiment；
（4）Analyzed using synthesis necessary technology extracting test data, choose optimal factor group technology；
（5）Step is carried out with the combination of optimal factor（1）Extraction test technology, repeat verification experimental verification, determine optimised process.
Further, the extraction experimental technique is comprised the following specific steps that：
（1）Slightly grind：Solid cloud detonator is ground to graininess；Increase contact area；
（2）Leaching：Cloud detonator particle is placed in the container equipped with leaching agent, ultrasound in supersonic wave cleaning machine, leaching is put into；RDX
Dissolve in acetone but insoluble in petroleum ether, HTPB then dissolubility on the contrary, matching suitable leaching agent and can reaching makes mixed system
The solubilizing effect being swelled, outside plus ultrasonication, RDX clad and three dimensional network structure, increases solvent in destruction cloud detonator
Contact with RDX, is more beneficial for RDX leaching；
（3）Suction filtration is simultaneously rotated：Leaching system is depressurized into suction filtration, filtrate revolving obtains RDX crystallizations；Acetone, petroleum ether boiling point exist
Less than 60 DEG C, and RDX bursting point is up to about 240 DEG C, this mixed solvent can ensure later stage RDX evaporative crystallization and drying process
In security；
（4）Washing：RDX crystallizations are washed with acetone, suction filtration, revolving obtain RXD；The removal of impurity is gone in enough acetone washings；
The acetone that revolving is reclaimed can be recycled；
（5）Dry：RXD is placed in drying in oven.
Further, the step（2）In, leaching agent is volume ratio petroleum ether：Acetone=2:8 mixed solvent.
Further, the step（2）In, the production of supersonic wave cleaning machine Qingdao Vista electric purification equipment Co., Ltd
SW-1024S standard single groove ultrasonic cleaning machines, its working method shakes the bottom of for, and ultrasonic peak power is up to 1200W, supersonic frequency
Rate 28KHz.
Further, the step（5）In, 45-65 DEG C of drying temperature, time 4-6h.
Further, the synthesis necessary technology includes analysis below step：
（1）Ask for the K of each factor leveliWith R values, KiFor factor the i-th level to the coefficient of evaluation index and；R is extreme difference,
R=max{Ki}-min{Ki}；
（2）According to KiValue determines preferred levels, wherein for corresponding to the maximum of more big more excellent selecting index respective column
Level；
（3）Primary and secondary order is determined according to R values, wherein, R values are bigger to represent that influence is bigger, and R values are smaller to represent that influence is smaller, obtains
Optimal factor group technology.
It is using the beneficial effect produced by above-mentioned technical proposal：Hexogen in a kind of extraction solid cloud detonator of the invention
Method, realize the safe and efficient extraction of hexogen in cloud detonator, the recovery rate of hexogen reaches as high as 99%.And we
Needed for method is common agents and instrument, and operating method is simple and easy to apply.
Embodiment
With reference to specific embodiment, the present invention is further detailed explanation.
First, the extraction experimental technique of RDX in cloud detonator is determined, including slightly grinds, leach, suction filtration and rotating, wash, do
It is dry, it is exemplified below：
Weigh 2g cloud bursting charges and be placed in conical flask, quantitative mixed solvent is measured with pipette（Petroleum ether：Acetone=2:8, volume
Than）, conical flask is placed in supersonic wave cleaning machine constant temperature water bath after ultrasound, suction filtration and is evaporated filtrate to obtain RDX crystallizations, by RDX
Washed after crystallization with enough acetone after the removal of impurity, suction filtration and collect filtrate be evaporated the RDX after being purified crystallization, be placed in 60
After being dried 5 hours in DEG C baking oven, the RDX rate of recovery is calculated using weight method.
Then, ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number of times are chosen using orthogonal test method
For experimental factor, evaluation index is used as using recovery rate.
According to orthogonal arrage（L25（56））Test combinations are determined, ultrasonic power comes the 1st row, and leaching time comes the 2nd row, temperature
Degree comes the 3rd row, and solid-liquid ratio comes the 4th row, and leaching number of times comes the 5th row, and sky is classified as the 6th row, and carries out extraction experiment；It is determined that
Optimal factor group technology simultaneously verifies optimised process.
Using ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number of times as experimental factor, factor water is built
Flat table is as shown in the table.
Because of the orthogonal test using five factors and five levels, while there are row, therefore use（L25（56））Orthogonal arrage, orthogonal arrage 1-
6 row are arranged respectively：Ultrasonic power（A）, leaching time（B）, ultrasonic temperature（C）, solid-liquid ratio（D）, leaching number of times（E）With sky row
（F）.Extraction experiment is carried out to each group technology, data handled using Comprehensive Balance Method, as a result such as following table institute
Show.
R values can be obtained in table, drawn using extreme difference as process optimization judgment basis the influence degree of each experimental factor as：Ultrasonic work(
Rate>Leaching time>Ultrasonic temperature>Solid-liquid ratio>Number of times is leached, because R values are bigger, illustrates that this factor is also bigger on experiment influence.
