DE1795396A1 - Process for removing volatile components from finely divided olefin polymers - Google Patents

Process for removing volatile components from finely divided olefin polymers

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Publication number
DE1795396A1
DE1795396A1 DE19681795396 DE1795396A DE1795396A1 DE 1795396 A1 DE1795396 A1 DE 1795396A1 DE 19681795396 DE19681795396 DE 19681795396 DE 1795396 A DE1795396 A DE 1795396A DE 1795396 A1 DE1795396 A1 DE 1795396A1
Authority
DE
Germany
Prior art keywords
finely divided
particles
olefin polymers
removing volatile
volatile components
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.)
Granted
Application number
DE19681795396
Other languages
German (de)
Other versions
DE1795396C3 (en
DE1795396B2 (en
Inventor
Richard Scholl
Hans-Georg Prof Dr Trieschmann
Karl Dr Wisseroth
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Priority to DE19681795396 priority Critical patent/DE1795396C3/en
Priority to FR6930909A priority patent/FR2022197A1/fr
Priority to AT877069A priority patent/AT296601B/en
Priority to BE738973D priority patent/BE738973A/xx
Priority to NL6914421A priority patent/NL6914421A/xx
Priority to GB4715069A priority patent/GB1272778A/en
Publication of DE1795396A1 publication Critical patent/DE1795396A1/en
Publication of DE1795396B2 publication Critical patent/DE1795396B2/en
Application granted granted Critical
Publication of DE1795396C3 publication Critical patent/DE1795396C3/en
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00—Post-polymerisation treatments
    • C08F6/26—Treatment of polymers prepared in bulk also solid polymers or polymer melts
    • C08F6/28—Purification

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Description

Verfahren zum Entfernen flüchtiger Bestandteile aus feinteiligenProcess for removing volatile constituents from finely divided

Olefinpolymerisaten .Olefin polymers.

Gegenstand der Erfindung ist ein Verfahren zum Entfernen flüchtiger Bestandteile aus Olefinpolymerisaten, bei dem die feinteiligen Polymerisate mit Inertgasen behandelt werden.The invention relates to a method for removing volatile Components made from olefin polymers, in which the finely divided polymers are treated with inert gases.

Feinteilige Olefinpolymerisate, die durch Polymerisation der Monomeren, z. B. von Äthylen oder Propylen in Abwesenheit von Losungsoder Verdünnungsmitteln hergestellt worden waren, enthalten im allgemeinen geringe Mengen niedermolekulare Verbindungen. Diese Verbindungen haben mitunter einen starken Geruch, so daß bei der Verarbeitung der Produkte Geruchsbelästigungen auftreten können, auch macht sich dieser Geruch selbst nach Verarbeitung der Polymerisate zu Formteilen bemerkbar.Finely divided olefin polymers obtained by polymerizing the monomers, e.g. B. of ethylene or propylene in the absence of solution or Diluents prepared generally contain small amounts of low molecular weight compounds. These Compounds sometimes have a strong odor, so that unpleasant odors can occur when processing the products, this odor is also produced after the polymers have been processed noticeable to molded parts.

Es wurde nun gefunden, daß man flüchtige Bestandteile aus feinteiligen Olefinpolymerisaten vorteilhaft entfernen kann, wenn man die Polymerisate, deren Teilchen einen durchschnittlichen Durchmesser von 100 bis 1 000 Ai haben, mit einem Inertgasstrom bei einer zwischen -f- 80 ° C und mindestens 5 ° C unter dem Kristallitschmelz-It has now been found that volatile constituents can advantageously be removed from finely divided olefin polymers if the polymers, the particles of which have an average diameter of 100 to 1000 Ai , are used with an inert gas stream at between -f- 80.degree. C. and at least 5.degree C under the crystallite melting

617/66617/66

109882/1557109882/1557

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T795396T795396

punkt liegenden Temperatur in einer Behandlungszone durchspült.rinsed temperature in a treatment zone.

