• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A process for obtaining improved rubberized silicate calcium or silicates vulcanizates, comprising preparing a mixture of a polymer, silica or calcium silicate and an additive, subjecting said mixture to a treatment in which it is sheared at a temperature from about 100 ° to about 175 ° C, cooling said mixture, incorporating vulcanizing active compounds into said mixture and curing by heating at an elevated temperature to produce the rubberized vulcanizate loaded with silica or improved calcium silicate.
    公开号:SU971106A3
    申请号:SU782603400
    申请日:1978-04-13
    公开日:1982-10-30
    发明作者:Камерон Эдвардс Дуглас；Сато Киосаку
    申请人:Полисар Лимитед(Фирма)；
    IPC主号:
    专利说明:

    The invention relates to the plastics industry and relates to the development of a method for the elimination of elastic rubbers. A known method for producing elastic rubbers by mixing hydroxyl-containing rubber with a filler and a vulcanizing agent 1. However, the known method does not improve the physico-mechanical properties of the vulcanizates. The purpose of the invention is to improve the physical and mechanical properties of the vulcanizates. This aim is achieved in that in the method for producing the elastic re zin mixing lsoderzhashego hydroxy Reflexion nitepem rubber and curing agent are mixed with acrylonitrile-butadiene copolymer or styrene and hydroxyl silakrilytom selected from the group hydroxyethyl acrylate, hydroxyethyl methacrylate, oksipropilmetakripat Content at 0.25- 5 wt.% with 0.5-3 wt.h. organic amine selected from the group: dodepipamine, N, N -methyloctadecylamine, di (pre-decyl) amine, hexamethiandiamine, tri-thylamine triisooctylamine, benzylamine, octadechyllamine, (NHP) (CH) MH with 1.5-2, 0 weight.h. Compounds selected from the group: sodium stearate, potassium stearate, zinc stearate, calcium stearate, ammonium stearate, ammonium silicate, stearic acid, oleic acid, 1-10 weight.h. magnesium oxide with 50-60 weight.h. calcium silicate silicate silicate for 1-3 min at 10 ° –150 ° C under shear force, followed by vulcanization at 160–166 ° C for 15–30 min. Example 1. An emulsion preparation at 13 ° C is prepared. A polymer containing 34% by weight of acrylonitrile and 1% by weight of hydroxyethyl methacrylate. The control polymer is butadiene-acrylonitripe polymer containing 34 wt.% Acrylonitripe. The polymers are mixed on rollers. In experiments 1A and 2A, polymers are mixed with 50 parts by weight. silica and 1.5 wt.h, dodecylamine, after which they are subjected to rolling at 150 ° C | In experiment 1B, the polymers are mixed with
    39711064
    60 Weight.h, capicum sipikata, and in experimentalum. Polymete 2B mixture filled with 1.5 parts by weight substances / gteepT measure is rolled out and vulcanized on a press. Then roll for 3 minutes in a mixture at 16Q ° C for 30 minutes.
    150 ° C, Ohpazhduyug and Vaga: tsuet with com-properties of vuccanizates predgsgavpeny
    tabuyu temperature together with perki- s in tab. one.
    Table 1
    Content of hydroxyethylmethacrylate, wt.% .OO Content of dicumyl peroxide, wt.% 3.54.0 Properties Strength at stretching, kgf / cm 266141 Elongation,% 52044 O Stress at elongation, kgf / cm
    Example 2. Polumery containing butadiene, acryponitrile, hydroxyethyl methacrylate, is prepared according to example 1, the ratio (total) of butadiene and hydroxyethyl megacrylate is 66% by weight, and the content of the bound 50 hydroxyethyl methacrylate is 0.25-5 weight .%.
    Per 100 weight parts Polymer Apply dodecylamine in the amount of 1.5 parts by weight According to Example 1, mixtures and samples are prepared for testing. Filled polymers are vulcanized at 16 ° C for 30 minutes.