In conjunction with KiThe size of value, according to K in tableiData, optimised process preferably is：A1B4C1D1E3, and consider in practical operation
Save efficient, E3 is changed to E1, that is, leach number of times and be changed to by 3 times 1 time, it is proper to choose optimum process A1B4C1D1E1
, i.e. ultrasonic power 960W, leaching time 60min, 40 DEG C of ultrasonic temperature, solid-liquid ratio 1/25, leaching number of times 1 time.
It can be obtained more than, using solid-liquid ratio 1/25, under the conditions of 40 DEG C, using 960W power ultrasonics and leach 60min as most
Good technique, and do not include this group of factor group technology in orthogonal test combination, confirmatory experiment, checking need to be carried out to the optimised process
Optimised process experimental result see the table below.
Data display in table, the recovery rate of three groups of confirmatory experiments is higher by recovery rate of the prior art more than 97%, it was demonstrated that
The optimised process is rational.A kind of method for extracting hexogen in solid cloud detonator of the present invention, operating method is simple and easy to apply, real
The safe and efficient extraction of hexogen in cloud detonator is showed.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, the present invention
Claimed scope is by appended claims, specification and its equivalent thereof.
Claims (6)
1. a kind of method for extracting hexogen in solid cloud detonator, it is characterised in that comprise the following steps：
（1）The extraction experimental technique of hexogen in cloud detonator is determined, the technique is supersonic leaching crystallisation；
（2）It is experiment to choose ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number of times using orthogonal test method
Factor, evaluation index is used as using recovery rate；The solid-liquid ratio is the mass ratio of cloud detonator and leaching agent；
（3）The orthogonal arrage of five factors and five levels is chosen according to the value of each factor（L25（56））Test combinations are determined, and are carried
Take experiment；
（4）Analyzed using synthesis necessary technology extracting test data, choose optimal factor group technology；
（5）Step is carried out with the combination of optimal factor（1）Extraction test technology, repeat verification experimental verification, determine optimised process.
2. a kind of method for extracting hexogen in solid cloud detonator according to claim 1, it is characterised in that the ultrasound
Leaching crystallisation is comprised the following specific steps that：
（1）Slightly grind：Solid cloud detonator is ground to graininess；
（2）Leaching：Cloud detonator particle is placed in the container equipped with leaching agent, ultrasound in supersonic wave cleaning machine, leaching is put into；
（3）Suction filtration is simultaneously rotated：Leaching system is depressurized into suction filtration, filtrate revolving obtains hexogen crystallization；
（4）Washing：Hexogen crystallization is washed with acetone, suction filtration, revolving obtain hexogen；
（5）Dry：Hexogen is placed in drying in oven.
3. a kind of method for extracting hexogen in solid cloud detonator according to claim 1 or 2, it is characterised in that the leaching
It is volume ratio petroleum ether to take agent：Acetone=2:8 mixed solvent.
4. a kind of method for extracting hexogen in solid cloud detonator according to claim 2, it is characterised in that the step
（2）In, the SW-1024S standard single groove ultrasonics of supersonic wave cleaning machine Qingdao Vista electric purification equipment Co., Ltd production
Cleaning machine.
5. a kind of method for extracting hexogen in solid cloud detonator according to claim 2, it is characterised in that the step
（5）In, 45-65 DEG C of drying temperature, time 4-6h.
6. a kind of method for extracting hexogen in solid cloud detonator according to claim 1, it is characterised in that the synthesis
Balancing method includes analysis below step：
（1）Ask for the K of each factor leveliWith R values, KiFor factor the i-th level to the coefficient of evaluation index and；R is extreme difference, R
=max{Ki}-min{Ki}；
（2）According to KiValue determines preferred levels, wherein for the water corresponding to the maximum of more big more excellent selecting index respective column
It is flat；
（3）Primary and secondary order is determined according to R values, wherein, R values are bigger to represent that influence is bigger, and R values are smaller to represent that influence is smaller, obtains
Optimal factor group technology.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109706317A (en) * | 2018-11-22 | 2019-05-03 | 西安近代化学研究所 | A kind of waste and old blunt black al explosive separation and recovery method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2616729C1 (en) * | 2016-01-28 | 2017-04-18 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" (Госкорпорация "Росатом") | Production method of the mixed gelatine explosive |
-
2017
- 2017-04-20 CN CN201710262093.9A patent/CN107098867B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2616729C1 (en) * | 2016-01-28 | 2017-04-18 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" (Госкорпорация "Росатом") | Production method of the mixed gelatine explosive |
Non-Patent Citations (1)
| Title |
|---|
| HANSSON,J.: "Thin-layer chromatographic analysis for the separation of common explosives", 《EXPLOSIVSTOFFE》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109706317A (en) * | 2018-11-22 | 2019-05-03 | 西安近代化学研究所 | A kind of waste and old blunt black al explosive separation and recovery method |
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