BS ISO 5794-3-2011 Rubber compounding ingredients Silica precipitated hydrated Evaluation procedures in a blend of solution styrene-butadiene rubber (S-SBR) and butadiene rubber (B.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 5794-3:2011Rubber compoundingingredients Silica,precipitated, hydratedPart 3: Evaluation procedures in a blend ofsolution styrene-butadiene rubber (S-SBR)and butadiene rub

2、ber (BR)BS ISO 5794-3:2011 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 5794-3:2011.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/23, Test methods for rubber and non-blackcompounding ingredients.A list of organizations repre

3、sented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 67344 3ICS 83.040.20Compliance with a British Standard cannot confer im

4、munity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 August 2011.Amendments issued since publicationDate Text affectedBS ISO 5794-3:2011Rubber compounding ingredients Silica, precipitated, hydrated Part 3:Evaluation

5、procedures in a blend of solution styrene-butadiene rubber (S-SBR) and butadiene rubber (BR)Ingrdients de mlange du caoutchouc Silices hydrates prcipites Partie 3: Mthodes dvaluation dans un mlange de solution de caoutchouc styrne-butadine (S-SBR) et butadine (BR) ISO 2011Reference numberISO 5794-3:

6、2011(E)First edition2011-08-01ISO5794-3INTERNATIONAL STANDARDBS ISO 5794-3:2011ISO 5794-3:2011(E)COPYRIGHT PROTECTED DOCUMENT ISO 2011All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, incl

7、uding photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in

8、Switzerlandii ISO 2011 All rights reservedBS ISO 5794-3:2011ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committ

9、ees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the Int

10、ernational Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International St

11、andards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.Attention is drawn to the possibility that some of the elements of this document may be the subj

12、ect of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 5794-3 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.ISO 5794 consists of the follo

13、wing parts, under the general title Rubber compounding ingredients Silica, precipitated, hydrated: Part 1: Non-rubber tests Part 2: Evaluation procedures in styrene-butadiene rubber Part 3: Evaluation procedures in a blend of solution styrene-butadiene rubber (S-SBR) and butadiene rubber (BR)ISO 579

14、4-3:2011(E) ISO 2011 All rights reserved iiiBS ISO 5794-3:2011BS ISO 5794-3:2011INTERNATIONAL STANDARD ISO 5794-3:2011(E)Rubber compounding ingredients Silica, precipitated, hydrated Part 3:Evaluation procedures in a blend of solution styrene-butadiene rubber (S-SBR) and butadiene rubber (BR)WARNING

15、 Persons using this part of ISO 5794 should be familiar with normal laboratory practice. This International Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and

16、to ensure compliance with any national regulatory conditions.1 ScopeThis part of ISO 5794 specifies the test formulation, equipment, procedure and test methods for determining the physical properties of precipitated hydrated silica in a compound based on a blend of solution styrene-butadiene and but

17、adiene rubber. The formulation can be regarded as a model compound for silica-based passenger car tyre treads.NOTE 1 ISO 5794-22specifies the test formulation, equipment, procedure and test methods for determining the physical properties of precipitated hydrated silica in a styrene-butadiene rubber

18、mix.NOTE 2 ISO 5794-11specifies methods for chemical analysis of precipitated hydrated silica, describes its physical and chemical properties, and classifies silicas with respect to their specific surface area obtained by nitrogen adsorption.2 Normative referencesThe following referenced documents a

19、re indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain pro

20、pertiesISO 48, Rubber, vulcanized or thermoplastic Determination of hardness (hardness between 10 IRHD and 100 IRHD)ISO 289-1, Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosityISO 2393, Rubber test mixes Preparation, mixing and vulcanizati

21、on Equipment and proceduresISO 3417, Rubber Measurement of vulcanization characteristics with the oscillating disc curemeterISO 6502, Rubber Guide to the use of curemeters3 Test formulationThe standard formulation is given in Table 1. The formulation shall be used for any type of silica precipitated

22、 for its evaluation.International or national standard chemicals shall be used if available. Materials used shall be chemically equivalent to those indicated in Table 1.For interlaboratory comparisons, the same type of S-SBR and BR shall be used. ISO 2011 All rights reserved 1BS ISO 5794-3:20114 Pro

