DE1132716B - Process for the production of finely divided plasticized polyvinyl chloride powder - Google Patents

Process for the production of finely divided plasticized polyvinyl chloride powder

Info

Publication number
DE1132716B
DE1132716B DEC15411A DEC0015411A DE1132716B DE 1132716 B DE1132716 B DE 1132716B DE C15411 A DEC15411 A DE C15411A DE C0015411 A DEC0015411 A DE C0015411A DE 1132716 B DE1132716 B DE 1132716B
Authority
DE
Germany
Prior art keywords
polyvinyl chloride
finely divided
production
chloride powder
plasticized polyvinyl
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
Application number
DEC15411A
Other languages
German (de)
Inventor
Dr Karl Weissbach
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.)
Huels AG
Original Assignee
Chemische Werke Huels AG
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 Chemische Werke Huels AG filed Critical Chemische Werke Huels AG
Priority to DEC15411A priority Critical patent/DE1132716B/en
Priority to FR1200555D priority patent/FR1200555A/en
Priority to GB2346458A priority patent/GB844008A/en
Publication of DE1132716B publication Critical patent/DE1132716B/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • C08J3/122Pulverisation by spraying
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/04Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06Homopolymers or copolymers of vinyl chloride

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Description

DEUTSCHESGERMAN

PATENTAMTPATENT OFFICE

C 15411 IVd/39bC 15411 IVd / 39b

ANMELDETAG: 31. AUGU ST 1957REGISTRATION DATE: AUGUST 31, 1957

BEKANNTMACHUN G
DER ANMELDUNG
UND AUSGABE DER
AUSLEGESCHRIFT: 5. JULI 1962
NOTICE
THE REGISTRATION
AND ISSUE OF THE
EDITORIAL: JULY 5, 1962

Neben der Verarbeitung von weichmacherfreiem Polyvinylchlorid spielt dessen Verarbeitung mit Weichmachern eine große Rolle bei der Herstellung von Formkörpern, wie Folien, Kunstleder, Schläuchen und Profilen. Das Mischen des Polyvinylchlorids mit den Weichmachern geschieht in Knetapparaten oder Mischern. Dieser Vorgang erfordert einen ziemlichen Zeitaufwand und führt nicht zu einer homogenen Verteilung des Weichmachers auf den Polyvinylchloridteilchen. Infolgedessen ist für manche Verarbeitungszwecke oftmals noch ein Homogenisieren unter Wärmezufuhr, d. h. ein Angelieren, vor der Weiterverarbeitung notwendig. Besonders für die Verarbeitung in Spritzgußmaschinen strebt man eine ideale Verteilung des Weichmachers auf den Polyvinylchloridteilchen an, da die Durchmischung während des Geliervorganges in der Förderschnecke nicht mehr allzu intensiv ist.In addition to the processing of plasticizer-free polyvinyl chloride, its processing also plays a role Plasticizers play an important role in the production of molded articles such as foils, artificial leather and hoses and profiles. The mixing of the polyvinyl chloride with the plasticizers is done in kneaders or Mixers. This process takes a fair amount of time and does not lead to a homogeneous one Distribution of the plasticizer on the polyvinyl chloride particles. As a result, it is for some processing purposes often a homogenization with supply of heat, d. H. a gelation before the Further processing necessary. One strives for one especially for processing in injection molding machines ideal distribution of the plasticizer on the polyvinyl chloride particles, since the mixing is no longer too intense during the gelling process in the screw conveyor.

