CN107098867B - A method of extracting hexogen in solid cloud detonator - Google Patents
A method of extracting hexogen in solid cloud detonator Download PDFInfo
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- CN107098867B CN107098867B CN201710262093.9A CN201710262093A CN107098867B CN 107098867 B CN107098867 B CN 107098867B CN 201710262093 A CN201710262093 A CN 201710262093A CN 107098867 B CN107098867 B CN 107098867B
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- hexogen
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- solid
- cloud detonator
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- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000007787 solid Substances 0.000 title claims abstract description 16
- 238000002386 leaching Methods 0.000 claims abstract description 34
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 238000005516 engineering process Methods 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 238000002474 experimental method Methods 0.000 claims abstract description 8
- 238000011156 evaluation Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- 238000012795 verification Methods 0.000 claims abstract description 5
- 238000010998 test method Methods 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000000284 extract Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000011017 operating method Methods 0.000 abstract description 4
- 239000002360 explosive Substances 0.000 description 3
- 229920002121 Hydroxyl-terminated polybutadiene Polymers 0.000 description 2
- 230000009172 bursting Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- LNDKRVOOYMEYTC-UHFFFAOYSA-N buta-1,3-dien-1-ol Chemical compound OC=CC=C LNDKRVOOYMEYTC-UHFFFAOYSA-N 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
Classifications
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a kind of methods of hexogen in extraction solid cloud detonator, are related to energetic material technical field, include the steps of determining that the extraction experimental technique of hexogen in cloud detonator, which is supersonic leaching crystallisation；Choosing ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number using orthogonal test method is experimental factor, using recovery rate as evaluation index；Test combinations are determined according to the orthogonal arrage that the value of each factor chooses five factors and five levels, and extract test；It is analyzed using synthesis necessary technology test data is extracted, chooses best factor group technology；It carries out repeating experimental verification with the combination of best factor, determines optimised process, have the used time few, operating method is simple and easy, the high feature of recovery rate.
Description
Technical field
The invention belongs to energetic material technical fields, and in particular to a method of extract hexogen in solid cloud detonator.
Background technique
Hexogen (RDX) also known as cyclonite are a kind of common high explosives, are had in numerous energetic materials extensive
Using.For the explosives such as the black aluminium of ladder, civilian production detonator, primacord and production priming glue etc. in national defense industry.Its chemistry
Property is stablized, and power is extremely strong, is a kind of explosive that comprehensive performance is splendid.
Hexogen in solid cloud detonator is coated by paraffin, end hydroxy butadiene (HTPB) etc., it is not easy to by organic molten
Agent is directly dissolved, and the increasing for extracting difficulty is caused.In the data found, contain energy using organic solvent technique recycling solid
Hexogen in material, recovery rate is generally lower, and highest recovery rate is 90%.
Summary of the invention
The technical problem to be solved by the present invention is in view of the above shortcomings of the prior art, provide a kind of extraction solid cloud detonator
The method of middle hexogen, solves the problems, such as to extract that difficulty is big, recovery rate is universal lower, has that the used time is few, operating method is simply easy
The high feature of row, recovery rate.
In order to solve the above technical problems, the technical solution used in the present invention is:
A method of hexogen in solid cloud detonator is extracted, is included the following steps:
(1) the extraction experimental technique of RDX in cloud detonator is determined, which is supersonic leaching crystallisation；
(2) choosing ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number using orthogonal test method is
Experimental factor, using recovery rate as evaluation index, the solid-liquid ratio is the mass ratio of cloud detonator and leaching agent；
(3) orthogonal arrage (L of five factors and five levels is chosen according to the value of each factor25(56)) determine test combinations, it goes forward side by side
Row extracts test；
(4) extraction test data is analyzed using synthesis necessary technology, chooses best factor group technology；
(5) the extraction test technology for carrying out step (1) is combined with best factor, is repeated verification experimental verification, is determined optimised process.