Das Verfahren eignet sich insbesondere zum Entfernen flüchtiger Bestandteile aus Olefinpolymerisaten, die nach dem Verfahren der Gasphasenpolymerisation, also durch Polymerisation der Monomeren in Abwesenheit von Lösungs- bzw. Verdünnungsmitteln erhalten wurden. Besonders vorteilhafte Ergebnisse werden mit Äthylen- oder Propylen-Homopolymerisaten, Copolymerisaten dieser Verbindungen untereinander, bzw. mit Copolymerisaten des Äthylens und Propylene mit Buten-1 erzielt. Die Vorteile treten in der Regel unabhängig von der Art des bei der Polymerisation der Polymerisate verwendeten Katalysators in Erscheinung.The method is particularly suitable for removing volatile Components made from olefin polymers, which are produced by the process of Gas phase polymerization, that is, by polymerization of the monomers in the absence of solvents or diluents. Particularly advantageous results are obtained with ethylene or propylene homopolymers and copolymers of these compounds with one another or with copolymers of ethylene and propylene achieved with butene-1. The benefits usually occur independently on the type of used in the polymerization of the polymers Catalyst in appearance.

Die Teilchen, die erfindungsgemäß behandelt werden sollen, haben einen Durchmesser im Bereich von etwa 10 bis etwa 5 000/U, vorteilhaft zwischen 100 und 1 000/U. Die Teilchen werden mit einem Inertgasstrom behandelt, dessen Temperatur zwischen 80 ° C und einer mindestens 5 ° C unter dem Kristallitschmelzpunkt des Polymerisates liegenden Temperatur liegt. Von den inerten Gasen eignen sich insbesondere Stickstoff, Kohlendioxid oder Wasserdampf für das Verfahren.The particles to be treated according to the invention have a diameter in the range from about 10 to about 5,000 / rev is advantageous between 100 and 1,000 / rev. The particles are exposed to a stream of inert gas treated, its temperature between 80 ° C and one at least 5 ° C below the crystallite melting point of the polymer lying temperature. Of the inert gases, nitrogen, carbon dioxide or water vapor are particularly suitable for the procedure.

Die Geschwindigkeit des Inertgasstromes soll so groß sein, daß die Polymerisatteilchen in der Behandlungszone bewegt werden. Dies ist in der Regel der Fall, wenn die auf den freien Querschnitt einer Schützung der beschriebenen Teilchen bezogene Gasgeschwindigkeit etwa 5 bis 20 cm/sec beträgt. Die Behandlung der Teilchen wird vorteilhaft in einer Behandlungszone vorgenommen, deren Längsausdeh-The speed of the inert gas flow should be so great that the Polymer particles are moved in the treatment zone. This is usually the case when the gas velocity related to the free cross-section of a protection of the particles described is about 5 to 20 cm / sec. The treatment of the particles becomes advantageous carried out in a treatment zone, the longitudinal extent of which

- 3 -109882/1557- 3 -109882/1557

-.--.. ->,Λ' / - 3 - 0..Z-. 25 805-.-- .. ->, Λ '/ - 3 - 0..Z-. 25 805

nung das 1- bis 20-fache der Querausdehnung beträgt. Unter Querausdehnung soll der Durchmesser eines Kreises verstanden werden, der der Querschnittsfläche der Behandlungszone entspricht. So können z. B. die Teilchen auch mittels eines Inertgasstromes durch eine Rohrleitung bewegt werden. Diese Behandlung kann z. B. während des Transportes der Teilchen von der Produktion zur Verpakkungsanlage erfolgen. Besonders vorteilhaft ist die Behandlung der Teilchen im Wirbelbett.voltage is 1 to 20 times the transverse dimension. Under transverse expansion should the diameter of a circle be understood, which corresponds to the cross-sectional area of the treatment zone. So can e.g. B. the particles through by means of a stream of inert gas a pipeline can be moved. This treatment can e.g. B. during the transport of the particles from production to the packaging plant take place. The treatment is particularly beneficial of the particles in the fluidized bed.

Die Teilchen werden mindestens für die Dauer von 1 bis 5· Minuten mit Inertgas umspült. In den meisten Fällen ist es nicht erforderlich, die Teilchen länger als 10 bis 20 Minuten mit Inertgas zu behandeln. Besonders vorteilhaft arbeitet man in einem Zeitraum von 5 bis 15 Minuten. Diese Angaben beziehen sich auf die vorstehend genannten Temperaturen in der Behandlungszone.The particles will remain for at least 1 to 5 minutes flushed with inert gas. In most cases it is not necessary to soak the particles with inert gas for more than 10 to 20 minutes treat. It is particularly advantageous to work within a period of 5 to 15 minutes. These details relate to the above mentioned temperatures in the treatment zone.