Es wurde gefunden, daß man feinteiliges, weichmacherhaltiges Polyvinylchlorid-Pulver, welches sich ohne jede weitere Behandlung hervorragend verarbeiten läßt, dadurch herstellen kann, daß man wäßrige, Polyvinylchlorid und flüssige Weichmacher enthaltende Suspensionen bzw. Emulsionen bei Temperaturen von 110 bis 1800C einer Sprühtrocknung unterwirft und an die Sprühtrocknung eine Behandlung des Polyvinylchlorids mit einem Heißluftbzw, inerten Gasstrom mit Temperaturen von 140 bis 200° C anschließt. Man erhält auf diese einfache Weise eine völlig homogene Verteilung des Weichmachers auf den Polyvinylchloridteilchen. Zweckmäßig versprüht man die bei der Suspensions- oder Emulsionspolymerisation des Vinylchlorids anfallenden wäßrigen Suspensionen oder Emulsionen, in denen man den Weichmacher in dem gewünschten Verhältnis zum Polyvinylchlorid in bekannter Weise, z. B. durch Rühren mit oder ohne Anwendung eines Emulgators, wie Alkylsulfonate oder Alkalisalze saurer Alkylschwefelsäureester, suspendiert bzw. emulgiert hat. Bei einem Emulgatorgehalt von etwa 2,5% lassen sich in einer durch Emulsionspolymerisation erhaltenen Emulsion von Polyvinylchlorid z. B. ohne weiteres bis zu 40% Weichmacher emulgieren. Jedoch lassen sich mit gleichem Erfolg auch Suspensionen bzw. Emulsionen verwenden, die man aus feinteiligem weichmacherfreiem Polyvinylchlorid-Pulver hergestellt hat. Zur Durchführung des erfindungsgemäßen Verfahrens, das auf Polyvinylchlorid jeden Polymerisationsgrades anwendbar ist, eignen sich alle für Polyvinylchlorid gebräuchlichen flüssigen Weichmacher, z. B. Dioctylphthalat, Dibutylphthalat, höhere Ester der Adipinsäure, der Verfahren zur HerstellungIt has been found that finely divided, plasticized polyvinyl chloride powder which can be processed excellently without any further treatment, can be prepared characterized in that aqueous, polyvinyl chloride and liquid plasticizer suspensions containing or emulsions at temperatures of 110 to 180 0C to spray drying and the spray drying is followed by a treatment of the polyvinyl chloride with a hot air or inert gas stream at temperatures of 140 to 200 ° C. In this simple way, a completely homogeneous distribution of the plasticizer on the polyvinyl chloride particles is obtained. The aqueous suspensions or emulsions obtained in the suspension or emulsion polymerization of vinyl chloride in which the plasticizer is in the desired ratio to the polyvinyl chloride in a known manner, for. B. has suspended or emulsified by stirring with or without the use of an emulsifier, such as alkyl sulfonates or alkali salts of acidic alkyl sulfuric acid esters. With an emulsifier content of about 2.5%, in an emulsion of polyvinyl chloride obtained by emulsion polymerization, for. B. easily emulsify up to 40% plasticizer. However, suspensions or emulsions which have been produced from finely divided plasticizer-free polyvinyl chloride powder can also be used with the same success. To carry out the process according to the invention, which can be applied to polyvinyl chloride of any degree of polymerization, all liquid plasticizers commonly used for polyvinyl chloride, e.g. B. dioctyl phthalate, dibutyl phthalate, higher esters of adipic acid, the process for production

von feinteiligem weichmacherhaltigemof finely divided plasticizer-containing

Polyvinylchlorid-PulverPolyvinyl chloride powder

Anmelder:Applicant:

Chemische Werke Hüls Aktiengesellschaft, Marl (Kr. Recklinghausen)Chemical works Hüls Aktiengesellschaft, Marl (Kr.Recklinghausen)

Dr. Karl Weißbach, Marl (Kr. Recklinghausen), ist als Erfinder genannt wordenDr. Karl Weißbach, Marl (Kr. Recklinghausen), has been named as the inventor

Sebacinsäure, Trikresylphosphat. Sie können in beliebiger Menge, beispielsweise bis zu 40%, mit dem Polyvinylchlorid vermischt werden.Sebacic acid, tricresyl phosphate. You can use any amount, for example up to 40%, with the Polyvinyl chloride are mixed.

Durch die sich an die Sprühtrocknung anschließende Behandlung mit einem Heißluft- bzw. inerten Gasstrom, der eine Temperatur von etwa 140 bis 200° C hat, erhält man aus dem bei der Sprühtrocknung mehr oder weniger klebrig anfallenden Polyvinylchlorid ein gut rieselfähiges Pulver.The subsequent treatment with a hot air or inert gas stream after spray drying, which has a temperature of about 140 to 200 ° C, is obtained from the spray drying more or less sticky polyvinyl chloride is a free-flowing powder.

Beispiel 1example 1

In eine nach dem Emulsionsverfahren erhaltene Polyvinylchloridemulsion mit etwa 48% Polyvinylchlorid vom K-Wert 70 und etwa 2,5% Natriumalkylsulfonat als Emulgator rührt man 20% Dioctylphthalat (bezogen auf den Feststoffgehalt an Polyvinylchlorid) ein und verdüst diese Mischung mit einer Sprühtrocknungsanlage in heiße Luft von etwa 140° C. Das als schneeweißes, etwas klebriges Pulver anfallende Trockengut wird in ein senkrecht stehendes Rohr von 100 cm Durchmesser und 1200 cm Höhe eingeführt, das mit einem Heißluftstrom (300 Nm3 je Stunde) von 170° C beaufschlagt wird. Bereits bei 4 Sekunden Verweilzeit bei zweimaligem Durchgang tritt eine nahezu völlige Durchgelierung der einzelnen Teilchen ein, und man erhält als Filtergut ein feinteiliges, weichmacherhaltiges Polyvinylchlorid, das ideal rieselfähig ist.20% dioctyl phthalate (based on the solids content of polyvinyl chloride) is stirred into a polyvinyl chloride emulsion obtained by the emulsion process with about 48% polyvinyl chloride with a K value of 70 and about 2.5% sodium alkyl sulfonate as an emulsifier and this mixture is atomized into hot air using a spray-drying system of about 140 ° C. The dry material, which is a snow-white, somewhat sticky powder, is introduced into a vertical tube 100 cm in diameter and 1200 cm in height, which is subjected to a stream of hot air (300 Nm 3 per hour) at 170 ° C. Already after a dwell time of 4 seconds with two passes, the individual particles are almost completely gelled, and the filter material obtained is a finely divided, plasticizer-containing polyvinyl chloride which is ideally free-flowing.

