EP1652574A2 - Verfahren und Vorrichtung zur Herstellung einer Komposit-Treibstoffpaste - Google Patents

Verfahren und Vorrichtung zur Herstellung einer Komposit-Treibstoffpaste Download PDF

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Publication number
EP1652574A2
EP1652574A2 EP05292264A EP05292264A EP1652574A2 EP 1652574 A2 EP1652574 A2 EP 1652574A2 EP 05292264 A EP05292264 A EP 05292264A EP 05292264 A EP05292264 A EP 05292264A EP 1652574 A2 EP1652574 A2 EP 1652574A2
Authority
EP
European Patent Office
Prior art keywords
fraction
extracted
paste
kneader
kneaded
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP05292264A
Other languages
English (en)
French (fr)
Other versions
EP1652574A3 (de
Inventor
Marie Gaudre
Christine Marraud
Eric Giraud
Eric Marchand
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eurenco SA
Safran Ceramics SA
Original Assignee
Eurenco SA
SNPE Materiaux Energetiques SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Eurenco SA, SNPE Materiaux Energetiques SA filed Critical Eurenco SA
Publication of EP1652574A2 publication Critical patent/EP1652574A2/de
Publication of EP1652574A3 publication Critical patent/EP1652574A3/de
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/57—Mixing high-viscosity liquids with solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/53—Mixing liquids with solids using driven stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle
    • B01F25/53—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle in which the mixture is discharged from and reintroduced into a receptacle through a recirculation tube, into which an additional component is introduced
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F2035/99—Heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0472—Numerical temperature values

