CN1048023C - 硫化或半硫化橡胶的快速再生方法 - Google Patents

硫化或半硫化橡胶的快速再生方法 Download PDF

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CN1048023C
CN1048023C CN93112734A CN93112734A CN1048023C CN 1048023 C CN1048023 C CN 1048023C CN 93112734 A CN93112734 A CN 93112734A CN 93112734 A CN93112734 A CN 93112734A CN 1048023 C CN1048023 C CN 1048023C
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路易·卡洛斯·奥利维亚·达·村哈·利马
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Abstract

本发明揭示了通过使用合适的溶剂溶胀橡胶块，并限制其与或存在于有毒或脱硫化学组份中来“快速再生硫化或半硫化橡胶的方法”。
该过程可在比常压高或低的压力下，以冷或热的方法进行。
该过程可使用任何类型的硫化或半硫化橡胶组合物。
由此过程可获得比那些由干燥或研磨过程获得再生产物具有更低价格的再生产物。

Description

硫化或半硫化橡胶的快速再生方法
本发明涉及通过使用合适的溶剂溶胀橡胶块，并通过其与或存在于有毒的或脱硫化学组份中的限制来再生硫化或半硫化橡胶的方法。
所有工业上的方法为了降低其费用，增加其效率而使用更廉价的原材料，并增加其副产物的利用价值。回收工业的发展方向是寻求提供具有更低成本和改进质量的能使用配方的方法，显而易见的是，越接近原始配方的性能，所得再生产品的质量就越好。
PI-8500981中所描述的方法披露了使用有毒试剂作为溶胀橡胶块的溶剂，它描述了使用研磨机的方法，其中使用了某些有毒的化学产物同时完成了橡胶粒子的还原。该方法与使用同样的配方的常规方法所获得的产品相比，能以更低的成本获得更高质量的再生产品，常规方法是用热作为再生剂(浸煮器或压热器)并配以机械研磨(精制机)的方法。
进一步的专利和在巴西专利PI-8500981，即专利GB1334718，US2088920，US4156508，BR7606727和GB505156，其它专利及集中在澳大利亚的PC9715中所述的方法，所有的这些专利全都使用溶胀以减弱橡胶强度，以使其中的补强成份，如纤维和金属线更易分离。在澳大利亚的方法中，尽管并未使橡胶再生，它只是将颗粒的尺寸降至0.3-0.8mm。由该过程获得的橡胶只作为其它配方中的载体。
本发明所涉及的整个橡胶(硫化或半硫化)的再生方法比巴西专利PI8500981更快，因为橡胶再生是与或是在有毒化学品中进行，在加工的同时，在过滤阶段进行颗粒还原，而不是偏重于研磨。当在压力下通过限制橡胶的情况下，会使橡胶尺寸减小，同时与有毒组份接触，随后将压力降至更低的压力，由于溶胀橡胶颗粒的溶剂产生闪蒸就会引起橡胶的第二次断裂。若每次重复此限制过程的橡胶颗粒尺寸越小，则每次获得的再生作用就越大，越均匀，且性能就越接近于原始的橡胶配方。
使用毒性组份的橡胶脱硫活化剂可改善再生性能并提高过程速度。所用的脱硫剂：胍及其衍生物如二苯基胍；肼及其衍生物如苯肼；苯胺类如苯胺等。其它较多使用的脱硫剂为油脂酸衍生物，有机金属配位化合物的混合物，异生(allogenated)衍生物，如五氯硫代苯，苯甲酸，苯二酸酐等。在该同样的过程顺序中，当橡胶配万被溶胀并由于限制作用而断裂时，可加入其它物质如增塑剂，树脂，载体，抗氧剂，促进剂，熟化剂等。这样获得的糊状的或稠厚的油在合适的干燥器中进行干燥，就可将溶剂回收并可再行使用。
本发明的限制包括一种或多种钻孔金属板，或筛网，或海绵，或多孔金属板，或任何其它的相同类型的或将它们组合起来使用的限制。
本发明过程可使用任何类型的硫化，半硫化，熟化，半熟化橡胶组合物进行。
本发明过程可以冷或热的方式来进行。
本发明过程可在比常压高或低的压力下进行。
实施例1   由下述天然橡胶配方制备：
    天然橡胶                           100.00
    氧化锌                             5.00
    硬脂酸                             2.00
    炭黑N-330                          45.00
    BLE抗氧剂                          1.00
    芳香油                             4.00
    促进剂(亚磺酰胺)                   0.60
    硫                                 2.50
硫化                30分                  145℃
拉伸强度           Pa(kg/cm2)            2.85×107(285)
300％模量          Pa(kg/cm2)            1.15×107(115)
断裂时的伸长       ％                    500
硬度               肖氏A                 65再生
样品1：        纯再生高弹体NR
样品2：        再生高弹体NR              100.00
               促进剂(亚磺酰胺)          0.30
               硫                        1.25
                                         101.55
硫化           30分                      145℃
                          样品1          样品2拉伸强度        Pa(kg/cm2)   1.5×107(150)  1.9×107(190)30％模量        Pa(kg/cm2)   9.5×106(95)   1.05×107(105)断裂时的伸长        ％          480          400硬度               肖氏A        65           67实施例2    由下述丙烯腈橡胶配方制备：
Hycar 1042                         100.00
氧化锌                             5.00
硬脂酸                             1.50
炭黑N-550                          30.00
炭黑N-762                          40.00
磷酸三                             7.00
环氧化蓖麻油                       8.00
促进剂(TMTMS)                      0.60
硫                                 1.00
                                   193.10
硫化          30分                   155℃
拉伸强度     Pa(kg/cm2)              1.6×107(160)
300％模量    Pa(kg/cm2)              1.5×107(150)
断裂时的伸长  ％                     330
硬度          肖氏A                  62
再生
样品1：    纯再生高弹体NBR
样品2：    再生高弹体NBR             193.00
           促进剂(TMTMS)             0.30
