DE1645079A1 - Process for the production of polybutadienes, in particular for use in solid propellants - Google Patents
Process for the production of polybutadienes, in particular for use in solid propellantsInfo
- Publication number
- DE1645079A1 DE1645079A1 DE19661645079 DE1645079A DE1645079A1 DE 1645079 A1 DE1645079 A1 DE 1645079A1 DE 19661645079 DE19661645079 DE 19661645079 DE 1645079 A DE1645079 A DE 1645079A DE 1645079 A1 DE1645079 A1 DE 1645079A1
- Authority
- DE
- Germany
- Prior art keywords
- production
- polybutadienes
- solid propellants
- nitrate
- weight
- 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.)
- Pending
Links
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
- C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
- C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
Description
Varfahren zur Herstallung von Polybutadienen insbosondere zur Verwendung für Feststofftreibsätze Gegenstand der Erfindung ist uin Verfahren zur Herstellung van Polymerisaten aus oligomeren, reaktionhsfähigen Gruppen enthaltenden Butadienen durch Vornutzen mit Epoxydsn, die insbesondere Varwendung finden als Sinder oder Inhibitorschichtan für Festofftrsibsätze. stellt Die Verwelldung der genannten Kunstharze Für Faststoffrakaten insofern besondere, in der sonstigen Kunststofftachnik nicht auftretande Problems, da sinarseits die technologischen Endeigenschaften in einam relativ gro#en Temperaturbereich von atwa-40 bis+60°C optimels Warte annehmen müssen, endererseits die Aushärtung möglichst schonend in einem begrenzten Temperaturbereich und mit Hilfe von solchen Beschleunigern durchgeführt werden m13, daren Chemische Eigenschaften im Gesamtsysten nicht stören. Eine grö#ere Anzahl der bisher bekannten Herstellungsverfahren scheiden daher aus den vorgennten Gründen von vornherein aug. Bel-Varwendung w n polybutadienen als Binder fur Composits-Treibsätze oder als Inhibierungsschicht treten diese Schwisrigkeiten in besonderem Ma#e auf und schlie#t beispielzweise die Verwendung von aminen als Härter solcher Systeme aus. Varfahren for the production of polybutadienes in particular for use for solid propellants The invention relates to a process for production van polymers of oligomeric butadienes containing reactive groups by prior use with Epoxydsn, which are used in particular as Sinder or Inhibitor layer for solid fuel sets. represents the curling of the synthetic resins mentioned For Faststoffrakaten this is special, but not for other plastics technology Occurring problems, since the technological end properties are combined in one relatively large temperature range from atwa-40 to + 60 ° C optimally must accept, on the other hand, the curing as gently as possible in a limited temperature range and with the help of such accelerators can be carried out m13, daren chemical Do not interfere with properties in the overall system. A larger number of those known so far Manufacturing processes are therefore excluded from the outset for the reasons mentioned above. It can be used as a binder for composite propellants or as an inhibition layer these difficulties occur to a particular degree and close, for example the use of amines as hardeners for such systems.
Gemä# der vorliegenden Erfindung werden die erwähnten Schwierigksiten bei der Herstallung von Polymerisaten aus oligomeren, reaktionsfähigen Gruppen enthaltenden Sute@@ianen durch Varnetzen mit Epoxyden dadurch Varmisden, da# als Häreter bis zu 3% vorzugsweise bis zu 1,5% eines Berium-, Calcium-, Blei-, Nickel-oder Zinitrats verwendet wird. Der Einflu# dieser Härter macht aich einerseite dadurch bemerkbar, daß die Härtezeiten verringert und die Temperaturen herabgesetzt werden. Die technologischen Eigenschaften der Endprodukte, insbesondere Zugfestigkeit und Elastizitätsmodul werden innerhalb eines großen Temperaturbereichs wesentlich verbessert.According to the present invention, the aforementioned difficulties become in the production of polymers from oligomeric, reactive groups containing Sute @@ ianen by varnetting with epoxies thereby Varmisden, because # as hardener up up to 3%, preferably up to 1.5%, of a berium, calcium, lead, nickel or zinc nitrate is used. The influence of these hardeners makes one thing through this it is noticeable that the hardening times are reduced and the temperatures are lowered. The technological properties of the final products, in particular tensile strength and The modulus of elasticity is significantly improved over a wide temperature range.