Further, the extraction experimental technique comprises the following specific steps that:
(1) it slightly grinds: solid cloud detonator is ground to graininess；Increase contact area；
(2) it leaches: cloud detonator particle is placed in the container equipped with leaching agent, be put into ultrasound in supersonic wave cleaning machine, leaching；
RDX dissolves in acetone but insoluble in petroleum ether, HTPB then dissolubility on the contrary, matching suitable leaching agent and can achieve makes mixture
It is the solubilizing effect of swelling, adds ultrasonication outside, destroy the clad and three dimensional network structure of RDX in cloud detonator, increases molten
Contact of the agent with RDX, is more advantageous to the leaching of RDX；
(3) it filters and rotates: leaching system decompression is filtered, filtrate rotates to obtain RDX crystallization；Acetone, petroleum ether boiling point
At 60 DEG C hereinafter, and the bursting point of RDX is up to about 240 DEG C, this mixed solvent can guarantee later period RDX evaporative crystallization and drying
Safety in the process；
(4) it washs: RDX crystallization being washed with acetone, filters, rotate, obtain RXD；Enough acetone washing removals
Impurity；The acetone of revolving recycling can recycle；
(5) dry: RXD is placed in drying in oven.
Further, in the step (2), leaching agent is volume ratio petroleum ether: acetone=2:8 mixed solvent.
Further, in the step (2), the production of supersonic wave cleaning machine Qingdao Vista electric purification equipment Co., Ltd
SW-1024S standard single groove ultrasonic cleaning machine, working method be bottom vibration, ultrasonic maximum power is up to 1200W, supersonic frequency
Rate 28KHz.
Further, in the step (5), 45-65 DEG C of drying temperature, time 4-6h.
Further, the synthesis necessary technology includes following analysis step:
(1) K of each factor level is soughtiWith R value, KiFor factor the i-th horizontal coefficient to evaluation index and；R is pole
Difference, R=max { Ki}-min{Ki}；
(2) according to KiIt is worth and determines preferred levels, wherein the maximum value institute for more bigger more excellent selecting index respective column is right
The level answered；
(3) primary and secondary sequence being determined according to R value, wherein R value is bigger, and expression influence is bigger, and the smaller expression influence of R value is smaller,
Obtain best factor group technology.
The beneficial effects of adopting the technical scheme are that hexogen in a kind of extraction solid cloud detonator of the present 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
It is common agents and instrument needed for method, operating method is simple and easy.
Specific embodiment
The present invention will be further described in detail below with reference to specific embodiments.
Firstly, determining the extraction experimental technique of RDX in cloud detonator, including slightly grinds, leaches, filters and rotate, washs, does
It is dry, it is exemplified below:
It weighs 2g cloud bursting charge and is placed in conical flask, measure quantitative mixed solvent (petroleum ether: acetone=2:8, body with pipette
Product ratio), conical flask is placed in ultrasound in supersonic wave cleaning machine constant temperature water bath, is evaporated filtrate to obtain RDX crystallization after suction filtration, it will
It is crystallized after RDX crystallization with after enough acetone washing removal impurity, filtering and collect filtrate and be evaporated the RDX after being purified, is set
After 5 hours dry in 60 DEG C of baking ovens, the rate of recovery of RDX is calculated using weight method.
Then, ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number are chosen using orthogonal test method
For experimental factor, using recovery rate as evaluation index.
According to orthogonal arrage (L25(56)) determining test combinations, ultrasonic power comes the 1st column, and leaching time comes the 2nd column, temperature
Degree comes the 3rd column, and solid-liquid ratio comes the 4th column, and leaching number comes the 5th column, and sky is classified as the 6th column, and extracts test；It determines
Best factor group technology simultaneously verifies optimised process.
Using ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number as experimental factor, factor water is constructed
Flat table is as shown in the table.
Because of the orthogonal test using five factors and five levels, column are existed simultaneously, therefore have used (L25(56)) orthogonal arrage, it is orthogonal
Table 1-6 column arrange respectively: ultrasonic power (A), leaching time (B), ultrasonic temperature (C), solid-liquid ratio (D), leaching number (E) and sky
It arranges (F).Test is extracted to each group technology, data are handled using Comprehensive Balance Method, as a result such as following table
It is shown.