            硫                       0.50
                                     193.80硫化                        30分          155℃
                        样品1         样品2拉伸强度    Pa(kg/cm2)     8×106(80)    1.1×107(110)300％模量   Pa(kg/cm2)     6×106(60)       -断裂时的伸长    ％           300          260硬度           肖氏A         62           65实施例3    由下述CR橡胶配方制备：
Neprene W                      100.00
氧化锌                         5.00
氧化镁                         4.0
硬脂酸                         1.0
炭黑N-110                      30.00
环烷酸                         4.00
氧茚树脂                       4.00
凡士林                         2.0
Banox H                        2.0
TMTMS                          0.60
DPG                            0.60
硫                             1.00
                               154.20
硫化            30分             155℃
拉伸强度     Pa(kg/cm2)           2.55×107(255)
300％模量    Pa(kg/cm2)           1.1×107(110)
断裂时的伸长    ％                520
硬度          肖氏A               66
再生：
样品1：    纯再生高弹体CR
样品2：    再生高弹体CR           154.00
           TMTMS                  0.30
           DPG                    0.80
           硫                     0.50
                                  155.60硫化                       30分         155℃
                       样品1        样品2拉伸强度    Pa(kg/cm2)   1.5×107(150) 2×107(200)300％模量   Pa(kg/cm2)   8×106(80)    1.4×107(140)断裂时的伸长    ％         500          410硬度           肖氏A       66           68实施例4    由下述SBR橡胶配方制备：
SBR1502                             100.00
氧化锌                              4.00
炭黑N-672                           25.00
Banox H                             1.00
Santocure                           1.80
TMTD                                1.30
TETD                                1.30
                                    134.40
硫化           20分                 155℃
拉伸强度    Pa(kg/cm2)              1.55×107(155)
300％模量   Pa(kg/cm2)              3.9×106(39)
断裂时的伸长    ％                    700
硬度          肖氏A                   49
再生：
样品1：    纯再生高弹体SBR
样品2：    再生高弹体SBR              134.40
           Santocure                  0.90
           TMTD                       0.60
           TETD                       0.60
                                      136.50
                          样品1        样品2拉伸强度    Pa(kg/cm2)     6.5×106(65) 1.05×107(105)300％模量   Pa(kg/cm2)     1.5×106(15)  6.5×106(65)断裂时的伸长   ％             650          570硬度         肖氏A            49           52实施例5    由下述丁基橡胶配方制备：
Exxon丁基268                     100.00
氧化锌                           5.00
炭黑N-550                        25.00
炭黑N-762                        25.00
石蜡油                           10.00
TTD                              1.00
MBTS                             0.50
硫                               2.00
                                 168.50
硫化           20分              152℃
拉伸强度    Pa(kg/cm2)           1.1×107(110.00)
300％模量   Pa(kcg/cm2)          5.5×106(55.00)
断裂时的伸长    ％               400.00
硬度          肖氏A              52.00
再生
样品1：    纯再生高弹体IIR
样品2：    再生高弹体IIR        168.50
           TMTD                 0.50
           MBTS                 0.25
           硫                   1.00
                                170.25硫化                     20分        152℃
                     样品1       样品2拉伸强度    Pa(kg/cm2)  5×106(50) 7.8×106(78)300％模量   Pa(kg/cm2)  2×106(20) 5.2×106(52)断裂时的伸长    ％        360       310硬度           肖氏A      52        54实施例6    由下述BR橡胶配方制备：
BR-55                       100.00
硬脂酸                      2.00
氧化锌                      5.00