    The properties of the vulcanizates are presented in table. 2. 11 3,04,0 318173 55О370
    Example 3. Popimer from the example of SO weight, h. polymer Peroxide is used.
    1 in Experiment 2 with the content of a hydrated 55-Cum Vallet at 150 ° C for
    hydroxyethyl methacrylate in the amount of 1 wt.% 3 min. Vuccinate at ieO ° C in a mixture with amines instead of octadecine ZO-min.
    amine from experiment 2A in example 1. Properties of vuccinates are represented by
    Amines are added in the amount of 1.5 parts by weight. Nav Tabg, 3.
    Table
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    Example 4. The polymer composition according to example 1 is mixed, thermoablative and vupkanizuyut. The properties of the vulcanizates are determined. As amine, dodecapamine is used in the amount of 5 1.5. Dicumine peroxide is used. on in the amount of 3.5 wt.%. For the experiment 35 100 weight.h. the polymer is mixed in a mixer with 5O weight.h. silica, 10 weight.h. dioctylphthate and
    Strength at stretching, kgf / cm
    Elongation,%
    Elongation stress, kgf / cm
    Table 5
    Strength at
    stretching, kgf / cm 320342
    Elongation,% ZZO490
    1.5 weight. h. A gte en T. First, the mixing temperature is 9 ° C, and the mixing is continued for 8 minutes without adjusting the temperature, which reaches 139 ° C by the end of 8 minutes. After cooling, the mixture is stirred on a vapor at room temperature with 4 parts by weight. per se dicumip and vulcanized.
    The properties of the vulcanizates are presented in table. four.
    i a b p and c a 4
    260 275
    239 51О 530 670
    thirty
    36,271,141

    cm 274 BUT
    9 6 81 87
    1197110612
    Example 6. Prepared for polymoxypropylmethacrylate. The amount of resilience according to Example 1 (the experiment of dicumip is 4 wt.% (SP 2). The silica content of the experiment. 57 - 1.5 wt.%). As a part, 50 weight.h, for 1OO weight.h. amine-amine use ArmeeriT, Wuppimer Blend. Dp experiment 56 popimer 5 scan when for 30 minutes, contains 1 wt.% Hydroxyethypate, Properties of vuccinates are presented and dp experiment 57-1 wt.% 2-hydr-in table. 6
    The amount of amine, wt.h.
     Properties
    Strength at stretching, kgf / cm
    Elongation,%
    Elongation stress,
    CGS / SM
    Example 7. A mixture of po-3S and 1.5 weight parts is prepared. dodenylamine. Mixes
    Pimera Containing 34 wt.% Acrylonite-heat treated at 150 ° C in
    rila, 61 wt.% butadiene and 5 wt.% hydr-for 3 min according to example 1. In
    hydroxyethyl methacrylate. Prepare a mixture from the mixture add dicumyl peroxide and
    industrial acrylonitrile butadiene-vulcanized at 160 ° C for 30 minutes th polymer containing 34 wt.% AC- 40
    riponitrile with a Mooney viscosity of 50. The mixtures and vulcanization properties of the mixtures contain 50 parts by weight. Creme dioxide is given in Table. 7, iOO 95. Akryponitripbutadiene, wt.h. Acrylonitrile butadiene hydroxy05 ethyl methacrylate, wt.h, O 0.25 Hydroxyethylmethacrylate, wt.% 54 Dicumyl peroxide, wt.%
    Table
    3.0
    1.5
    1.5
    301 282
    231 370 34O 430
    .Table 7 10 0.5 4
    13
    Properties
    Strength at stretching, kgf / cm
    elongation,%
    Elongation stress, kgf / cm Example 6. The compositions of the mixtures are presented in Table. S. Control - butadiene 30
    acrylic is a pony polymer containing 34% by weight acrylonitrile with a Muni viscosity of 5O. In the sample composition according to Example 7, amine is added in an amount of
    Polymer Composition and Vulcanization Conditions
    Butadiene Acrylonitrilsch
    polymer weight.h.100
    The polymer composition according to example 7
    Silicon dioxide, parts by weight Dioctyl phthalate, wt.h.
