DE1570141A1 - Process for vulcanizing carbon black blends of natural rubber and butyl rubber - Google Patents

Process for vulcanizing carbon black blends of natural rubber and butyl rubber

Info

Publication number
DE1570141A1
DE1570141A1 DE19651570141 DE1570141A DE1570141A1 DE 1570141 A1 DE1570141 A1 DE 1570141A1 DE 19651570141 DE19651570141 DE 19651570141 DE 1570141 A DE1570141 A DE 1570141A DE 1570141 A1 DE1570141 A1 DE 1570141A1
Authority
DE
Germany
Prior art keywords
rubber
blends
vulcanizing
natural rubber
carbon black
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
DE19651570141
Other languages
German (de)
Inventor
Roy Hrishikesh Chandra
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.)
Metzeler AG
Original Assignee
Metzeler 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 Metzeler AG filed Critical Metzeler AG
Publication of DE1570141A1 publication Critical patent/DE1570141A1/en
Pending 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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C08L9/06—Copolymers with styrene
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/32—Compounds containing nitrogen bound to oxygen
    • C08K5/33—Oximes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00—Compositions of unspecified rubbers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
    • C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
    • C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L7/00—Compositions of natural rubber
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers

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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)
  • Compositions Of Macromolecular Compounds (AREA)

Description

Verfahren zwn Vulkanisieren von rußhaltigen Verschnittmischungen aus Naturkautschuk und Butylkautschuk Die Erfindung bezieht sich auf ein Verfahren zum Vulkanisieren von rußhaltigen Verschnittmischungen aus Naturkautschuk und Butylkautschuk, die neben einem schwefelhaltigen Vulkanisationssystem Zinkoxyd und Stearinsäure enthalten, unter Druck und Wärme.Process for vulcanizing carbon black blends Natural rubber and butyl rubber The invention relates to a method for Vulcanization of soot-containing blends of natural rubber and butyl rubber, which in addition to a sulfur-containing vulcanization system, zinc oxide and stearic acid contained, under pressure and heat.

Zu nicht-schwarzen Wandqualitäten von Fahrzeugluftreifen werden gern Vulkanisate von Naturkautschuk-Chloroprenkautschuk oder auch von Naturkautschuk-Chloroprenkautschuk-chlorsulfoniertes Polyäthylen-Verschnitten verwendet. Diese Vulkanisate sind sehr teuer.Non-black wall qualities of pneumatic vehicle tires are popular Vulcanizates of natural rubber-chloroprene rubber or natural rubber-chloroprene rubber-chlorosulfonated Polyethylene blends used. These vulcanizates are very expensive.

Bekannt wurden bereits Verschnittmischungen aus Naturkautschuk und Butylkautschuk, die neben Kanalruß als schwarzem Füllstoff, Zinkoxyd und Stearinsäure ein Vulkanisationssystem enthalten, das aus Mercaptobenzothiazol, Tetramethylthiuramdisulfid und zwei bis drei Gewichtsteilen elementarem Schwefel, bezogen auf 100 Gewichtsteile Gesamtkautschuk, besteht. Die Anteile aus Naturkautschuk dieser Verschnittmischungen sind sehr niedrig gehalten.Blends of natural rubber and Butyl rubber, which is used as a black filler, zinc oxide and stearic acid in addition to soot contain a vulcanization system consisting of mercaptobenzothiazole, tetramethylthiuram disulfide and two to three parts by weight of elemental sulfur based on 100 parts by weight Total rubber. The proportions of natural rubber in these blends are kept very low.

Vulkanisate aus solchen Verschnittmischungen heizen nicht aus und sind deshalb insbesondere fUr Seitenwände von FahrzeugluStreifen zu weich.Vulcanizates from such blends do not heat up and are therefore too soft, especially for the side walls of vehicle air strips.

Es wurde gefunden, daß diese Nachteile bekannter Kautschukverschnittmischungen vermieden werden können, wenn solche Verschnittmischungen vulkanisiert werden, die Kieselsäure, Alterungsschutzmittel und Weichmacher enthalten und deren Vulkanisationssystem aus Mercaptobenzothiazol, Tetramethylthiuramdisulfid, Diphenylguanidin, Dibenzothiazyldisulfid, pp' -Dibenzoylchinondioxim, Phthalsäureanhydrid und weniger als einen Gewichtsteil elementarem Schwefel, bezogen auf 100 Gewichtsteile Gesamtkautschuk, zusammengesetzt ist.It has been found that these disadvantages of known rubber blend compounds can be avoided if such blends are vulcanized that Contain silica, anti-aging agents and plasticizers and their vulcanization system from mercaptobenzothiazole, tetramethylthiuram disulfide, diphenylguanidine, dibenzothiazyl disulfide, pp '-dibenzoylquinone dioxime, phthalic anhydride and less than one part by weight elemental sulfur, based on 100 parts by weight of total rubber is.

