• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
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  • 优先权
    • 专利摘要:
    RUBBER MIXTURE, including natural rubber or its mixture with butadiene rubber in the ratio of 70 80: 20-30, or its mixture with butadiene and styrene-butadiene rubber in the ratio of 30:25:45, soot, zinc oxide, a pair of naphthenic-aromatic oil, vulcanization accelerator, selected from the group: 2- (morpholinothio) benzthiazole, N, N -dicyclog xyl-benzthiazole 2 sulfenamide, N-cyclohexon1-benzt 1azol-2-sulfenamide and dimorpholodisulfide mixture in a ratio of 54.5: 45.5, 2-mercaptobeistiazole, 2,2-bis- (benzthiazole yl) -disulfide, and sulfur, characterized in that the purpose of thermal stability of rubber from this mixture, the latter additionally contains as a stabilizer a compound selected from the group: disodium salt of decametine pen-bis- (thiosulfate), disodium salt of hexamethylene-bis- (thiosulfate), disodium salt of pentamethylene-bis- ( thiosulfate), disodium salt of ethylene bis (thiosulfate) hydrate of disodium cyclohexylene-1,4-dimethylene-bis (thiolulfate), decamethylene-bis- (methylthiosulfonate), decamethylene-bis- (tolylthiosulfonate), sodium, sodium, disodium salt, decamethylene bis (tolithiosulfonate), sodium, disodium salt; -but octylphenyl ether, 4,4-bis (thiosulphate) sodium salt of n-Bu-. ts1-carboxy-sfir-bis- (thiosulfate), sodium salt of di-n-hexylsulfone-6,6-bis- (thiosulfate), sodium salt of amino-chloride-bis- (hexamethylene thiosulfate), sodium sal dimethylsilylbutanesulfonic acid, hexamethylene-bis- ( thiosulfate) -Y-
    公开号:SU1159491A3
    申请号:SU823463048
    申请日:1982-07-07
    公开日:1985-05-30
    发明作者:Жерар Моньотт Филипп
    申请人:Монсанто Ороп С.А. (Фирма)；
    IPC主号:
    专利说明:

    Kami in the ratio of 30:25:45
    Soot
    Zinc oxide
    Paraffin naphthenic aromatic oil
    Sulfur
    Vulcanization accelerator Thermal stabilizer specifiedPriority by features
    59491
    07.07.81. Signs related to the use as a heat stabilizer of the disodium salt hydrate of decamethylene bis- (thiosulfate), the disodium salt hydrate of hexamethylene bis- (thiosulfate), the disodium salt of pentamethylene bis- (thiosulfate), disodium salt of ethylene disodium salt thiosulfate), disodium salt hydrate cyclohexylene-1,4 dimethylene bis- (thiosulfate), decamethylene bis- (methylthiosulfonate).
    13.08.81. All ocTajibHjjie signs,
    one
    The invention relates to the production of rubber, in particular rubber with high heat resistance.
    A rubber mixture based on diene (natural and / or synthetic) rubber is known, including carbon black, zinc oxide, a vulcanization accelerator, petroleum oil (paraffico-naphthenic-aromatic) and sulfur, for example,
    the ratio of 100: 20-70: 5-10 3-5: 3-8 D
    The rubbers from this mixture are characterized by a low temperature of 5%.
    The purpose of the invention is to increase the thermal stability of rubber.