Definitions

  • the subject of the present invention is a process for preparing a composite propellant paste and a device that is suitable for carrying out said method.
  • the method and device are improvements to the existing method and device to date.
  • the invention finds particular application in the field of the manufacture of solid propellant loadings for space launcher, strategic and / or tactical.
  • a composite type solid propellant comprises a solid polymeric matrix or binder, powdery solid fillers (oxidizing, optionally reducing and / or energetic) and various additives.
  • the binder is prepared from a liquid resin, having chemically reactive terminations, capable of being crosslinked by at least one also liquid crosslinking agent.
  • the various ingredients of the propellant and the crosslinking agent are introduced into the liquid resin in an appropriate order.
  • the resin by hardening (by crosslinking) by baking at a temperature compatible with the presence of pyrotechnic materials, coats all the ingredients and in particular the powdery fillers to form a solid body.
  • the process currently used to manufacture blocks of such propellants is a batch process, called "batch", consisting of preparing a quantity of product in several kneaded and poured in one or more loads.
  • a first step the various ingredients are introduced into a kneader in a proper order and carefully and long kneaded, under pressure conditions (usually vacuum) and very precise temperature.
  • the mixture which is in the form of a highly viscous paste is poured into a mold, with shaping tools. The whole is baked to ensure the hardening of the dough.
  • the mold is in some cases the same envelope of the propellant, envelope that is properly prepared for carrying out the loading.
  • the mixing phase of highly viscous paste is essential for the quality of the finished product. It is a long and expensive phase by the immobilized material and the consumed energy.
  • a first problem to be solved is to develop a composite propellant paste mixing process, in which the mixing time is reduced without altering the quality of the finished product.
  • Another problem to be solved is to be able to use, if necessary, sensitive charges (for example charges that could to react very violently, to detonate, for low stresses (very low drop height (a few cm), low friction)) without substantial modification of the kneading process, and therefore without increasing cost and risk.
  • sensitive charges for example charges that could to react very violently, to detonate, for low stresses (very low drop height (a few cm), low friction)
  • an improvement is proposed to the mixing phase of the process for preparing a composite propellant paste.
  • Said improvement is based on the implementation of a heat exchange on at least a fraction of the dough (being kneaded) put into external circulation.
  • the invention relates to a process for preparing a propellant paste based on a binder containing solid charges (composite propellant paste).
  • Said method in a conventional manner, comprises successively the introduction into a kneader of the constituent ingredients of said dough and then kneading, in said kneader, under conditions of adequate temperature and pressure, the dough constituted.
  • a fraction of the kneaded pulp (or even several fractions thereof) is (are) circulated, in a loop, outside the kneader and undergone (ssen) t an exchange at the level of this external circulation loop (of each of these external circulation loops).
  • ssen undergone
  • At least one fraction in this text means “one or more fractions” but does not cover the one-time extraction of all the pulp, the entire mixer. Of course, it is not excluded that, by fraction, the entire load of the mixer is concerned with the release.
  • a single dough fraction is removed, undergoes heat exchange and returns to the mixer, cooled or reheated.
  • the process of the invention can be used to prepare propellant pastes containing more or less sensitive powdery solid charges.
  • said process may comprise the introduction into the kneader of solid powder charges not or little sensitive and / or solid powdery solid charges phlegmatized with at least one phlegmatizing fluid.
  • phlegmatizing fluid in the sense of the prior art and the present invention a liquefied gas or, most often, an inert liquid, that is to say not reacting to the previously mentioned solicitations.
  • a sensitive or very sensitive charge is suspended in this liquid, it reacts much less to the stresses and can be handled with much less severe precautions.
  • This process of phlegmatization is known per se.
  • the phlegmatizing fluid is a liquid, this liquid must be a non-solvent for the powdery filler so as not to alter the particle size of said filler; it must also be preferentially non-toxic and non-flammable under the conditions of use.
  • a phlegmatizing fluid that may be used, mention may be made of CO 2 , N 2 , acetone, ethyl acetate and hydrofluoroethers.
  • the mass ratio between phlegmatizing fluid and sensitive powdery fillers is generally of the order of 75/25 to 25/75. Knowing that the propellant paste ready for casting may comprise from 65 to 80% by weight of sensitive powdery fillers, there is therefore in general a very large amount of phlegmatizing liquid to eliminate.
  • such a phlegmatizing fluid is generally removed before the charges are introduced into the mixer. It will be seen later that, in the context of the process of the invention, the phlegmatized charges can be introduced directly into the mixer, the phlegmatizing fluid being eliminated in said mixer.
  • At least a fraction of the kneaded paste is extracted from the kneader, reheated, and then re-introduced into said kneader.
  • this first variant - with heating - advantageously comprises the implementation of the heating (at least at the start of mixing) under temperature conditions in which the at least one phlegmatizing fluid is vaporized.
  • These temperature conditions are obviously to be optimized in view of the nature of the phlegmatizing fluid (s) in question and the possible presence of pyrotechnic materials. It is indicated, in no way limiting, that the at least one fraction of milled paste extracted is then advantageously heated to a temperature between 50 ° C and 95 ° C, very advantageously at a temperature between 55 and 80 ° C.
  • At least a fraction of the kneaded paste is extracted from the kneader, cooled, and then reintroduced into said kneader.
  • the at least one fraction of milled paste extracted can thus be cooled to a temperature between 55 ° C and 20 ° C, more generally at a temperature between 55 ° C and 40 ° C.
  • the method of the invention can be implemented firstly according to the first variant and in a second step according to the second variant.
  • the method of the invention does not pose any particular difficulty as to its implementation.
  • the parameters to be managed or even optimized are obviously, for an external circulation loop, the flow rate of the pulp concerned and the intensity of the heat exchange to be implemented. It may be mentioned here, incidentally, that the (the) fraction (s) of pulp is (are) advantageously taken (s), extracted (s), the lower part of the mixing tank, or even the bottom of said tank and reintroduced (s) in the upper part of said tank.
  • the reintroduction operation is generally carried out above the dough mass within the mixer.
  • the invention relates to a device suitable for implementing the method described above.
  • Said device is of the type of those of the prior art, it has been modified, to a lesser extent, to include at least one external circulation loop equipped with at least one heat exchanger.
  • the device of the invention adapted to the preparation of a propellant paste based on a binder containing powdery solid charges comprises a kneader including a kneading tank and means of mixing, means of thermoregulation and depressurization of said vessel and means for introducing the constituent ingredients of the dough, including means for introducing powdery solid charges.
  • said device is of the type of those of the prior art. Characteristically, it comprises in addition at least one external circulation loop equipped with circulation means and at least one heat exchanger. Each loop with its equipment must allow circulation with heat exchange of a fraction of the kneaded dough.