Die physikalischen Eigenschaften solcher Vulkanisate sind denen von Verschnittmischungen aus Naturkautschuk-Chloroprenkautschuk-oder Naturkautschuk-Chloroprenkautschuk-chlorsulfoniertes Polyäthylen-Verschnitten nahe und dabei wesentlich preiswerter als diese.The physical properties of such vulcanizates are those of Blends of natural rubber-chloroprene rubber or natural rubber-chloroprene rubber-chlorosulfonated Polyethylene blends close and at the same time much cheaper than this.

In den nachfolgenden beiden Mischungsbeispielen sind die Prü£-ergebnisse zum Vulkanisat einer Naturkautschuk-Chloroprenkautschuk-Mischung einer erfindungsgemäßen Naturkautschuk-Butylkautschuk-Mischung mit zugehörigen Prürergebnissen gegenübergestellt.The test results are shown in the following two mixing examples to the vulcanizate of a natural rubber-chloroprene rubber mixture of an inventive Natural rubber-butyl rubber mixture compared with the corresponding test results.

Mischung I Gewichtsteile Metunkautschuk (Bermeo I) 40,-Nesprenkautschuk und Chleroprenkautschuk (Moopren W) Chlorsulfoniertes Polyäthylen (Mypalon 20) 20,-Zinkonyd (Zimk I RS) 62,-Titandioxyd (Schwedischwois) 49,-Kieselsäure (VN 3) 8,5 Stearinsäure (Stearin P) 1,-Alterungesehutamittel auf phenolischer Easis (Nenox WSL) 0,45 Phenolkondensationspredukt als Alterungsschutzmittel (Nonox LX) 0,45 Wsschblau 0,45 Wachs (Antilux) 3,3 Schwefel (Ölsehwefel 0,2) 0,7 Dibemmothiazyldisulfid mit Öl (Ölvulkazit M) 0,65 Totrametkylthiuramidsulfid (Vulkazit Th) 0,2 2-Moreaptoimidazolin (NA 22) 0,2 Prüfergebnisse: Keisung bei 143° C 35 Min 60 Min Modul bei 300% kg/cm2 33 35 Modul bie 500% kg/cm2 59 66 Zugfestigkeit kg/cm2 89 92 Bruchdehnung % 670 640 Shore-Härte Shoregrade 54 46 Elastizität % 35 35 Misehung II Gewichtsteile Matarkautschuk (Para II) 70,-Butylkautschuk (Butyl 325) 30,-Zinkoxyd (Zink I RS) 62,-Titandioxyd (Schwedischweiß) 49,-Mieselsäure (VN 3) 8,5 Stearinsäure (Stearin P) 1,-Alterungsschutzmittel auf phenolisch4er Basis (Konox WSL) Phenolkendonsationsprodukt als Alterungsschutzmittel (Nonox EX) 0,45 Wasehblau 0,45 Wachs (Antilux) 3,3 Schwefel (Ölschwefel 0,2) 0,66 Fortsetzung Mischung II Gewichtsteile Dibenzothiasyldiculfid mit Öl (Ölvulkazit M) 2,06 Tetramethylthiuramdiaulfid (Vulkazit Th) 0,1 Mereaptobenzothiazol (Vulkazit C) 0,5 Diphenylg@@@idin rit Öl (Ölvulkazit D) 0,33 pp'-Dibenzoylchinondioxim (dibenzo GMF) 1,-Phtalsäureanhydrid (Vulkalent B) 1,-Prüfergebnisse: Heizung ei 143° C 35 Min 60 Min Modul bei 300% kg/cm2 43 44 Modul bei 500% kg/cm2 ~ » Zugfestigkeit kg/cm2 94 102 Bruchdehnung % % 485 5 Shore-Härte Shoregrade 55 56 Elastizität % 45 45 Das Vulkamisat der : Butylkautschukverschnittmischung gemäß Mischung II ist gut, aber - bei Verwendung weiß er Füllstoffe -nicht eimmundfrei weiß. Dieser kleine Mangel ist jedoch bedoutungsles, de nicht nur schwarz-weiße, sendern auch schwarzbunte, z. B. schwarz-rote, schwarz-gelbe, schwarz-blaue usf., Reifen @ergestellt werden. Der Grundmischung ist also nach Bedarf nur noch die erforderliche Farbe zuzusetzen.Mixture I parts by weight of metal rubber (Bermeo I) 40 Nesprene rubber and chloroprene rubber (Moopren W) chlorosulfonated polyethylene (Mypalon 20) 20, -zinc cony (Zimk I RS) 62, -Titanium dioxide (Swedish Wois) 49, -Silicic acid (VN 3) 8,5 stearic acid (Stearin P) 1, phenolic Easis anti-aging drug (Nenox WSL) 0.45 phenol condensation product as an anti-aging agent (Nonox LX) 0.45 azure blue 0.45 wax (Antilux) 3.3 sulfur (Oil sulfur 0.2) 0.7 Dibemmothiazyl disulfide with oil (oil volkacite M) 0.65 Totrametkylthiuramide sulfide (Vulkazit Th) 0.2 2-Moreaptoimidazoline (NA 22) 0.2 Test results: Keisung at 143 ° C 35 min 60 min module at 300% kg / cm2 33 35 module at 500% kg / cm2 59 66 tensile strength kg / cm2 89 92 Elongation at break% 670 640 Shore hardness Shore grade 54 46 Elasticity% 35 35 Mixture II parts by weight Matar rubber (Para II) 70, -Butyl rubber (Butyl 325) 30, -Zinc oxide (Zinc I RS) 62, -Titanium dioxide (Swedish white) 49, -Miesel acid (VN 3) 8,5 stearic acid (stearin P) 1, phenolic4-based anti-aging agent (Konox WSL) Phenol kendonsation product as an anti-aging agent (Nonox EX) 0.45 Wash blue 0.45 wax (Antilux) 3.3 sulfur (oil sulfur 0.2) 0.66 continuation Mixture II parts by weight of dibenzothiasyl diculphide with oil (oil volkacite M) 2.06 tetramethylthiuram diaulphide (Vulkazit Th) 0.1 Mereaptobenzothiazol (Vulkazit C) 0.5 Diphenylg @@@ idin rit oil (Oil volkacite D) 0.33 pp'-dibenzoylquinone dioxime (dibenzo GMF) 1, -phthalic anhydride (Vulkalent B) 1, -test results: heating at 143 ° C 35 min 60 min module at 300% kg / cm2 43 44 module at 500% kg / cm2 ~ »tensile strength kg / cm2 94 102 elongation at break %% 485 5 Shore hardness Shore grade 55 56 Elasticity% 45 45 The vulcanized material of: Butyl rubber blend mixture according to mixture II is good, but - when used he knows fillers -not free from immunity white. This little flaw, however, is bedoutungsles, de not only black and white, but also black and white channels, e.g. B. black-red, black-yellow, black-blue etc., tires @ can be created. So the basic mix is as needed just add the required color.

