CN109289249A - The recovery method of plasticizer and stabilization agent in a kind of high-energy propellant - Google Patents
The recovery method of plasticizer and stabilization agent in a kind of high-energy propellant Download PDFInfo
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- CN109289249A CN109289249A CN201811498304.XA CN201811498304A CN109289249A CN 109289249 A CN109289249 A CN 109289249A CN 201811498304 A CN201811498304 A CN 201811498304A CN 109289249 A CN109289249 A CN 109289249A
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- Prior art keywords
- supercritical
- plasticizer
- propellant
- stabilization agent
- recycling
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- 239000003380 propellant Substances 0.000 title claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000004014 plasticizer Substances 0.000 title claims abstract description 23
- 230000006641 stabilisation Effects 0.000 title claims abstract description 22
- 238000011105 stabilization Methods 0.000 title claims abstract description 22
- 238000011084 recovery Methods 0.000 title claims abstract description 13
- 238000004064 recycling Methods 0.000 claims abstract description 18
- 239000004449 solid propellant Substances 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims description 21
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- SNIOPGDIGTZGOP-UHFFFAOYSA-N Nitroglycerin Chemical compound [O-][N+](=O)OCC(O[N+]([O-])=O)CO[N+]([O-])=O SNIOPGDIGTZGOP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 229960003711 glyceryl trinitrate Drugs 0.000 claims description 4
- LYAGTVMJGHTIDH-UHFFFAOYSA-N diethylene glycol dinitrate Chemical compound [O-][N+](=O)OCCOCCO[N+]([O-])=O LYAGTVMJGHTIDH-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 3
- 230000007246 mechanism Effects 0.000 claims description 3
- VBEGHXKAFSLLGE-UHFFFAOYSA-N n-phenylnitramide Chemical compound [O-][N+](=O)NC1=CC=CC=C1 VBEGHXKAFSLLGE-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- AGCQZYRSTIRJFM-UHFFFAOYSA-N triethylene glycol dinitrate Chemical compound [O-][N+](=O)OCCOCCOCCO[N+]([O-])=O AGCQZYRSTIRJFM-UHFFFAOYSA-N 0.000 claims description 3
- 150000001448 anilines Chemical group 0.000 claims description 2
- 239000002360 explosive Substances 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 8
- 239000002351 wastewater Substances 0.000 abstract description 7
- 239000002904 solvent Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 229920001220 nitrocellulos Polymers 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RDLIBIDNLZPAQD-UHFFFAOYSA-N 1,2,4-butanetriol trinitrate Chemical compound [O-][N+](=O)OCCC(O[N+]([O-])=O)CO[N+]([O-])=O RDLIBIDNLZPAQD-UHFFFAOYSA-N 0.000 description 2
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 description 2
- 239000000028 HMX Substances 0.000 description 2
- 229920002121 Hydroxyl-terminated polybutadiene Polymers 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000011978 dissolution method Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- UZGLIIJVICEWHF-UHFFFAOYSA-N octogen Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)CN([N+]([O-])=O)C1 UZGLIIJVICEWHF-UHFFFAOYSA-N 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- -1 nitrate ester Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/80—Destroying solid waste or transforming solid waste into something useful or harmless involving an extraction step
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/20—Waste processing or separation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to the recovery methods of plasticizer and stabilization agent in a kind of high-energy propellant, using supercritical CO2As solvent, the safe and efficient recycling of plasticizer, stabilization agent component in high-energy propellant is realized.The present invention uses CO2Secondary pollution is not generated as extractant, recycling component is not necessarily to complicated last handling process, and simple process is easy to implement, and is very suitable to scrap the recycling of active principle in the dangerous explosive wastewater waste such as solid propellant.
Description
Technical field
The present invention relates to the recovery methods of plasticizer and stabilization agent in a kind of high-energy propellant, are specifically faced using super
Boundary carbon dioxide (CO2) it is safe and efficient handle discarded high-energy propellant, therefrom recycle active principle plasticizer and stabilization agent.
Background technique
Solid propellant occupies status of crucial importance in military field, and the power source that it is used as engine is remarkably improved
Weapon survival ability and operational exertion ability.Active service solid propellant is mostly high molecular material, such as double base propellant, complex solid
Propellant, composite double base propellant etc., these propellants all have after curing molding aging rapidly and are unable to lacking for long term storage
Point.Once exceeding storage period, if continuing to use the tactical qualities that can not only seriously affect guided missile, and safe thing may be led to
Therefore.Therefore, how effectively, safe and pollution-free ground mass disposal is expired or the solid propellant scrapped, be that various countries are paid much attention to
The problem of, and various discussions, research and practice are being carried out always.