    The goal is achieved by the fact that the rubber skid., Including natural rubber or a mixture of it with butadiene in the ratio of 70-80: 20-30, or a mixture of it with butadiene and styrene-butadiene rubber in the ratio of 30:25 45j soot, zinc oxide, paraffin a naphthenic-aromatic vulcanizing accelerator masop selected from fpynnH: 2- (morphons), benzthiazole, N, N-dicyclohexyl-benzthiazol-2-sulfenamide, a mixture of N-cyclohexylbenzthiazol-2-sulfenes, and 19-sulfenamide mixtures 5, 2-mercaptobenzthiazole,
    2,2-bis- (benzthiazolyl) disulfide, and sulfur, additionally contains as a thermal stabilizer a compound selected from the group: disodium salt of decamethylene bis (thiosulfate) disodium salt, pentamethylene-bis- (thiosulfate) disodium salt hydrate, disodium salt of disodium hexameti2
    flax bis (thiosulfate), ethylene bis (thiosulfate) disodium salt hydrate, cyclohexylene-1, 4-dimethylene bis- (thiosulfate) disodium hydrate, decamethylene bis- (methylthiosulfonate), decamethylene bis (tolylthiosulfonate) , sodium salt of di-n-butyl ether-4, 4-bis- (thiosulfate) sodium salt of n-butyl-carboxy-ether-bis- (thiosulfate), sodium salt of di-n-hexylsulfone-b, 6-6HC- ( thiosulfate), sodium salt of amino-bis- (hexamethylene thiosulfate), sodium salt of dimethylsilyl butanesulfonic acid, hexamethylene-bis (thiosulfate) K- (1,1,3,3-tetramethylb util) -K-benzine salt; hexameti; Len-bis (thiosulfate) -Y-isopropyl-N- (p-phenylaminophenyl) ammonium salt, hexamethylene-bis- (thiosulfate) -1, 6-bis- (isothiourionium) hexane salt, its baryev 1 Hexamethylene-bis- ( thiosulfate), cobalt salt of hexamethylene bis- (thiosulfate), nickel salt of hexamethylene bis- (thio sulfate) zinc salt of hexamethylene bis- (thiosulfate), magnesium salt of hexamethylene bis (thiosulfate), calcium salt of hexamethylene bis (( thiosulphate), hexamethylene-bis- (thiosulfate) -N-tert.-butyl-M-benzylammonium salt, hexamethylene-bis- (thiosulfate) -2, 2,4-trimethyl-1,2-dihydrohi olinieva salt, sodium salt of poly (epihlorgidrintiosulfata), with the following ratio of components, May, h .:
    Natural rubber
    or its mixture with butadiene in the ratio of 70-80: 20-30, or a mixture of it with butadiene and styrene-butadiene rubber
    in the ratio of 30:25:45 100 Sazh40-60
    Zinc Oxide 5-10
    Refined Oil Oil2-10
    Sulfur 1,5-7,0
    Vulcanization accelerator 0, 5-1,1 Said thermostabilizer 0, 5-5 Example 1. The use of the vulcanization stabilizers according to the invention in natural rubber-based rubber.
    A masterbatch of the following composition is prepared, wt.
    Natural rubber 100 Carbon black 50 Zinc Oxide5
    Stearic acid 2 Para4 “but-naphthenic-aromatic oil 3 N-Phen l-H (1,3-dimethyl6yTH .ti) -n- einoteHAHaMH-H 2 The masterbatch is mixed with sulfur, C2-morpholinothio) -benzthiazole and a stabilizing compound in ratio, respectively, of 2.5: 0.7: 3 hours to 100 May. h of rubber. The stabilizer is introduced into the mixture as a suspension of finely ground solid in an equal amount of (refined oil) refined oil. For control, loading masterbatches are used, to which only sulfur and 2- (morpholinothio) benzothiazole are added,
    “In tab. 1 presentation, the properties of the known and proposed mixtures and rubbers based on them.
    In tab. 1 The following conventions are accepted;
    And monohydrate disodium salt decamethan-bis- (thiosulfate) j
    B - disodium salt hydrate hexamethylene-bis- (thiosulfate),
    C - pentamethylene bis bis (thiosulfate) disodium salt hydrate;
    D - disodium salt hydrate of ethyl ethyl bis- (thiosulfate),
    E - disodium salt hydrate cyclohexylene-1, 4-dimethylene bis- (thiosulfate).
    The effect of a hundred or a binding compound on aging is shown by comparison
    the percentage of voltage retention when the sample is elongated by 300% during the pre-vulcanization of the samples containing the stabilized compound (3 hours), compared with the control one. Stabilizing compound contributes to the preservation of elasticity.