Beispiel 2Example 2

Setzt man der im Beispiel 1 beschriebenen Polyvinylchloridemulsion 40% Dioctylphthalat zu, so erhält man durch Verdüsen der Mischung beiThe polyvinyl chloride emulsion described in Example 1 is used 40% dioctyl phthalate is obtained by spraying the mixture at

209 618/345209 618/345

140° C ein stärker klebriges Polyvinylchlorid, das bei der Nachbehandlung mit einem Heißluftstrom von 1700C ebenfalls ein feinteiliges, gut rieselfähiges Pulver ergibt.140 ° C, a more sticky polyvinyl chloride, which also results in a finely divided, free-flowing powder at the post-treatment with a hot air current of 170 0 C.

Claims (1)

PATENTANSPRUCH:PATENT CLAIM: Verfahren zur Herstellung von feinteiligem, weichmacherhaltigem Polyvinylchlorid-Pulver, da durch gekennzeichnet, daß man wäßrige, Polyvinylchlorid und flüssige Weichmacher enthaltende Suspensionen bzw. Emulsionen bei Temperaturen von 110 bis 180° C einer Sprühtrocknung unterwirft und an die Sprühtrocknung eine Behandlung des Polyvinylchlorids mit einem Heißluft- bzw. inerten Gasstrom mit Temperaturen von 140 bis 200° C anschließt.Process for the production of finely divided, plasticized polyvinyl chloride powder, characterized in that aqueous suspensions or emulsions containing polyvinyl chloride and liquid plasticizers are subjected to spray drying at temperatures of 110 to 180 ° C. and the spray drying is followed by treatment of the polyvinyl chloride with hot air - or an inert gas stream with temperatures of 140 to 200 ° C follows. In Betracht gezogene Druckschriften:
Deutsche Patentschrift Nr. 749 509;
USA.-Patentschrift Nr. 2 530 852.
Considered publications:
German Patent No. 749 509;
U.S. Patent No. 2,530,852.
©209 618/345 6.62© 209 618/345 6.62
DEC15411A 1957-08-31 1957-08-31 Process for the production of finely divided plasticized polyvinyl chloride powder Pending DE1132716B (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DEC15411A DE1132716B (en) 1957-08-31 1957-08-31 Process for the production of finely divided plasticized polyvinyl chloride powder
FR1200555D FR1200555A (en) 1957-08-31 1958-07-21 Process for the preparation of finely divided polyvinyl chloride containing plasticizers
GB2346458A GB844008A (en) 1957-08-31 1958-07-22 Improvements in the production of readily-trickling, fine-particled polyvinyl chloride containing plasticizer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEC15411A DE1132716B (en) 1957-08-31 1957-08-31 Process for the production of finely divided plasticized polyvinyl chloride powder

Publications (1)

Publication Number Publication Date
DE1132716B true DE1132716B (en) 1962-07-05

Family

ID=7015834

Family Applications (1)

Application Number Title Priority Date Filing Date
DEC15411A Pending DE1132716B (en) 1957-08-31 1957-08-31 Process for the production of finely divided plasticized polyvinyl chloride powder

Country Status (3)

Country Link
DE (1) DE1132716B (en)
FR (1) FR1200555A (en)
GB (1) GB844008A (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2434853C3 (en) * 1974-07-19 1981-04-30 Pelikan Ag, 3000 Hannover Process for the softening of plastic masses

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE749509C (en) * 1942-02-13 1944-12-27 Process for the production of polyvinyl chloride powder containing additives
US2530852A (en) * 1947-09-04 1950-11-21 Goodrich Co B F Production of dry powdery thermoplastic compositions

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE749509C (en) * 1942-02-13 1944-12-27 Process for the production of polyvinyl chloride powder containing additives
US2530852A (en) * 1947-09-04 1950-11-21 Goodrich Co B F Production of dry powdery thermoplastic compositions

Also Published As

Publication number Publication date
FR1200555A (en) 1959-12-22
GB844008A (en) 1960-08-10

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