Usually there are 3 kinds of ways in the world at present: first is that using conventional method, such as burning, explosion, recycling thermal energy;Second is that
The various recovery and utilization technologies of active development mainly have at present with certain main components and portions additive (such as AP, heisuojin
(RDX), octogen (HMX), aluminium (Al)) etc. centered on recovery technology with by properties of product and function conversion centered on return
Receipts technology (such as re-works and switchs to civilian explosive wastewater product, industrial chemicals);Third is that just in the design of novel solid propellant
Consider that its R3 (returns and receives/recirculate/huge profit use) characteristic and more meets green ring as the design object of novel propellant
Factoring is read.
Patent US3,451,789 by dissolution, extraction ammonium perchlorate in the aqueous solution of heat, then from obtained solution
Propellant is gradually handled by the solid residue after multistep separation extraction.It is disadvantageous in that in treatment process and forms solid
The aggregation of residue, energy consumption is high, reduces recovery efficiency.
Patent US4,854,982 recycles ammonium perchlorate using Liquid Ammonia Treatment propellant.It is disadvantageous in that liquefied ammonia has poison
Property, operating pressure is higher, and relative to cost of investment, and technology production capacity is lower.
Patent US4,909,868 uses near critical or supercritical CO2It is dissolved as solvent and separates biradical or be crosslinked biradical
Plasticizer (such as nitroglycerine) and its stabilizer (such as diphenylamines and nitroaniline) in propellant, CO2It can be followed by processing
Ring uses.
Chinese periodical " solid-rocket technology " the 6th phase in 2014 reports document, and " extracting RDX etc. from NC base propellant has
Imitate the design of ingredient ", the document is using pressurized, heated extraction method (PLE) to black rope in retired nitrocotton (NC) base solid propellant
Effective components such as modern (RDX) are recycled, and CH is used2Cl2Make extractant, extract and NC can be made to separate, extraction efficiency is high.
Chinese periodical " explosive wastewater journal " the 1st phase in 2016 reports document " in swelling/dissolution method recycling HTPB propellant
The experimental study of AP component ", the document use tetrahydrofuran/aqueous solution swelling/dissolution method, carry out to the AP in HTPB propellant
Leaching recycling, under specific process conditions, the AP rate of recovery is 95%, purity 96.1%.
Chinese periodical " explosive wastewater journal " the 1st phase in 2001 reports document and " handles composite solid with critical liquid abstraction technique
The technical study of body propellant ", the document describe the process using critical liquefied ammonia separating and extracting AP from propellant.
Chinese periodical " explosive wastewater journal " the 6th phase in 2013 reports document, and " waste and old B Explosives are in overcritical titanium dioxide
Dissolubility and its separating technology in carbon ", the document determine B Explosives TNT, RDX using High-pressure phase equilibria method and face super
Boundary CO2Solubility in fluid proposes the technique of supercritical technology separating waste, worn B explosive.
Document disclosed above reflects the state of the art for scrapping that active principle recycles in explosive wastewater.Generally using organic
Solvent swell/dissolution or supercritical fluid carry out the separating and extracting of component.It is recycled using organic solvents such as tetrahydrofuran, halogenated hydrocarbons
The components such as AP, RDX in propellant consume a large amount of toxic and volatile solvents;Use overcritical liquefied ammonia as solvent, liquefied ammonia has poison
Property, operating pressure is higher;Use supercritical CO2As solvent, be applied to double base propellant, in B explosive component recycling, with
Double base propellant, B explosive are compared, and high-energy solid propellant matrix is high polymer cross-linked structure, and component is more complicated, therefore super
Critical CO2Abstraction technique is not applied to the recycling of component in the high-energy propellant containing nitrate.
Summary of the invention
The technical problem to be solved in the present invention is to provide the recovery method of plasticizer and stabilization agent in a kind of high-energy propellant,
Active principle plasticizer and stabilization agent are therefrom recycled to solve the problem of to handle discarded high-energy propellant safe and efficiently.
To solve, the technical solution adopted by the present invention are as follows: in a kind of high-energy propellant plasticizer and
The recovery method of stabilization agent, using supercritical CO2The method of plasticizer, stabilization agent, specific to wrap in extraction, recycling high-energy propellant
Include following steps:
(1) equipment and preparation of samples
High-energy propellant is prepared into graininess, partial size is no more than 5mm, is placed in extraction kettle;By supercritical CO2Feeding mechanism,
Temperature, pressure control device, extraction kettle, recycling component collection device, CO2Recyclable device, using piping connection;
(2) supercritical extract
Supercritical CO is inputted into extraction kettle2It is extracted, supercritical CO2Pressure should be maintained within the scope of 10MPa ~ 30MPa, temperature
Degree should be maintained within the scope of 40 DEG C ~ 60 DEG C, and extraction time is 2h ~ 4h;
(3) it separates and collects
The supercritical CO of extract will be dissolved with2Enter separator through pressure reducing valve, reduces pressure, supercritical CO2Gasification, extract
Plasticizer, stabilization agent enter in collector;
(4) CO2Recycling
By gaseous state CO2It is re-compressed after drying, filtering, input extraction equipment is recycled.