    Example 2. The use of vulcanization stabilizers according to the invention O in a mixture of natural rubber with butadiene rubber.
    Masterbatch is prepared as follows.
    Natural rubber 70 5 Butadiene rubber 30
    Carbon black 50
    Zinc Oxide5
    Stearic acid 2
    Athena-naphteno steam aromatic oil 6
    N-Fvnil-K- (1,3-dimethylbutyl) -n-phenylenediamine 2
    Part of the masterbatches are selected and mixed with sulfur and 2- (morpholotho) benzthiazole in a ratio of 2.5 and 0.7 mash respectively, respectively. on 100 lu.ch rubber (control sample). The other part of the masterbatch is mixed with the same amounts of sulfur and 2- (morpholinothio) benzthiazole, as well as 3 parts by weight. decamethylene bis bis (thiosulfate) disodium salt (A) hydrate, which is introduced into the mixture as a dispersion of finely divided solid in an equal mass of the processed oil.
    In tab. 2 presents the characteristics of rubber-based mixtures in example 2.
    As can be seen from the table. 2, in the control sample, the voltage after 200 min of vulcanization was reduced to 88% of the maximum value, while the stress upon elongation by 300% of the mixture containing the stabilizing compound after vulcanization for 200 min was slightly higher than 0 voltage after 60 min vulcanization.
    Example 3. A control sample and samples containing 3 ma.h. a stabilizing compound, prepared 5 as indicated in example 1, from masterbatch.
    The test results are shown in Table. 3, where F is decamethylen-bisS11
    - (methylthiosulfonate) and C, β-decamegilene bis-Sp-tolylthiosulfonate).
    As can be seen from the data table. 3, stabilizers have a beneficial effect on stress upon elongation of the sample by 300%.
    Example 4; A mixture of the same composition as in Example 1 (but from a different batch of natural rubber) is used for the HYKJ complex.
    The masterbatch is mixed with a Banbury B mixer with sulfur, 2- (morpholino-thio) benzthiazole and a stabilizing compound in a ratio of 2.5 j 0.7 j 3 mas, respectively, per 100 May. rubber Another part of the masterbatch in which only sulfur and 2- (morpholinothio) benzthiazole are added is used as a control.
    The vulcanization characteristics of the mixtures obtained and the physical properties of the rubber obtained on their basis are determined.
    The test results are presented in Table. 4, where you accept the following conventions; A. - sodium salt of di-n-butyl ester-4,4-bis- (thiosulfate) j B - sodium salt of n-b util-carboxy-ester-bis - (thiosulfate); C is the sodium salt of di-n-hexylsulfone-x} ab-bis- (thiosulfate); D - sodium salt of amino-bis-bis- (hexmethylenethiosulfate).
    As can be seen from the table. 4, rubber mixtures 5 containing a stabilizer, have improved indicators (voltage retention, elasticity).
    Example 5. A masterbatch is used; a mixture of the same composition as in Example 1, but from another batch of natural rubber. Part of the masterbatch is mixed in a Banbury mixer with sulfur and 2- (morpholinothio) benzthiazole and a stabilizer in a ratio of 2.5, respectively. , 7.3.0 math. on too mac rubber
    Another part of the masterbatch, only sulfur is added to KOTopi o and 2- (morpholinothio) benzthiazole is used as a control.
    The vulcanization characteristics of the resulting deposits and the physical properties of rubber based on them are determined. The test results are given in Table. 5, where you accept the following legends:
    6
    A - sodium salt of dimethylsilyl butane sulfonic acid; J - hexamethylene bis (thiosulfate) -N- (1,1,3,3-tetramethylbutyl) -N-benzyl ammonium salt; C is hexamethylene bis- (thiosulfate) -Y-isopropyl-N- (p-phenylaminophenyl) ammonium salt; D - hexamethylene bis- (thiosulfate) -1, 6-bis- (isothiouronium) -hexane salt.