  • each of the outer circulation loops (equipping the outer circulation loop) are obviously adapted to the nature of the dough in question.
  • the circulation means of the pump type are more particularly adapted to the viscosity of said paste.
  • said means comprise a peristaltic pump.
  • the at least one heat exchanger is a static mixer of the jacketed type with forced circulation of heat transfer fluid against the current.
  • a static mixer not only ensures the heating or cooling of the circulating propellant paste, but also makes it possible to improve the homogenization of said paste before it is reintroduced into the mixer tank. This contributes to the good quality of the finished product.
  • the means for introducing powdery solid charges into the mixing tank can be arranged on the tank, independently of any external circulation loop. They are advantageously arranged to open into an external circulation loop, very advantageously arranged, in such a case, downstream of the heat exchanger (s).
  • the means of thermoregulation and depressurization make it possible to control the conditions of temperature and pressure within the kneader.
  • the depressurization means generally provide vacuum, within said mixer. They intervene in fact in the same way as they do in the devices of the prior art but are in addition capable of contributing to the elimination of the phlegmatizing fluid introduced into the mixer (according to the prior art, said fluid was eliminated off the mixer).
  • Said depressurization means is advantageously coupled to a condensing unit. Such a unit intervenes for the recovery of vaporized phlegmatized fluids, possibly introduced with the pulverulent solid charges.
  • the outer loop (s) is (are) advantageously arranged (s) to ensure a flow from a lower part of the tank, or even the bottom of said tank, to the top of said tank.
  • (the) said (s) loop (s) leads (nt) generally in the upper part, above the filling level provided for said vessel.
  • Figure 1 shows schematically an alternative embodiment of a device of the invention.
  • FIG. 2 represents the cooling rate of an inert propellant paste prepared according to the method of the invention.
  • FIG. 2 is to be considered with Comparative Examples 1a and 1b as well as Examples 2a and 2b of the invention, given below.
  • FIG. 1 there is shown in 1 a jacketed type of mixer in which circulates a heat transfer fluid that can be heated or cool at will, such as glycol water; at 10, the vessel of said mixer 1; at 12 and 12a, kneading means, more precisely vertical blades, secured to the cover of the kneader 1 and driven by a motor 11; at 14, thermoregulation means able to control the temperature of the tank 10; at 16, depressurization means able to control the pressure (vacuum or low pressure) of said tank 10.
  • a condensation unit 17 is coupled capable of allowing the recovery of a phlegmatizing fluid, in the hypothesis where such a phlegmatizing fluid intervenes.
  • the tank 10 of the kneader 1 is associated with an external circulation loop 20 equipped with circulation means, a pump 22, and a heat exchanger 30.
  • the temperature of the coolant circulating in said heat exchanger 30, is regulated via the thermal group 32.
  • the outer circulation loop 20 has at its reintroduction mouth a tube 24 equipped with a grid 26.
  • a grid 26 is advantageously used to prevent the entry of foreign bodies and to promote the degassing of the reintroduced paste, by sharing the flow of said dough in thin threads.
  • a hopper for the introduction of powdery solid charges.
  • Said hopper 18 opens into the circulation loop 20, downstream of the heat exchanger 30.
  • the open mixer 1, the liquid binder, the reducing charges (for example aluminum powder), the various additives except the crosslinking agent and the crosslinking catalyst, and the oxidizing charges are introduced beforehand into the tank 10. for example ammonium perchlorate.
  • the kneader 1 is closed and the ingredients are mixed and heated to about 70 ° C (for this purpose, the coolant of the tank is heated to about 80 ° C); vacuuming (or low pressure) allows the mixture to be degassed.
  • the powdery oxidizing charge is introduced via the hopper 18: the heating makes it possible to compensate for the increase in viscosity due to the introduction of the pulverulent fillers.
  • the kneading and homogenization of the dough is then continued (it is generally intended to bring said homogenized dough to a temperature between 20 ° C. and 80 ° C., preferably between 50 ° C. and 65 ° C.).
  • Said paste is then cooled (for this purpose, the coolant of the tank is heated to about 30 ° C), to the casting temperature, about 50 ° C.
  • the crosslinking agent and the crosslinking catalyst are then introduced, still through the hopper 18, before casting after a last homogenization sequence.
  • the temperature of the tank 10 of the kneader 1 is controlled by the means 14; the pressure by the depressurization system 16.
  • At least one of the above heating and cooling steps is improved by extracting a flow of dough from the bottom of the vessel 1, circulating it in the loop 20 with heating or cooling (effective) at the heat exchanger 30 and reintroducing it, warmed or cooled, in the upper part of the tank 1 (above the level of the dough body surface).
  • the reheating in question may be a simple reheating or may also help to effectively extract a phlegmatizing fluid introduced with phlegmatized sensitive powdery solid charges.
  • Comparative Examples 1a and 1b Cooling according to a conventional method
  • the inert propellant paste obtained above is cooled in the mixer by circulation of coolant at 40 ° C in the jacket of the tank of the kneader.
  • the tank is under vacuum (about 5 mm Hg), and the speed of rotation of the blades is 5 rpm.
  • the temperature of the dough at the bottom of the tank is measured during the cooling step.
  • the cooling of the propellant paste takes place over 12 minutes (eg Comp. and the cooling from 70 ° C. to 55 ° C. is carried out in 13 to 14 minutes (eg Comp 1b).
  • the same propellant paste as that prepared above is cooled according to the method of the invention.
  • the operating conditions of the kneader are identical to those of the two preceding comparative examples. But, for the cooling phase, the propellant paste is taken at the bottom of the tank via a peristaltic pump, passes into a heat exchanger and is reinjected into the mixer tank according to the diagram shown in Figure 1; for these tests, the device comprises a single external circuit.
  • the peristaltic pump is a pump type ABAQUE ALO type, whose flow varies between 250 kg / h and 150 kg / h depending on the increasing viscosity of the dough when it cools and its temperature decreases about 70 ° C at about 45 ° C.
  • the heat exchanger consists of a SULZER static mixer type SMXL 30 mm in diameter and 800 mm in length; it comprises a double wall with circulation of a heat transfer fluid at 30 ° C for Example 2a and at 20 ° C for Example 2b.
  • the temperature of the propellant paste is measured at the bottom of the tank during the cooling step. For two separate kneaded kneads, the results are shown in Table 2 and shown in Figure 2. ⁇ u> Table 2 ⁇ / u> T initial dough Heat transfer fluid exchanger V cooling Ex. 2a 66 ° C 30 ° C 1.75 ° C / min Ex. 2b 69 ° C 20 ° C 3 ° C / min
  • the implementation of the method of the invention allows to cool the propellant paste from 66 ° C to 55 ° C in about 6 min. (Ex 2a), and 69 ° C to 55 ° C in 5 min (Ex 2b).
  • the cooling rate is thus doubled (eg 2a v. Ex .: Comp 1a) or tripled (eg 2b v. Ex Comp 1b).
  • a sensitive charge (hexogen) is phlegmatized by mixing 1.5 kg of said sensitive charge with 4.5 kg of a liquid hydrofluoroether, marketed under the name HFE 7100 by the company 3M.
  • HFE 7100 The boiling point of HFE 7100 is 61 ° C at atmospheric pressure; moreover, this product is neither carcinogenic nor mutagenic and is not harmful for reproduction (non-CMR). Finally it is not flammable in these conditions of use.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
EP05292264A 2004-11-02 2005-10-26 Verfahren und Vorrichtung zur Herstellung einer Komposit-Treibstoffpaste Withdrawn EP1652574A3 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR0411638A FR2877333B1 (fr) 2004-11-02 2004-11-02 Procede et dispositif de preparation d'une pate de propergol de type composite