Wie weiterhin festgestellt wurde, kann es zweckmäßig sein, Gemische der genannten Nitrate zu verwenden, da die einzelnen Verbindungen die technologischen Eigenschaften bzw. Härtezeit und Härtetemperatur verschieden stark beeinflussen.As has also been stated, it can be useful to use mixtures to use the nitrates mentioned, since the individual compounds the technological Influence properties or hardening time and hardening temperature to different degrees.
Es war überraschend, dan optimale Verbesserungen schon mit so geringen Mengen, wie bis zu 3% der erfindungsgemäßen Härter srzielt werden, im allgemeineri sind schon bis zu 1,5% ausreichend. Die Nitrate, die vorzugsweise als kristaliwasserhaltige Falze verwendet werden, haben weder bei der Verwendung als Binder für Composite-Treibsätze noch bei der Verwandung als Inhibitorschichten eine nachteilige Wirkung, zeigen aber zusätzlich beim Abbrand den Vorteil verminderter Rauchbildung.It was surprising to see optimal improvements even with such minor ones Quantities such as up to 3% of the hardeners according to the invention are generally achieved up to 1.5% are sufficient. The nitrates, which are preferably used as crystalline water-containing Seams are used neither when used as a binder for composite propellants show an adverse effect even when used as inhibitor layers but also the advantage of reduced smoke formation when burning.
Die folgenden Beispiele beschreiben die erfindungsgemäße Arbeitsweise und zeigen die erreichten Verbesserungen und Vorteile, ohne Jedoch ihre Ausführung oder ihren Einsatzbereich einzuschränken. So kennen gemäß der Erfindung ganz allgemein gummielastische Massen hergestellt werden, fUr die ähnliche Herstellungs-Qualitätaforderungen zu stellen sind, wie im vorgenannten Fall.The following examples describe the procedure according to the invention and show the improvements and advantages achieved, but without their implementation or to limit their area of application. So know according to the invention in general Rubber-elastic masses are produced for the similar production quality requirements are to be provided, as in the aforementioned case.
Beispiel 1: rn sine bei 65° C eine Stunde im Vakuum (15 mm Hg) entgast8 Grundmischung aus 920 Gew.Teilen oligomeres Butadien mit reaktionsfähigen carboxylgruppen (Butarez CTL II der Fa. Phillips Petroleum Comp. mit 1,6 - 1,9 Gew. % Carhoxylgehalt) und Eo Gew. Teilen eines Epoxydherzes (Epikot8 162 der Fa. Shell, Kondensationsprodukt aus 1-Mol Pentaerythrit und 3 Molen Epichlorhydrin) wurde Calciumnitrat Ca(N03)2 2 4H2O in Mengen von 0 bis 4,5% eingerührt und gelöst.Example 1: rn sine degassed at 65 ° C for one hour in a vacuum (15 mm Hg )8 Basic mixture of 920 parts by weight of oligomeric butadiene with reactive carboxyl groups (Butarez CTL II from Phillips Petroleum Comp. With 1.6-1.9% by weight carhoxyl content) and Eo parts by weight of an epoxy heart (Epikot8 162 from Shell, condensation product 1 mole of pentaerythritol and 3 moles of epichlorohydrin) became calcium nitrate Ca (NO3) 2 Stir in and dissolve 2 4H2O in amounts of 0 to 4.5%.
Alie Proben wurden nach neuerlichem Entgasen 6 Tage bei 80° ausgehärtet und anschließend die mechanisch-physikalischen Werte bestimmt. Wie aus Fig. 1 ersichtlich, werden die besten technologischen Endeigenschaften bei einem Zusatz bis zu etwa 2$ Calciumnitrat erreicht.All samples were cured for 6 days at 80 ° after renewed degassing and then the mechanical-physical values are determined. As can be seen from Fig. 1, become the best final technological properties with an addition of up to about Reached $ 2 calcium nitrate.
Beispiel 2: Einer Feststofftreibsatz-Masse folgender Grundzusammensetzung: 18 Gew. Teils Binder gemä# Beispiel 1, 78 Gew. Teile Ammonimperchlorst, 4 Gew, Teile ballistische Additive und Gleitmittel wurden 0,15 bis 1,7 Gew.-% Cauf Bindern bezogen) Calciumnitrat Ca(NO3)2. 4H2O zugesetzt und in der bei Composits-Massen üblichen Arbeitsweiss zu Formlingen Vergossen. Nach Aushärtung während 6 Tagen bei 800 wurden dis machanisch-physikalischen Eigenschaften bei + 50°, + 20°, -20° und - 400 Bestimmt (sieche Fig. 2 bis 4).Example 2: A solid propellant mass of the following basic composition: 18 parts by weight of the binder according to Example 1, 78 parts by weight of ammonium perchlorate, 4 parts by weight ballistic additives and lubricants were 0.15 to 1.7% by weight C based on binders) Calcium nitrate Ca (NO3) 2. 4H2O added and in the usual way for composites Working white potted to moldings. After curing for 6 days at 800 dis mechanical-physical properties at + 50 °, + 20 °, -20 ° and - 400 Determined (See Figures 2-4).