    As can be seen from the data table. 5, that the rubber containing the stabilizer retains the voltage during pereuvlanisadia, the compound B exhibiting good activity at a relatively low concentration (1.7 parts by weight per 100 parts of rubber). Fatigue properties are particularly well manifested when compound C is used,
    PRI me R 6. Use uterine mixture of the same composition as in example 1, but from a different batch of natural rubber. In the Banbury mixer, a portion of the masterbatch is mixed with sulfur, 2- (morpholinothio) benzthiazole and a stabilizing compound in a ratio of, respectively, 7: 3 ma.h at 100 May. h, rubber. The part of the masterbatch, in which only sulfur and 2- (morpholinothio) benzthiazole are introduced, is used as a control.
    The vulcanization characteristics of the compositions obtained are determined, as well as the physical properties of rubbers based on them.
    The results are shown in Table. 6, where the following conditional abbreviations are accepted: A — hexamethylene-bi- (thiosulfate) barium salt; B — hexamethylene bi- (thiosulfate) cobalt salt; C - hexamethylene bi- (thiosulfate) nickel salt; D - hexamethylene-bi- (thiosulfate) zinc salt; E - hexamethylene-bi- (thiosulfate) magnesium salt;
    F - hexamethylene-bi- (thiosulfate) calcium salt.
    As can be seen from the table. 6, the presence of a stabilizing compound provides good retention (or even an increase) of stress upon elongation of 300% of the sample upon re-vulcanization; the preservation of elasticity is also higher than in the control sample, when perecannula; the rupture time determined during the tests on the Goodrich flexometer also increases with pere-vulcanization in all samples, except for the control one. This increase is particularly noticeable for rubbers based on mixtures of compounds containing B, C, D, E (salts of cobalt, nickel, zinc and magnesium). Example 7. A masterbatch of the same composition was used as in Example 1, but prepared from another batch of natural rubber. A part of the masterbatch is mixed with sulfur, 2- (morpholinothio) benzthiazole and a stabilizing compound in a ratio of 2.5, 0.7: 3 mash, respectively. on May 100, h rubber The mother bed for the mixture in which only sulfur and 2- (morpholinothio) benzthiazole are added is used as a control. The vulcanization characteristics of the compositions obtained and the physical properties of rubber based on them are determined. The results are shown in Table 7, where the following conditional carts are accepted. : A - hexamethylene bis (thiosulfate -N-tert.-butylbenzyl ammonium salt salt; B - hexamethylene bis (thiosulfate -2,2,4-trimethyl-1,2-dihydroquinoline salt; C - sodium salt of poly- (epichloro hydrin) -thiosulfate. Samples containing {stabilizing substances, in all cases have a greater percentage of preservation than the control sample (see Table 7). Examples 8-14. Prepared matrices mixtures, E which are entered below are vulcanization accelerators and the stabilizer I, Example 8. The mixture contains, May, h,: Natural rubber100 Soot55 Shchshka oxide8 Stearic acid ta2 Paraffin-iafeno rum, ch1i chseo o oil 3 V.cuitiCTPo; |, l, 1 (5k of K..lfM) .TH3 H-Phenyl-I- (1,3-dimethylbutyl) -n -Phenylenediamine 2 Poly (1,2-dihydr D-2,2, A-trimethylquinolin1) EXAMPLE 9, Preparing a mixture, as a reamer 1 but without a stearic pussy, Example 10, Preparing a masterbatch, as in the example 1, but with the use of a mixture of natural rubber Mac.h,) and polybutadiene Cahua (20 