It can be obtained by R value in table, using the very poor influence degree for obtaining each experimental factor as process optimization judgment basis are as follows: super
Acoustical power > leaching time > ultrasonic temperature > solid-liquid ratio > leaching number illustrates that this factor influences also to get on experiment because R value is bigger
Greatly.In conjunction with KiThe size of value, according to K in tableiData, preferred optimised process are as follows: A1B4C1D1E3, and consider practical behaviour
It is saved efficiently in work, E3 is changed to E1, is i.e. leaching number is changed to 1 time by 3 times, and choosing optimum process A1B4C1D1E1 is to compare conjunction
Suitable, i.e. ultrasonic power 960W, leaching time 60min, 40 DEG C of ultrasonic temperature, solid-liquid ratio 1/25 leaches number 1 time.
By that can obtain above, using solid-liquid ratio 1/25, under the conditions of 40 DEG C, with 960W power ultrasound and 60min is leached for most
Good technique, and do not include this group of factor group technology in orthogonal test combination, confirmatory experiment, verifying need to be carried out to the optimised process
Optimised process experimental result see the table below.
Data are shown in table, and the recovery rate of three groups of confirmatory experiments 97% or more, is higher by recovery rate in the prior art,
Prove that the optimised process is reasonable.A kind of method for extracting hexogen in solid cloud detonator of the present invention, operating method are simply easy
Row, realizes the safe and efficient extraction of hexogen in cloud detonator.
The basic principles, main features and advantages of the present invention have 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 above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, the present invention
Claimed range is delineated by the appended claims, the specification and equivalents thereof from the appended claims.
Claims (4)
1. a kind of method for extracting hexogen in solid cloud detonator, which comprises the steps of:
(1) the extraction experimental technique of hexogen in cloud detonator is determined, which is supersonic leaching crystallisation；
(2) choosing ultrasonic power, leaching time, ultrasonic temperature, solid-liquid ratio and leaching number using orthogonal test method is test
Factor, using recovery rate as evaluation index；The solid-liquid ratio is the mass ratio of cloud detonator and leaching agent；
(3) orthogonal arrage (L of five factors and five levels is chosen according to the value of each factor25(56)) determine test combinations, and mentioned
Take test；
(4) extraction test data is analyzed using synthesis necessary technology, chooses best factor group technology；
(5) the extraction test technology for carrying out step (1) is combined with best factor, is repeated verification experimental verification, is determined optimised process,
Wherein, the supersonic leaching crystallisation comprises the following specific steps that:
(a) it slightly grinds: solid cloud detonator is ground to graininess；
(b) it leaches: cloud detonator particle is placed in the container equipped with leaching agent, be put into ultrasound in supersonic wave cleaning machine, leaching, it is described
Leaching agent is volume ratio petroleum ether: acetone=2:8 mixed solvent；
(c) it filters and rotates: leaching system decompression is filtered, filtrate rotates to obtain hexogen crystallization；
(d) it washs: hexogen crystallization being washed with acetone, filters, rotate, obtain hexogen；
(e) dry: hexogen is placed in drying in oven.
2. a kind of method for extracting hexogen in solid cloud detonator according to claim 1, it is characterised in that the step
(2) in, the SW-1024S standard single groove ultrasonic of supersonic wave cleaning machine Qingdao Vista electric purification equipment Co., Ltd production
Cleaning machine.
3. a kind of method for extracting hexogen in solid cloud detonator according to claim 1, it is characterised in that the step
(5) in, 45-65 DEG C of drying temperature, time 4-6h.
4. 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 following analysis step:
(1) K of each factor level is soughtiWith R value, KiFor factor the i-th horizontal coefficient to evaluation index and；R is very poor, R
=max { Ki}-min{Ki}；
(2) according to KiIt is worth and determines preferred levels, wherein water corresponding to the maximum value for more bigger more excellent selecting index respective column
It is flat；
(3) primary and secondary sequence is determined according to R value, wherein R value is bigger, and expression influence is bigger, and the smaller expression influence of R value is smaller, obtains
Best factor group technology.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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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 |
|---|
| Thin-layer chromatographic analysis for the separation of common explosives;Hansson,J.;《Explosivstoffe》;19631231;第1963卷(第11期);摘要 |
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