Die Zugfestigkeit z.B. wird bei + 200 durch Zusatz von 0,9% Calciumnitrat auf 8,5 kp/cm2 erhöht (Ausgengswet 9,8 kp/cm2).The tensile strength, for example, is increased at + 200 by adding 0.9% calcium nitrate increased to 8.5 kp / cm2 (Ausgengswet 9.8 kp / cm2).
Beispiel 3..Example 3 ..
In die Grundmischung gemä# Beispiel 1 wurden wechselnde Mengen Nickelnitrat Ni (NO3)2 . 6H2O eingearbeitet1 Gehärtet wurde untsr gleichen Bedingungen wie im Beispiel 1. Bei Zusatz von 1% Nickeloxyd steigt die Zugfestigkeit von 4,8 kp/cm2 auf 8,9 kp.cm2.In the basic mixture according to Example 1, varying amounts of nickel nitrate were added Ni (NO3) 2. 6H2O incorporated1 Hardening took place under the same conditions as in Example 1. With the addition of 1% nickel oxide, the tensile strength increases by 4.8 kp / cm2 to 8.9 kp.cm2.
Beispiel 41 In eine Grundmischung gemä# Beispiel 1 wurden 1% Bariumnitrat Ba (NO3)2 und im anderen Falle 1% 8leinitrat Pb (NO3)2 eingearbeitet und wie üblich bei 800 ausgehärtet. Nach 60 Stunden war die Aushärtung beendet, wätirend bei nitratfreien Proben 130 Stunden für den gleichen Aushärtungsgred benötigt wurden.Example 41 1% barium nitrate was added to a basic mixture according to Example 1 Ba (NO3) 2 and in the other case 1% 8lein nitrate Pb (NO3) 2 incorporated and as usual cured at 800. After 60 hours, the curing was complete, while nitrate-free Samples took 130 hours for the same curing ingredient.
Claims (3)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEN0029411 | 1966-10-27 |
Publications (1)
Publication Number | Publication Date |
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DE1645079A1 true DE1645079A1 (en) | 1972-07-27 |
Family
ID=7345082
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19661645079 Pending DE1645079A1 (en) | 1966-10-27 | 1966-10-27 | Process for the production of polybutadienes, in particular for use in solid propellants |
Country Status (1)
Country | Link |
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DE (1) | DE1645079A1 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2510130A1 (en) * | 1981-07-08 | 1983-01-28 | Ppg Industries Inc | COATING COMPOSITIONS CONTAINING A CATALYST PARTICULARLY FOR THE REFECTION OF MOTOR VEHICLES |
EP0169066A1 (en) * | 1984-07-18 | 1986-01-22 | Minnesota Mining And Manufacturing Company | Fast curing expoxy resin compositions |
US4668736A (en) * | 1984-07-18 | 1987-05-26 | Minnesota Mining And Manufacturing Company | Fast curing epoxy resin compositions |
US4704331A (en) * | 1984-07-18 | 1987-11-03 | Minnesota Mining And Manufacturing Company | Method for adhering surfaces using fast curing epoxy resin compositions |
-
1966
- 1966-10-27 DE DE19661645079 patent/DE1645079A1/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2510130A1 (en) * | 1981-07-08 | 1983-01-28 | Ppg Industries Inc | COATING COMPOSITIONS CONTAINING A CATALYST PARTICULARLY FOR THE REFECTION OF MOTOR VEHICLES |
EP0169066A1 (en) * | 1984-07-18 | 1986-01-22 | Minnesota Mining And Manufacturing Company | Fast curing expoxy resin compositions |
US4668736A (en) * | 1984-07-18 | 1987-05-26 | Minnesota Mining And Manufacturing Company | Fast curing epoxy resin compositions |
US4704331A (en) * | 1984-07-18 | 1987-11-03 | Minnesota Mining And Manufacturing Company | Method for adhering surfaces using fast curing epoxy resin compositions |
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