mas.ch,) instead of natural chuka. Example 11. Prepare uterine mat of the following composition, mac.h .: Natural rubber100 Soot 40 Zinc oxide 10 Stearic acid1 Paraffino - naphthenic-aromatic oil3 Н-Phenyl-K- (1,3-d imethylbutyl) -n-phenylenediamine2 Clump product2 Silica 10 Example 12. Prepaid uterine trail of lean composition, May, h,: Natural rubber Polybutadiene rubber Styrene-butadiene rubber, filled with oil (37.5%) 67.5 (45 rubber, 60) Oxy zinc Stearic acid Paraffin-naphthenic-aromatic maelo10 K-Phenyl-K- (1,3-dimethylbutyl) -n-phenylenediamine2 Poly (1,2-dihydro-2,2,4-trimethylquinoline) 1 Example 13. Preparing a masterbatch Subscribe to the following composition, May, h .: Natural rubber 100 Soot 50 Zokia zinc5 Stearinova kielota2 Paraffin-naphthenic-aromatic mael 3 N-Phenyl-N- (1,3-dimethylbutyl) -p-fennlendiamin 2 Example 14 is prepared following matochemee soetala, May h .: maturSh1iy Rubber 100 Carbon Black 30 Zinc Okie H 9P Stearic acid. Paraffin-naphthenic-aromatic-3 oil Thermal stabilizers used in examples 8-14: 1 - disodium salt hexamethylene bis (thiosulfate) hydrate 2 - hexamethylene bis bis (thiosulfate) nickel salt hydrate; 3- Decamethylene bis (thiosulfate) disodium salt hydrate ,, Vulcanization accelerators used according to examples 1 „2- (morpholinothio) benzthiazole 5 2-M, M-dicyclohexyl-benzothiazole-2-sulfenamide Rubber mixtures, including Characteristics
    Vulcanization time at
    14 ° C, min
    Elongation stress
    by 300%, MPa Fatigue failure at a voltage energy of 1 mPN; kilo-cycles Stress retention during perevulkanization, 5 Decrease in endurance during repeated deformations as a result of perevulkanization,%
    Time to vulcanize
    t40Cj min60
    Scrubbing at lengthening
    300% MPa
    Fatigue damage at a stress energy of 1 MPa, kilocycles
    Voltage saving
    during perelevkulizacin,%
    Reduction of endurance during repeated deformations 8 as a result of over-vulcanization,% 59491 heck 45, 5 their vayu sv 15 beat (in the Prototype
    4020060200 60200
    14,011,014,414,2 13,3 12,7
    151121
    84
    98,695,5
    20
    200 60
    60 200
    200
    13.9 13.3 15.4 14.0
    13.9 12.7
    91, 4
    91.0 10 3 - mixture of 54.5 wt.%. N-cyclosylbenzthiazole.-Sulfenamide and 5 Bes.% Dimorpholine indisulfide; 4- 2-mercaptobenzthiazole, 5-2,2-bis- (benzthiazolyl) disulphages. The composition of the mixtures and the properties of rubbers on the basis are presented in table. 8. (The re-cured sample is heated for 240 minutes), presented in table. 8, these data show an increase in the thermal temperature of rubbers from the proposed mixture compared with the prototype). iT a bl and c a 1 tabilizatr
    Specifications
    The vulcanization time at 140 ° C, min
    Stress at elongation by 300%, mPa Vulcanization time at, min 40 200 Stress at elongation 16.0 13.0 at 300%, mPa 68.9 57.9 Elasticity,% Stress retention during perevulkanizatsiya,% Storing elasticity during reculcanization, / Cure time at, min 42 200 60 200 Stress at elongation by 300%, MPa 16.0 14.2 16.5 16, Elasticity, 66.7 58.5 68 62 Stress retention during reculcanization % Retention of elasticity during perevulkanization,%
    L lj d 3 2
    Rubber containing stabilizer A
    200
    60
    50
    200
    126
    122
    126
    111 17.9 17.5 17.718.1 68.661.2 60 200 45 200 40 200. 16.1 17.1 15.6 15.6 17.2 16.4 63.6 62.9 60.5 58.5 65.0 58.5 106.2 100.0 95.3 96.7 90, 0
    with I s
    with me
    ABOUT
    ABOUT
    go
    KS
    aiaJ
    EC
    &but.