Die Verläbung des pp'-Dibenzoylchinondioxims der Mischung ist mit "non staining" zu bezeichnen, d.h. nur die betreffende Qualität verfärbt sich geringfügig, eine angrenzende Mischung verfärbt sjch Jedoch nicht. in geringer Anteil an Cis-1,4-Polybutadien ist zur Verbesserung der Vulltanisation bei Naturkautschuk-Butylkautschukverschnitt vorteilhaft. Der Grund hierfür ist noch nicht bekannt.The variation of the pp'-dibenzoylquinone dioxime in the mixture is with to be called "non staining", i.e. only the quality in question is slightly discolored, however, an adjacent mixture does not discolor. in a small proportion of cis-1,4-polybutadiene is to improve the vulltanization of natural rubber-butyl rubber offcuts advantageous. The reason for this is not yet known.

Es ist klar, daß ähnlich vorteilhafte naturkautschuk-Butylkautschuk-Verschmittvulkanisate auch mit gegenüber der Mischung II abweichenden Gewichtsteilen der Mischungsbestandteile derselben erreichbar sind.It is clear that natural rubber-butyl rubber vulcanizates are similarly advantageous also with parts by weight of the mixture constituents which differ from mixture II the same are attainable.

Claims (2)

Patentansprüche 1. Verfahren zum Vulkanisieren von rußhaltigen Verschnittmischungen aus Naturkautschuk und Butylkautschuk, die neben einem schwefelhaltigen Vulkanisationssystem Zinkoxyd und Stearinsäure enthalten, unter Druck und Wärme, dadurch gekennzeichnet, daß solche Verschnittmischungen vulkanisiert werden, die Kieselsäure, Alterungsschutzmittel und Weichmacher enthalten und deren Vulkanisationssystem aus Mercaptobenzothiazol, Tetramethylthiuramdisulfid, Diphenylguanidin, Dibenzothiazyldisulfid, pp'-Dibenzoylchinondioxim, Phthalsäureanhydrid und weniger als einen Gewichtsteil elementarem Schwefel, bezogen auf 100 Gewichtsteile Gesamtkautschuk, zusammengesetzt ist. Claims 1. A method for vulcanizing carbon black blends made of natural rubber and butyl rubber, in addition to a sulfur-containing vulcanization system Containing zinc oxide and stearic acid, under pressure and heat, characterized that such blends are vulcanized, the silica, anti-aging agents and plasticizers and their vulcanization system from mercaptobenzothiazole, Tetramethylthiuram disulfide, diphenylguanidine, dibenzothiazyl disulfide, pp'-dibenzoylquinone dioxime, Phthalic anhydride and less than one part by weight elemental sulfur to 100 parts by weight of total rubber. 2. Verfahren zum Vulkanisieren von Verschnittmischungen nach Anspruch 1, dadurch gekennzeichnet, daß zumindest ein Teil der Alterungsschutzmittel auf phenolischer Basis aufgebaut und ein Phenolkondensationsprodukt ist.2. A method for vulcanizing blends according to claim 1, characterized in that at least some of the anti-aging agents on phenolic basis and is a phenolic condensation product.
DE19651570141 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and butyl rubber Pending DE1570141A1 (en)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
DEM0067092 1965-10-28
DEM0067093 1965-10-28
DEM0067089 1965-10-28
DEM0067090 1965-10-28
DEM0067091 1965-10-28
DEM0067094 1965-10-28

Publications (1)

Publication Number Publication Date
DE1570141A1 true DE1570141A1 (en) 1969-05-22

Family

ID=27544885

Family Applications (6)

Application Number Title Priority Date Filing Date
DE19651570140 Pending DE1570140A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and butyl rubber
DE19651570141 Pending DE1570141A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and butyl rubber
DE19651570138 Pending DE1570138A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and butyl rubber
DE19651570137 Pending DE1570137A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing blends consisting of natural rubber, butyl rubber and ethylene terpolymer rubber
DE19651570136 Pending DE1570136A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing blends of butyl rubber and, optionally oil-expanded, butadiene styrene rubber
DE19651570139 Pending DE1570139A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and ethylene propylene terpolymer rubber

Family Applications Before (1)

Application Number Title Priority Date Filing Date
DE19651570140 Pending DE1570140A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and butyl rubber

Family Applications After (4)

Application Number Title Priority Date Filing Date
DE19651570138 Pending DE1570138A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and butyl rubber
DE19651570137 Pending DE1570137A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing blends consisting of natural rubber, butyl rubber and ethylene terpolymer rubber
DE19651570136 Pending DE1570136A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing blends of butyl rubber and, optionally oil-expanded, butadiene styrene rubber
DE19651570139 Pending DE1570139A1 (en) 1965-10-28 1965-10-28 Process for vulcanizing carbon black blends of natural rubber and ethylene propylene terpolymer rubber

Country Status (2)

Country Link
DE (6) DE1570140A1 (en)
GB (1) GB1127102A (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2202852B (en) * 1987-03-31 1991-07-24 Acushnet Co Rubber composition for use with potable water
US4946593A (en) * 1987-03-31 1990-08-07 Acushnet Company Rubber composition for use with potable water
US5405105A (en) * 1993-05-28 1995-04-11 Hudson Valley V/Stol Aircraft, Inc. Tilt wing VTOL aircraft
DE102010060355B4 (en) 2010-11-04 2022-01-13 Continental Reifen Deutschland Gmbh Rubber mixture and its use for the manufacture of a tyre, belt, strap or tube
JP6068949B2 (en) * 2012-09-05 2017-01-25 住友ゴム工業株式会社 Rubber composition for tire, pneumatic tire and method for preventing tire discoloration
JP6068951B2 (en) * 2012-09-05 2017-01-25 住友ゴム工業株式会社 Rubber composition for tire, pneumatic tire and method for preventing tire discoloration
JP6068950B2 (en) * 2012-09-05 2017-01-25 住友ゴム工業株式会社 Rubber composition for tire, pneumatic tire and method for preventing tire discoloration

Also Published As

Publication number Publication date
DE1570137A1 (en) 1969-08-21
DE1570140A1 (en) 1969-08-14
DE1570139A1 (en) 1969-08-28
DE1570136A1 (en) 1970-03-26
GB1127102A (en) 1968-09-11
DE1570138A1 (en) 1969-08-28

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