Santocure                   1.25
TMTD                        0.15
硫                          10.00
                            118.40
硫化    10分                150℃
硬度    肖氏A               66
回弹     ％                 92
再生
样品1：  纯再生高弹体BR
样品2：  再生高弹体BR       118.40
         Santocure          0.60
         TMTD               0.10
         硫                 2.00
                            121.10硫化                 10分       150℃
                 样品1      样品2硬度         肖氏A    66         68回弹         ％       70         85实施例7    由下述CSM橡胶配方制备：
HYPALON-40                         100.00
密陀僧(即氧化铅)                   20.00
炭酸镁                             20.00
碳黑N-762                          50.00
芳香油                             10.00
MBTS                               0.50
TETRONE A                          2.00
                                   202.50硫化           30分                    155℃拉伸强度       Pa(kg/cm2)              2.25×107(225)断裂时的伸长   ％                      200硬度           肖氏A                   73再生
样品1：    纯再生高弹体CMS
样品2：    再生高弹体CMS             202.50
           MBTS                      0.25
           TETRONEA                  1.00
                                     203.75硫化                        30分         155℃
         样品1          样品2        拉伸强度Pa(kg/cm2) 1.4×107(140) 1.8×107(180)断裂时的
                                     伸长％            120            100         硬度肖氏A         73             76实施例8    由下述FMK橡胶配方制配：
VITON B                            100.00
密陀僧(即氧化铅)                   15.00
炭黑MT                             30.00
Diak 3                             3.00
                                   148.00
硫化           20分                177℃
加热           24小时              260℃
拉伸强度    Pa(kg/cm2)             1.55×107(155)
断裂时的伸长    ％                 200
硬度           肖氏A               78
再生
样品1：    纯再生高弹体FMK
样品2：    再生高弹体FMK           148.00
           Diak 3                  1.5
                                   149.5硫化                       20分        177℃
                      样品1        样品2拉伸强度    Pa(kg/cm2)  8.0×107(80)  1.1×107(110)断裂时的伸长    ％         160         140硬度           肖氏A       78          82实施例9    由下述EPDM橡胶配方制备：
NITRIFLEX EP-21                     100.00
氧化锌                              5.00
硬脂酸                              2.00
炭黑N-660                           80.00
石蜡油                              10.00
MBTS                                1.50
TMTD                                0.80
DMDTC Zn                            0.80
硫                                  2.00
                                    202.10
硫化        25分                    170℃
拉伸强度    Pa(kg/cm2)              1.6×107(160.00)
300％模量   Pa(kg/cm2)              8×106(80.00)
断裂时的伸长 ％                     350.00
硬度        肖氏A                   73.00
再生
样品1：    纯再生高弹体EPDM
样品2：    再生高弹体EPDM             100.00
           MBTS                       0.70
           TMTD                       0.40
           DMDTC Zn                   0.40
           硫                         1.00
                                      102.50硫化                     25分             170℃
                     样品1            样品2拉伸强度    Pa(kg/cm2)  6×106(60.00)    1×107(100.00)30％模量    Pa(kg/cm2)  3.5×106(35.00)  6×106(60.00)断裂时的伸长    ％       340.00           300.00硬度           肖氏A     73               76.00A.从制备基本组合物开始比较各种再生方法
1.基本组合物
2.再生高弹体A-通过研磨降低颗粒尺寸，在浆料中再生，专利PI-8500981。
3.再生—使用压热器和干法精制机。
4.再生高弹体B-通过本发明所述的限制降低颗粒尺寸，在浆料中再生，。
1.基本组合物
SBR-1712                      100.00
炭黑N-220                     27.50