Eine vorteilhafte Vorrichtung zur Durchführung des erfindungsgemäßen Verfahrens ist in der Figur dargestellt» Über ein Steigrohr An advantageous device for carrying out the method according to the invention is shown in the figure “Via a riser pipe

(1) wird das feinteilige Polymerisat (2) duith das Ventil (3) in einen Cyklon (4) gefördert. Durch das Ventil (5) tritt ein Inertgasstrom (6) in den Cyklon ein. Der Inertgasstrom (6) durchstreicht die Polymerisatteilchen (2) und tritt durch Rohrleitung (7) aus dem Cyklon aus. Das Ventil (3) wird kurzzeitig und intervallweise, z. B. alle zwei Minuten, geöffnet. Solange Ventil (3) geöffnet ist, sind die Ventile (5) und (8) geschlossen. Nach dem Schließen von Ventil (3) wird Ventil (5) geöffnet. Die Polymerisatteilchen(1) the finely divided polymer (2) duith the valve (3) in a cyclone (4) promoted. A stream of inert gas passes through the valve (5) (6) into the cyclone. The inert gas stream (6) sweeps through the polymer particles (2) and exits through pipe (7) the cyclone. The valve (3) is briefly and at intervals, z. B. every two minutes. As long as valve (3) is open is, the valves (5) and (8) are closed. After closing valve (3) opens valve (5). The polymer particles

(2) sammeln sich nach einer bestimmten mittleren Verweilzeit im Fallrohr (9) an. Das behandelte Polymerisat kann über Ventil (8)(2) accumulate in the Downpipe (9). The treated polymer can be discharged via valve (8)

- 4 -109882/1557- 4 -109882/1557

. - 4 - O.Z. 25 805. - 4 - O.Z. 25 805

179539g179539g

aus dem Fallrohr (9) entnommen werden.can be removed from the downpipe (9).

In den erfindungsgemäß behandelten Polymerisatteilchen ist der Gehalt an flüchtigen Bestandteilen so weit reduziert, daß Geruchsbelästigungen bei der Verarbeitung der Teilchen nicht r&ehr auftreten. Es zeigte sich außerdem, daß die Teilchen beim Behandeln mit heißen Inertgasen eine Struktur erhalten, die ein besseres Rieseln der Teilchen bewirkt. Aufgrund der besseren Rieselfähigkeit können die Teilchen leichter in den für die Kunststoffverarbeitung, gebräuchlichen Maschinen verarbeitet werden. Auch zeigt es daß eine Erhöhung des Schüttgewichtes eintritt, .In the polymer particles treated according to the invention, the content is of volatile constituents is reduced to such an extent that unpleasant odors do not arise when the particles are processed. It was also found that the particles, when treated with hot inert gases, acquire a structure that allows better trickling the particle causes. Due to the better flowability you can the particles more easily in those for plastics processing, commonly used machines. It also shows that there is an increase in the bulk density.

Beispielexample

In eine Vorrichtung, wie sie in der Figur wiedergegeben ist, wird durch Rohrleitung (l) Polypropylen, das durch Gasphasenpolymerisation erhalten wurde, über Ventil (j5) in einen Cyklon (4) ein gebracht. Die Teilchen haben einen Durchmesser, der zwischen 10 und 5 000/U liegt. Der Cyklon hat einen Durchmesser von 50 cm und eine Höhe von 150 cm. Das vom Polymeren eingenommene Volumen im Cyklon beträgt im Mittel etwa 200 Liter. Pro Stunde werden etwjt 350 kg Polypropylen in den Cyklon (4) eingetragen. Durch Leitung; mit Ventil (5) wird ein Stickstoffatom von etwa TO m/Std. einge^. leitet. Durch Fallrohr (9) und Ventil (8) wird das Polypropylen aus dem Cyklon ausgetragen. Bei einer Bettdichte von etwa 0,j5 beträgt die mittlere Verweilzeit etwa 10 Minuten.In a device, as it is shown in the figure, is through pipe (l) polypropylene, which by gas phase polymerization was obtained, placed in a cyclone (4) via valve (j5). The particles have a diameter between 10 and 5,000 / rev. The cyclone has a diameter of 50 cm and a height of 150 cm. The volume occupied by the polymer im Cyklon averages around 200 liters. There are sth 350 kg of polypropylene entered into the cyclone (4). By line; with valve (5) a nitrogen atom of about TO m / h. turned ^. directs. The polypropylene is released through the downpipe (9) and valve (8) discharged from the cyclone. At a bed density of about 0.15 the mean residence time is about 10 minutes.