23、cedure4.1 Equipment and procedure4.1.1 GeneralEquipment and procedure for preparation, mixing and vulcanization shall be in accordance with ISO 2393. The following procedure is an example which has been found suitable for a 1,5 l internal mixer of the Banbury1)type.4.1.2 First stage Filling factor:

24、0,74. Rotational speed: 70 r/min. Starting temperature: 80 C. Friction: 1:1,11. Ram pressure: 0,55 MPa.The first stage procedure is given in a) to j) herafter.Duration mina) Add polymers. 0,0 to 0,5b) Add half of the silica, carbon black/silane, ZnO, stearic acid, oil. 0,5 to 1,5c) Clean. 1,5d) Add

25、half of the silica, antioxidant, wax. 1,5 to 3,5e) Clean. 3,5f) Mix and adjust rotational speed if required to reach discharge temperature. 3,5 to 5,0g) Discharge batch (batch temperature: 155 C to 165 C). 5,0h) Transfer to mill. i) Band for 45 s using a clearance of 4 mm between the rolls. j) Store

26、 compound for 24 h at room temperature before proceeding to second stage. 1) Banbury is the trade name of a product supplied by Farrel Corp. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products

27、 may be used if they can be shown to lead to the same results.ISO 5794-3:2011(E)2 ISO 2011 All rights reservedBS ISO 5794-3:2011Table 1 Standard test formulationMaterial Parts by mass1st stage S-SBR, extended with TDAEa96,25BRb30Silica, precipitated 80Carbon black N 330 6,4Organosilane TESPTc6,4ZnOd

28、3Stearic acide2Oil TDAEf11,25Antioxidant (6PPD)g1,5Waxh12nd stage (no additional ingredient) 3rd stage DPGi2CBSj1,5TBzTDk0,2Sulfurl2,1Total 243,6aSolution styrene-butadiene rubber, extended with treated distilled aromatic extract (TDAE) oil, vinyl content 50 % mass fraction, styrene content 25 % mas

29、s fraction. Oil content is 37,5 % mass fraction referring to 100 parts of rubber or 27,3 % mass fraction referring to the oil-extended material, respectively.bSolution butadiene rubber, manufactured with neodymium catalyst, 96 % cis 1,4 content.cFor convenience, TESPT bis(3-triethoxysilylpropyl)tetr

30、asulfide may be added in the form of a 50:50 admixture with carbon black N 330. If such an admixture is used, no additional carbon black is used in the compound.dZinc oxide, indirect type, class B1a according to ISO 9298:19955, Table D.1.eStearic acid, stearic/palmitic 65/30, class B according to IS

31、O 83123.fTreated distillate aromatic extract.gN-(1,3-Dimethylbutyl)-N-phenyl-p-phenylenediamine.hWax, mixture of refined hydrocarbons.iN,N-Diphenylguanidine.jN-Cyclohexyl-2-benzothiazylsulfenamide.kTetrabenzylthiuram disulfide.lSulfur, soluble (rhombic), class W according to ISO 8332:20064, Table A.

32、1.4.1.3 Second stage Filling factor: 0,71. Rotational speed: 80 r/min. Starting temperature: 80 C. Friction: 1:1,11. Ram pressure: 0,55 MPa.The second stage procedure is given in a) to f) herafter.ISO 5794-3:2011(E) ISO 2011 All rights reserved 3BS ISO 5794-3:2011Duration mina) Plasticize batch from

33、 first stage. 0,0 to 2,0b) Maintain batch temperature of 160 C by adjusting the rotational speed. 2,0 to 5,0c) Discharge batch (batch temperature: 155 C to 165 C). 5,0d) Transfer to mill. e) Form a sheet for 45 s using a clearance of 4 mm between the rolls. f) Store compound for 4 h at room temperat

34、ure before proceeding to third stage. 4.1.4 Third stage Filling factor: 0,68. Rotational speed: 40 r/min. Starting temperature: 50 C. Friction: 1:1,11. Ram pressure: 0,55 MPa.The third stage procedure is given in a) to h) herafter.Duration mina) Add batch of second stage. 0,0 to 0,5b) Add DPG, CBS,