Wherein, the high-energy propellant is the composite solidpropellant containing nitrate ester plasticizer, and the plasticizer is
Nitrate can be nitroglycerine (NG), 1,2,4-butanetriol trisnitrate (BTTN), triethylene glycol dinitrate
(TEGDN), one or more of diglycol dinitrate (DEGDN), the stabilization agent are phenyl amines, nitroaniline
Type organic.
The beneficial effects of the present invention are:
The present invention is characterized in that using supercritical CO2Instead of organic solvent, plasticizer, stabilization agent group in high-energy propellant are realized
The recycling divided.The advantage of the invention is that using CO2Secondary pollution is not generated as extractant, after recycling component is without complexity
Treatment process, simple process are easy to implement, and are very suitable to scrap active principle in the dangerous explosive wastewater waste such as solid propellant
Recycling.
Detailed description of the invention
Fig. 1 is supercritical CO2Recycle the process flow chart of plasticizer, stabilization agent in high-energy propellant.
Fig. 2 is the liquid chromatogram of high-energy propellant extract.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, but does not limit the present invention.
In the following embodiments, as shown in Fig. 1, using supercritical CO2It recycles and increases in certain representative formula high-energy propellant
Agent, stabilization agent are moulded, specific implementation step is as follows.
Step 1, equipment and preparation of samples.Propellant is prepared into the particle of partial size about 5mm, 20g sample is taken, is placed in capacity
For in the extraction kettle of 50mL.By supercritical CO2Feeding mechanism, temperature, pressure control device, extraction kettle, recycling Fraction collection dress
It sets, CO2Recyclable device, using piping connection.
Step 2, supercritical extract.CO is inputted into extraction kettle2, pressure is set as 20MPa, and temperature is 50 DEG C, extraction
2.5h。
Step 3, it separates and collects.The supercritical CO of extract will be dissolved with2Enter separator through pressure reducing valve, reduce pressure,
Supercritical CO2Gasification, extract plasticizer, stabilization agent enter in collector.
Step 4, CO2Recycling.By gaseous state CO2It is re-compressed after drying, filtering, input extraction equipment is recycled.
Fig. 2 is the liquid chromatogram of selected high-energy propellant extract.Four chromatographic peaks correspond respectively to two kinds in spectrogram
Plasticizer and two kinds of stabilization agents.
Calculate the extraction yield of four kinds of components, respectively plasticizer 1:95.4%;Plasticizer 2:91.8%;Stabilization agent 1:85.7%;
Stabilization agent 2:88.9%.
The above described is only a preferred embodiment of the present invention, not making any form to technical solution of the present invention
On limitation.According to the technical essence of the invention any simple modification to the above embodiments, equivalent variations and repair
Decorations, fall within the protection scope of the present invention.
Claims (3)
1. the recovery method of plasticizer and stabilization agent, specific steps in a kind of high-energy propellant are as follows:
Step 1, equipment and preparation of samples
High-energy propellant is prepared into graininess, partial size is no more than 5mm, is placed in extraction kettle;By supercritical CO2Feeding mechanism, temperature
Spend pressure control device, extraction kettle, recycling component collection device, CO2Recyclable device, using piping connection;
Step 2, supercritical extract
Supercritical CO is inputted into extraction kettle2It is extracted, supercritical CO2Pressure should be maintained within the scope of 10MPa ~ 30MPa, temperature
Degree should be maintained within the scope of 40 DEG C ~ 60 DEG C, and extraction time is 2h ~ 4h;
Step 3, it separates and collects
The supercritical CO of extract will be dissolved with2Enter separator through pressure reducing valve, reduces pressure, supercritical CO2Gasification, extract
Plasticizer, stabilization agent enter in collector;
Step 4, CO2Recycling
By gaseous state CO2It is re-compressed after drying, filtering, input extraction equipment is recycled.
2. recovery method according to claim 1, it is characterised in that: the high-energy propellant is to be plasticized containing nitrate
The composite solidpropellant of agent.
3. recovery method according to claim 1, it is characterised in that: the plasticizer is nitrate, is nitroglycerine, 1,
One or more of 2,4- butanetriol trinitrate, triethylene glycol dinitrate, diglycol dinitrate, institute
Stating stabilization agent is phenyl amines, nitroaniline type organic.
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CN201811498304.XA CN109289249A (en) | 2018-12-08 | 2018-12-08 | The recovery method of plasticizer and stabilization agent in a kind of high-energy propellant |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110452124A (en) * | 2019-06-13 | 2019-11-15 | 内蒙合成化工研究所 | A method of TCTNB explosive is purified using supercritical extract |
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