炭黑N-336                     20.00
Dutrex R                      4.00
氧茚树脂                      5.00
Banox H                       1.50
氧化锌                        5.00
硬脂酸                        1.00
Santocure                     1.50
DPG                           0.50
硫                            1.50
                              167.50
硫化          45分             150℃
拉伸强度    Pa(kg/cm2)    1.39×107(139.30)
300％模量   Pa(kg/cm2)    6.2×106(62.10)
断裂时的伸长   ％              540.00
硬度          肖氏A            58.00
磨损           mm3             0.26
2.再生高弹体A
      SBR-1712                 100.00
      再生高弹体A              63.20
      炭黑N-336                23.10
      炭黑N-220                32.00
氧化锌                      7.10
硬脂酸                      1.40
Dutrex R                    5.70
氧茚树脂                    7.10
Banox H                     2.20
Santocure                   2.20
DPG                         0.70
硫                          2.20
                            246.90硫化             45分            150℃拉伸强度      Pa(kg/cm2)      1.4×107(139.80)300％模量     Pa(kg/cm2)      6×106(60.60)断裂时的伸长      ％             500.00硬度             肖氏A           58.00磨损              mm3            0.293.再生—通常工业方法
SBR-1712                     100.00
再生橡胶                     63.20
炭黑N-336                    23.10
炭黑N-220                    32.00
氧化锌                       7.10
硬脂酸                       1.40
Dutrex R                     5.70
氧茚树脂                     7.10
Santocure                    2.20
硫                           2.20
                             244.00硫化           45分            150℃拉伸强度     Pa(kg/cm2)    1.18×107(118.40)300％模量    Pa(kg/cm2)    5.4×106(54.20)断裂时的伸长    ％             520.00  硬度           肖氏A           58.00磨损            mm3            0.344.再生高弹体B-A新方法
SBR-1712                  100.00
再生高弹体B               63.00
炭黑N-336                 23.10
炭黑N-220                 32.00
氧化锌                    7.10
硬脂酸                    1.40
Dutex R                   5.70
氧茚树脂                  7.10
Banox H                   2.20
Santocure                 2.20
DPG                       0.70
硫                        2.20
                          246.70硫化            45分            150℃拉伸强度      Pa(kg/cm2)    1.35×107(135.00)300％模量     Pa(kg/cm2)    6.2×106(62.00)断裂时的伸长    ％              450.00硬度           肖氏A            58.00磨损           mm3              0.30
表1各商品名的物质及其供应商和化学名称
商品名 供应商 化学名称
Butyl 268 Exxon 异丁烯-异戊二烯弹性体，门尼粘度(ml 1±8，125℃)
BanoxH Bann 1，2-二氢-2，2，4-三甲基喹啉
BLE Uniroyal 二苯胺和丙酮的高温反应物
BR-55 Coperbo 聚丁二烯弹性体，门尼粘度(ml 1±4，100℃47-57)
Diak 3 Dupont 无环胺盐
DMDTCZn Bann 二甲基二硫代氨基甲酸锌
DPG Cyanamid 对称的二苯基胍
DutrexR Shell 高度芳香油，ASTM D2226
Hycar 1042 BFGoodrich 丁二烯-丙烯腈中-高丙烯腈
Hypalon 40 Dupont 氯磺化聚乙烯，门尼粘度(ml 1±4，100℃56)
MBTS Akron 2，2’-二苯并thiasyl二硫化物
Neoprene W Dupont 聚氯丁二烯，门尼粘度(ml 1±4，100℃34-41)
Nitriflex EP-21 Petroflex 乙烯-丙烯-Dirner三聚物，门尼粘度(ml 1±4，125℃ 45)
Santocure Monsanto N-环己基-2-苯并thyasole亚磺酰胺
Tetrone A Dupont 二(五亚甲基)秋兰姆四硫化物
TETD Bann 四乙基秋兰姆四硫化物
TMTD Bann 四甲基秋兰姆二硫化物
TMTMS Henley 四甲基秋兰姆一硫化物
TTD Rialt 四甲基秋兰姆二硫化物
VitonB Dupont 氟弹性体，门尼粘度(ml-10，121℃ 74)

Claims (5)

1.一种再生硫化或半硫化橡胶的方法，使之在合适的溶剂中溶胀，其特征在于，提供溶胀的橡胶块，并限制其与或存在于有毒或脱硫化学阻份中。
2.如权利要求1所述的方法，其特征在于，限制包括一种或多种钻孔金属板，或筛网，或海绵，或多孔金属板，或任何其它的相同类型的或将它们组合起来使用的限制。
3.如权利要求1所述的方法，其特征在于，过程可使用任何类型的硫化，半硫化，熟化，半熟化橡胶组合物进行。
4.如权利要求1所述的方法，其特征在于，过程可以冷或热的方式来进行。
5.如权利要求1所述的方法，其特征在于，过程可在比常压高或低的压力下进行。
CN93112734A 1993-01-22 1993-12-31 硫化或半硫化橡胶的快速再生方法 Expired - Fee Related CN1048023C (zh)

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