-. 5 -109882/155 7-. 5 -109882/155 7

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Das erfindungsgemäß behandelte Polymerisat ist praktisch geruchsfrei. Durch Extraktion mit siedendem Isopropanöl können etwa 0,8 Gewichtsprozent niedermolekulare Anteile aus dem Polymerisat entfernt werden» Vergleichsweise können aus einem Polymerisat, das nicht erfindungsgemäß behandelt wurde, 1,4 Gewichtsprozent niedermolekulare Anteile extrahiert werden.The polymer treated according to the invention is practically odorless. Extraction with boiling isopropane oil can remove about 0.8 percent by weight of low molecular weight fractions from the polymer In comparison, 1.4 percent by weight of low molecular weight polymer can be obtained from a polymer that has not been treated according to the invention Fractions are extracted.

Das Polymerisat kann mittels Spritzgußmaschinen bei einer Verarbeitungstemperatur von 300 bis JlO ° C zu Formkörpern verarbeitet werden. Verwendet man den nicht mit Inertgas behandelten Ausgangsstoff , so erhält man Formkörper, die mit feinen Gasbläschen durchsetzt sind. The polymer can by means of injection molding machines at a processing temperature from 300 to 100 ° C can be processed into moldings. If you use the raw material that has not been treated with inert gas , this gives moldings which are interspersed with fine gas bubbles.

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Claims (1)

PatentanspruchClaim Verfahren zum Entfernen flüchtiger Bestandteile aus feinteiligen
Olefinpolymerisaten, dadurch gekennzeichnet, daß man die Polymerisate, deren Teilchen einen durchschnittlichen Durchmesser von 100 bis 1 000/U haben, mit einem Inertgasstrom bei einer zwischen 80 ° C und mindestens 50C unter dem Kristallitschmelzpunkt liegenden Temperatur in einer in kräftiger Bewegung gehaltenen Pulverschicht durchspült.Process for removing volatile constituents from finely divided
Olefin polymers, characterized in that the polymers whose particles have an average diameter from 100 to 1000 / U, with an inert gas at a temperature between 80 ° C and at least 5 0 C below the crystallite melting temperature in a maintained in vigorous agitation powder layer flushed through. Badische Anilin- & Soda-Fabrik AGBadische Anilin- & Soda-Fabrik AG Zeiohn.Zeiohn. 109882/1557109882/1557
DE19681795396 1968-09-26 1968-09-26 Process for removing volatile, odor-causing constituents from finely divided olefin polymers Expired DE1795396C3 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
DE19681795396 DE1795396C3 (en) 1968-09-26 1968-09-26 Process for removing volatile, odor-causing constituents from finely divided olefin polymers
FR6930909A FR2022197A1 (en) 1968-09-26 1969-09-11
AT877069A AT296601B (en) 1968-09-26 1969-09-16 Process for removing volatile constituents from finely divided olefin polymers
BE738973D BE738973A (en) 1968-09-26 1969-09-17
NL6914421A NL6914421A (en) 1968-09-26 1969-09-23
GB4715069A GB1272778A (en) 1968-09-26 1969-09-25 Removing volatile constituents from particulate olefin polymers produced by gas-phase polymerization

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19681795396 DE1795396C3 (en) 1968-09-26 1968-09-26 Process for removing volatile, odor-causing constituents from finely divided olefin polymers

Publications (3)

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DE1795396A1 true DE1795396A1 (en) 1972-01-05
DE1795396B2 DE1795396B2 (en) 1979-02-22
DE1795396C3 DE1795396C3 (en) 1982-05-19

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DE19681795396 Expired DE1795396C3 (en) 1968-09-26 1968-09-26 Process for removing volatile, odor-causing constituents from finely divided olefin polymers

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AT (1) AT296601B (en)
BE (1) BE738973A (en)
DE (1) DE1795396C3 (en)
FR (1) FR2022197A1 (en)
GB (1) GB1272778A (en)
NL (1) NL6914421A (en)

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Also Published As

Publication number Publication date
BE738973A (en) 1970-03-17
DE1795396C3 (en) 1982-05-19
GB1272778A (en) 1972-05-03
DE1795396B2 (en) 1979-02-22
NL6914421A (en) 1970-04-01
AT296601B (en) 1972-02-25
FR2022197A1 (en) 1970-07-31

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E77 Valid patent as to the heymanns-index 1977
C3 Grant after two publication steps (3rd publication)