    AgteePT, weight.h. Zinc oxide, wt.-i. Stearic acid, parts by weight
    Benzothiazopyl difyrupid,
    weight parts
    14
    97,1106
    Continued tab, 7
    242,275
    255,235
    235 300 39О 37О 390 440
    ingredients are administered at 35-40 C.
    The properties of the vulcanizates are presented in tab. 9.
    Table 8
    Experiment
    71
    72
    70
    1,51,5 1,5 weight,%, process on vaptsah at during within 3 min. Rest
    15
    97110616
    Tetrametiptiuramdisufid,
    weight. h
    Sulfur, by weight
    Salicylic acid, weight, h.
    The time of sub-evaporation at ° 125 ° С, min
    Vulcanization at
    Vulcanization properties
    Strength at stretching who / cm
    Elongation,%
    Elongation stress, kgf / cm
    by 1OO% to ZOO%
    Yunta module, kgf / cm Residual elongation,% Shore hardness, A2
    Example 9. Polymer styropbutamine hydroxymegyl methacrylate with a content of 0.5 wt.% Hydroxyethyl megacrylag In 23 wt.% Styrene is mixed with 5 Owe% silicon dioxide and 1.5 wt.% Arfneen T ,. Rolled at for 3 min.
    Continued table. eight
    0,50,5
    1,751.75
    1.0
    6.5
    20 15 15
    Table 9
    Experiment
    71
    70
    72
    273
    273 58О 56О
    17
    15 89
    98
    65 13 75
    76 13 75
    at room temperature, mixed with dicumyl peroxide and vulcanized for 30 min. The properties of vugsanizates are presented in Table 1O, where hot rolling is used in experiments with VO-81.
    The content of dicumyl peroxide, wt.%
    Properties Strength at growth of 1 .0
    0.67 0.67
    nineteen
    Young's modulus, kgf / cm Residual elongation,% Shore hardness, A2
    Example 11. The polymer composition according to Example 1 is mixed with silicon dioxide and additives on Wapes at 150 ° C for 3 minutes. Mixed with
    The content of dicumide peroxide, wt.%
    Properties
    Strength at growth Note. I20
    971106 Continued table. eleven
    1465948
    847
    808075
    peroxide of dicumip and vulcanized at 160 ° C for 30 minutes.
    The composition of the polymer and the properties of the vuccinaeates are presented in tab. 12.
    Table 12 Sodium stearate, m - potassium stearate, III - calcium stearate, IV - zinc stearate, V - ammonium stearate, Y - stearic acid, VII - P-toluenesulfonic acid.
    Note 12. The composition of the composition according to example 1 is mixed with 60 parts by weight. DV silica, 15 weight.h. dioctipphate and 2 weight.h. additives. Rolling is carried out at 150 ° C for 3 minutes, after cooling the mixture at 40 ° C.
    Strength at stretching, kgf / cm
    dt, weight.h. zinc oxide 5; stearic acid 1,5; benethiaeopigispuid 1,5 {tetrametiptiuramdisufid 0,5; sulfur 1.75. Vulcanize the mixture for 15 minutes. The properties of vuccinae are presented in table. 13. Ta b p and c a 13
    333
    294.