35、TBzTD and sulfur. 0,5 to 2,0c) Discharge batch (batch temperature: 90 C to 110 C). 2,0d) Transfer to mill. e) Form a sheet for 20 s using a clearance of 3 mm to 4 mm between the rolls. f) During the next 40 s, cut three times left, three times right, nip and pass the rolled batch twice endwise throu

36、gh the rolls using a mill opening of 3 mm.g) From the freshly prepared batch, form one sheet of the desired thickness. h) Store the sheet for at least 12 h at room temperature before cure. 4.2 Testing of the uncured mixDetermine the viscosity at 100 C using the shearing disc viscometer in accordance

37、 with ISO 289-1.ISO 5794-3:2011(E)4 ISO 2011 All rights reservedBS ISO 5794-3:20115 Evaluation of vulcanization characteristics5.1 Evaluation according to oscillating disc curemeter testMeasure the following standard test parameters:ML, MH, ts1, tc(50)and tc(90)in accordance with ISO 3417, using the

38、 following test conditions: oscillation frequency: 1,7 Hz (100 cycles per minute); amplitude of oscillation: 3 arc; 1 arc may be used if required; selectivity: to be chosen to give at least 75 % full scale deflection at MH; die temperature: 160 C; pre-heat time: none.5.2 Evaluation according to roto

39、rless curemeter testMeasure the following standard test parameters:FL, Fmaxat a specified time, ts1, tc(50) and tc(90)in accordance with ISO 6502, using the following test conditions: oscillation frequency: 1,7 Hz (100 cycles per minute); amplitude of oscillation: 0,5 arc; selectivity: to be chosen

40、to give at least 75 % full scale deflection at Fmax; die temperature: 160 C; pre-heat time: none.5.3 Evaluation according to stress-strain propertiesVulcanize the test slabs at 160 C for 15 min.Determine the tensile stress-strain properties stress at 300 % strain, stress at 500 % strain (if elongati

41、on at break exceeds 600 %), tensile strength and elongation at break in accordance with ISO 37 using type 2 test pieces.5.4 HardnessDetermine the hardness in accordance with ISO 48.6 PrecisionThe test precision may vary depending on the type of silica and on the rubber properties determined.ISO 5794

42、-3:2011(E) ISO 2011 All rights reserved 5BS ISO 5794-3:20117 Test reportThe test report shall include the following information:a) a reference to this part of ISO 5794;b) all details necessary for the identification of the sample;c) the test formulation used (Clause 3);d) the viscosity of the uncure

43、d mix (see 4.2);e) the cure characteristics (see 5.1 or 5.2);f) the stress-strain properties (see 5.3);g) the hardness (see 5.4);h) any operations not included in this part of ISO 5794 or in the International Standards to which reference is made, as well as any operation regarded as optional;i) the

44、date of the test.ISO 5794-3:2011(E)6 ISO 2011 All rights reservedBS ISO 5794-3:2011BibliographyISO 5794-1, Rubber compounding ingredients Silica, precipitated, hydrated Part 1: Non-rubber testsISO 5794-2, Rubber compounding ingredients Silica, precipitated, hydrated Part 2: Evaluation procedures in

45、styrene-butadiene rubberISO 8312, Rubber compounding ingredients Stearic acid Definition and test methodsISO 8332:2006, Rubber compounding ingredients Sulfur Methods of testISO 9298:1995, Rubber compounding ingredients Zinc oxide Test methodsISO 23529, Rubber General procedures for preparing and con

46、ditioning test pieces for physical test methodsISO 5794-3:2011(E) ISO 2011 All rights reserved 7BS ISO 5794-3:2011ISO 5794-3:2011(E)ICS 83.040.20Price based on 7 pages ISO 2011 All rights reservedThis page deliberately left blankBSI is the independent national body responsible for preparing British

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49、rateful if anyone finding an inaccuracy or ambiguity whileusing this British Standard would inform the Secretary of the technical com-mittee responsible, the identity of which can be found on the inside frontcover.Tel: +44 (0)20 8996 9001 Fax: +44 (0)20 8996 7001BSI offers Members an individual updating service called PLUS which ensuresthat subscri