    O) d
    O) S
    оs tа and vulcanization time at 1D ТС | MINH 40 200 Voltage at lengthening by 16.1 14.2 15, 300%, mPa Storing the voltage during perevulcanization,% 45 200 60 200 45 200 16.2 13.9 14 3 15.3 15.0
    权利要求:
    Claims (1)
    [1]
    . RUBBER MIXTURE, including natural rubber or its mixture with butadiene rubber in the ratio of 70-80: 20-30, or its mixture with butadiene ^ and styrene-butadiene rubbers in the ratio of 30:25:45, carbon black, zinc oxide, paraffin-naphtheno- aromatic oil, vulcanization accelerator, selected from the group: 2- (morpholinothio) benzthiazole, N, N 1 -dicyclo-xyl-benzthiazole ~ 2-sulfenamide, a mixture of Y-cyclohexyl-benzothiazole-2-sulfenamide and dimorpholinodisulfide in the ratio of 54.5: 45.5, 2-mercaptobenzthiazole, 2,2'-bis- (benzthiazole yl) disulfide, and sulfur, characterized in that, for the purpose to increase the thermal stability of rubbers from this mixture, the latter additionally contains as a thermal stabilizer a compound selected from the group: decamethylene bis (thiosulfate) disodium salt, hexamethylene bis (thiosulfate) disodium salt, pentamethylene bis (thiosulfate disodium salt hydrate) ), ethylene bis (thiosulfate) disodium salt hydrate (cyclohexylene-1,4-dimethylene bis (thiosulfate) disodium salt, decamethylene bis (methylthiosulfonate), decamethylene bis (tolyl thiosulfonate), di- sodium salt n-butyl ether p-4,4-bis- (thiosulfate), sodium salt of n-butyl-carboxy-ether-bis- (thiosulfate), sodium salt of di-n-hexylsulfone-6,6-bis- (thiosulfate), sodium salt of ammonia chloride- bis- (hexamethylene entiosulfate), sodium salt of dimethylsilyl-butanesulfonic acid, hexamethylene-bis- (thiosulfate) -M- (1,1, -3,3-tetramethylbutyl) -Y-benzylammonium salt, hexamethylene-bis- (thiosulfate) -Ν -Η3οπροπηπ-ν '- (p-phenylaminophenyl) ammonium salt, hexamethylene bis (thiosulfate) -1,6-bis (isothiouronium) hexane salt, hexamethylene bis (thiosulfate) barium salt, cobalt hexame salt ethylene bis (thiosulfate), nickel salt of hexamethipene bis (thiosulfate), zinc salt of hexamethylene bis (thiosulfate), magnesium salt of hexamethylene bis (thiosulfate), calcium salt of hexamethylene bis (thiosulfate), hexamethylene bis - (thiosulfate) -N-tert-butyl-N-benzylammonium salt, hexamethylene bis (thiosulfate) -2,2,4-trimethyl-1,2-dihydroquinolinium salt, sodium salt of poly (epichlorohydrinthiosulfate), in the following ratio of components , ma.ch .:
    Natural rubber or its mixture with butadiene rubber in a ratio of 70-80:: 20-30 or its mixture with butadiene and styrene-butadiene rubber SU a 1159491 in the ratio
    30:25:45 one hundred Soot 40-60 Zinc oxide 5-10 Paraffin-naphtheno-aroma tic oil 2-10 Sulfur 1.5-7.0 Vulcanization accelerator tions 0.5-1.1 Indicated thermo stabilizer- 0.5-5.0
    Priority by signs:
    07/08/81. Signs related to the use of decamethylene bis (thiosulfate) disodium salt, hexamethylene bis (thiosulfate) disodium salt, pentamethylene bis (thiosulfate) disodium salt, ethylene bis disodium salt as a thermal stabilizer (thiosulfate), disodium salt of cyclohexylene-1,4 dimethylene bis- (thiosulfate) disodium, decamethylene bis- (methylthiosulfonate).
    08/13/81. All other signs
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    同族专利:
    公开号 | 公开日
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    EP0070143B1|1985-02-20|
    IE821638L|1983-01-08|
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    US4417012A|1983-11-22|
    IE53303B1|1988-10-12|
    AU8563982A|1983-01-13|
    NO160847C|1989-06-07|
    NO160847B|1989-02-27|
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    UA5970A1|1994-12-29|
    US4587296A|1986-05-06|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    GB8121098|1981-07-08|
    GB8124716|1981-08-13|
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