    274
    311, 341
    420 45О
    Elongation,%
    Tension at lengthening, kgf / cm As can be seen from tab. 1-14, the properties of the eucalyptses based on the mixtures proposed are significantly superior to those of the erythrocytes based on industrial rubbers and vulcanizates in contrast to examples. Formula of the invention. A method of obtaining elastic rubber by mixing a hydroxyl-containing rubber with a filler and a rubberizing agent, characterized in that, in order to improve the physical and chemical properties of the vulcanizates, the copolymer of butadiene is mixed with acrylic polyl or styrene and hydroxylacrylate selected. from the group: hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypopimethacrylate, with a content of 0.25-5 wt.% with 0.5-3 weight.h. OrContinue table. 14
    320
    360
    350 ganic amine selected from the group: dodecylamine, N, N -dimetypoctadecylamine, de {dodecyl) amine, hexamethylenediamine, trioctylamine, triisooctipamine, benzylamine, octadeiyl amine, C, T. (NHP) (CH2) NH2, 1.5-2.0 parts by weight a compound selected from the group; sodium stearate, potassium stearate, zinc stearate, calcium stearate, ammonium stearate, ammonium silicate, stearic acid, opeic acid, with 1-10 weight.h. magnesium oxide, with 50-60 weight.h. silicon dioxide or calcium silicate for 1-3 minutes at 1OO-150 ° C under shear force, followed by vulcanization at 16O- for 15-ZO minutes. Sources of information taken into account in the examination 1. British patent No. 1383390, cf. From 08 to 3/34, publ. 1975 (prototype).
    权利要求:
    Claims (1)
    [1]
    Claim'
    A method for producing flexible 'hydroxy psoderzhaschego rubbers by mixing rubber with a filler i.vulkanizuyuschim agen- 35 is characterized in that, with a chain of improving the physicochemical properties of the vulcanizates were mixed sopopi measures · butadiene with acrylonitrile or styrene and gidroksilakrilatom selected. '40 from the group oksietilakripat, oksietipme- takripat, oksipopimetakripat, when the content of 0.25-5 wt% with 0.5-3 parts by weight. an organic amine selected from the group: dodecylamine, N, N-dimethipoctadecylamine, di (dodecyl) amine, hexametipene · diamine, trioctipamine, triisooctipamine, benzylamine, octadecylamine, C lv N E5 MH 1 '(NHP) = (CH 2 ) NH 2 , s 1.5-2.0 parts by weight compounds selected from the group: sodium stearate, potassium stearate, zinc stearate, calcium stearate, ammonium stearate, ammonium silicate, stearic acid, oleic acid, from 1-10 parts by weight magnesium oxide, with 50-60 parts by weight silicon dioxide or calcium silicate for 1-3 min at 100-150 ° C under shear, followed by vulcanization at 160 160 ° C for 15-30 min.
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    同族专利:
    公开号 | 公开日
    DE2816065A1|1978-10-26|
    ES468275A1|1978-12-01|
    FR2400532A1|1979-03-16|
    MX149286A|1983-10-10|
    BR7802236A|1978-12-26|
    AR221483A1|1981-02-13|
    AU521489B2|1982-04-08|
    SE7804127L|1978-10-15|
    SE439923B|1985-07-08|
    NL7803767A|1978-10-17|
    TR19890A|1980-04-09|
    FR2400532B1|1982-01-29|
    IN147279B|1980-01-12|
    GB1601434A|1981-10-28|
    AU3492978A|1979-10-18|
    JPS53128647A|1978-11-09|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4357432A|1981-05-11|1982-11-02|Polysar Limited|Vulcanizates|
    ES2028101T3|1986-11-11|1992-07-01|Imperial Chemical Industries Plc|A COMPOSITION THAT INCLUDES A CARBOXYLIC ACID AND AN AMINE.|
    EP0806452A4|1995-01-23|1998-05-13|Nippon Zeon Co|Rubber composition and process for preparing the same|
    US5939493A|1997-03-11|1999-08-17|Bridgestone Corporation|Pneumatic tire|
    EP0864604A3|1997-03-11|1999-01-13|Bridgestone Corporation|Rubber composition|
    FR2984896B1|2011-12-21|2014-10-24|Michelin Soc Tech|PNEUMATIC COMPRISING A COMPOSITION ESSENTIALLY FREE OF GUANIDIC DERIVATIVE AND COMPRISING PRIMARY AMINE|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    CA276,216A|CA1100659A|1977-04-14|1977-04-14|Vulcanizates containing siliceous fillers|
    CA276,217A|CA1096084A|1977-04-14|1977-04-14|Siliceous filled vulcanizates|
    CA276,224A|CA1094721A|1977-04-14|1977-04-14|Vulcanizates containing silica|
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