Publications (2)

Publication Number Publication Date
EP1652574A2 true EP1652574A2 (de) 2006-05-03
EP1652574A3 EP1652574A3 (de) 2010-12-01

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Application Number Title Priority Date Filing Date
EP05292264A Withdrawn EP1652574A3 (de) 2004-11-02 2005-10-26 Verfahren und Vorrichtung zur Herstellung einer Komposit-Treibstoffpaste

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EP (1) EP1652574A3 (de)
FR (1) FR2877333B1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108295718A (zh) * 2018-03-13 2018-07-20 无锡市锡东橡塑机械有限公司 一种碱液配液箱装置

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1333015A2 (de) 2002-02-01 2003-08-06 Snpe Semikontinuierliches Verfahren zur Herstellung einer explosiven Komposit-Ladung mit einer Polyurethanmatrix durch Verwendung von zwei Komponenten

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Publication number Priority date Publication date Assignee Title
US2353991A (en) * 1941-09-02 1944-07-18 Clarence E Boutwell Process for forming plastic solutions and incorporating solid filling material therein
US3561047A (en) * 1968-03-04 1971-02-09 Stirling A Mcinnis Plastic mixing and injection system
US4251627A (en) * 1978-05-30 1981-02-17 E. I. Du Pont De Nemours And Company Jet mixing in preparation of monodisperse silver halide emulsions
DE3838251C1 (de) * 1988-11-11 1990-03-08 Kloeckner Ferromatik Desma Gmbh, 7831 Malterdingen, De
JP4177103B2 (ja) * 2000-12-07 2008-11-05 イーストマン ケミカル カンパニー 管型反応器を使用する低コストポリエステルの製造方法
DE10320739B3 (de) * 2003-05-09 2004-10-21 Ika - Werke Gmbh & Co. Kg Vorrichtung zum Dispergieren und/oder Homogenisieren

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1333015A2 (de) 2002-02-01 2003-08-06 Snpe Semikontinuierliches Verfahren zur Herstellung einer explosiven Komposit-Ladung mit einer Polyurethanmatrix durch Verwendung von zwei Komponenten

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"DAVENAS", 1989, article "Technologie des propergols solides"

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108295718A (zh) * 2018-03-13 2018-07-20 无锡市锡东橡塑机械有限公司 一种碱液配液箱装置

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Publication number Publication date
EP1652574A3 (de) 2010-12-01
FR2877333B1 (fr) 2007-09-07
FR2877333A1 (fr) 2006-05-05

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