• 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 granulate organosilane preparation is made consisting essentially of (a) 30 to 60 weight percent of at least one organosilane of the formula <IMAGE> (I) where R1 is an alkyl group with 1 to 3 carbon atoms, R2 is an alkyl or alkoxy group with 1 to 3 carbon atoms, R is an alkylene group with 1 to 5 carbon atoms and x has a value from 2.0 to 6.0, and (b) 70 to 40 weight percent of carbon black.
    公开号:SU795495A3
    申请号:SU782562403
    申请日:1978-01-05
    公开日:1981-01-07
    发明作者:Вольфф Зигфрид；Ротбюр Лотар
    申请人:Дегусса (Фирма)；
    IPC主号:
    专利说明:

    54) GRANULATED ORGANORPRESSOR COMPOSITION
    This invention relates to the rubber industry, in particular to a granular silicone composition. A granular silicone composition for rubber mixtures is known that contains a silicone compound (silane) and an inorganic powdery substance — silicic acid 1. However, the known composition has a low storage stability. The purpose of the invention is to increase the storage stability of the composition. This goal is achieved by the fact that, in a granulated creme, an organic compound for rubber compounds containing a silicone compound and an inorganic powdery substance, it contains as a silicone compound compounds of the general formula 1 0. / B0- $ iB - $, - B-Si where R is monovalent alkyl group. R is a monovalent alkyl or alkoxy group C -; - Cz; R is a divalent alkyl group C —Cy; X 2.0-6.0.5 as an inorganic particulate soot substance with a weight ratio of 30:70 to 60:40, respectively. Preferably, according to the invention, organosilicon compounds are used in which R is an alkoxy group. These organosilicon compounds with three alkoxy groups at each silicon atom, which also contain one divalent alkyl group (R) with two four carbon atoms and two four sulfur atoms (x). In particular, according to the invention, a product produced on an industrial scale, bis- (3-triethoxysalylpropyl) tetrasulfide, is well suited. Mixtures of several organosilicon compounds can also be used to prepare the preparations. Moreover, several means in this case, in particular, 2.3 or 4. Particularly preferred organosilicon preparations offered
    invention, consisting of 45 57 silicone compound of the formula
     . (C2HjO) 2 -S i-R -Sx -R --Si () где where R is a bivalent alkyl group.; х is a number equal to 2.0-4, О, and -55-43 wt.% of carbon black NAG with the following indicators: Brunauer Emmett and Teller surface 78 + 3 m / g. The average value of the primary particles (arithmetic average) J2 / + 2 them, pH 9 + 1.
    Absorption of dibutyl phthalate 100 + +. 5 ml / 100 g
    To obtain the organosilicon compositions, known soot species are used. Preferably, so-called furnace soot is used, including HAF-type rage. The designation HAP is a known abbreviation for High Abrasion Furnace (high abrasive kiln) rubber technology. Particularly suitable for use with carbon blacks are the varieties of powdered soot from commercial, Printex - carbon black from the DeGuss company with a Brunauer, Emmet and Teller surface within the order of 30-140 m / g and the average (arithmetic magnitude) value of the primary particles within about 20-60 nm. For: the preparation of the silane preparations according to the invention, mixtures of different types of carbon black may be used, for example a mixture of Printer, 60 and Printex 300 or a mixture of P.rintex 30 and Printex 300.
    To obtain new compositions, the starting materials are placed in appropriate devices and mixed. If these weight ratios are observed, neither the powder nor the paste is formed, but granules are obtained in the form of grains or beads.
    Devices that can be used to make the compositions are known mixers for powders such as a mixing chamber of a rubber mixer (trough) with a rotating propeller agitator. Such mixtures-. So far, the bodies have been used to mix blemishes of polymeric materials and to obtain dry blends of polyvinyl chloride. With typically spinning speeds of the order of 3003,000 rpm, granular formulations are prepared within a few seconds, for example, about 10-13 seconds.
    The invention is illustrated by the following examples.
    Example 1. Printex 30 is used as carbon black with the following parameters: Brunauer, Emmett, and Teller 78 surface. The average size of the primary particles. (arithmetic mean) 27 nm; pH value 9; dibutyl phthalate absorption (reduced abs - BDF, ASTM D 2414) 100 ml / 100 g
    In a trough-shaped powder mixer with a 150-liter propeller mixer, 10 kg of Printex 30 furnace soot are weighed, then added. 10 kg of bis- (3-triethoxysilylpropyl) tetrasulfide (abbreviated as Si 69) are added and both products are mixed and homogenized for 25 s at 360 rpm. After opening the unloading lug pour 20 kg of granules with particles of about 0.8 mm. No granules. are hot, do not stick together and have good flowability.
    Example 2. Silicone composition is produced in a continuous manner. For its implementation using a bead machine. According to 80 kg / h of Printex 30 and 80 kg / h of Si 69, 160 kg / h of practically non-dusty granulate in the form of beads are obtained.
    Example 3 To obtain the silane compositions according to the invention, carbon black and S i 69 are used in the amounts indicated in Table. 1. Table 1
    The compositions are prepared as in Example 1. The resulting silane compositions possess optimal properties of the granules,. the shape of beads with particles of an average size of 0.8-1.0 and abrasion of beads of 0.5-2%. (Dean 53583).
    Example 4 According to example 1, receive the following formulations:
    100 g of Printex 30 and 200 g of silane 1: СНзО) s Si (СН2) s SS- (CH.j) 3 Si (OCHg) 200 g of Printex 30 and 200 g of silane (CHjO)} Si (CH) jSSS- (CHi ) 3Si (OSSN) s 200 g Printex 30 and 200 g of silane
    (c.) j.siicw2 -:. § r o-ssnrz
    In each case, the mixture is homogenized in a 7-liter trough-type mixer. Stirring time 10 seconds at a speed of 1400 / min. A non-friable, free-flowing, well-processed granulate is obtained.
    权利要求:
    Claims (3)
    [1]
    Example 5: To test storage stability and determine efficacy, depending on the duration of storage, a known powder mixture of 50% by weight of siliconic acid Ultras was introduced into the rubber mixture based on styrene-butadiene rubber (SBR 1500); VNjH 50 is the weight of bis- (3-triethoxysilylpropyl) tetrasulfide, on the one hand, and proposed by the invention, a rotten non-dusting composition of 50 wt.% Printex 30 carbon black and 50 wt.% Bis- (3-triethoxysilylpropyl) tetrasulfide, the other side. The rubber mixtures have the following composition, parts by weight: Styrene-butadiene rubber (SBR 1500) 100 Silicic acid — filler (Ultrasil VNj) 35 Silicone composition or mixture indicated in this example10 Zinc oxide3 Stearic acid 2 Sulfur2 Sulfenamide accelerator1 These mixtures are tested at temperature 155 ° C in the Monsant rheometer with amplitude of 3 and 3 cycles. The following values are measured: DOO is the maximum torque; Off — the minimum torque D, Dq — moment exerting due to stitching (the final stitching value); ti is the incubation period; K is the crosslinking rate constant for the first order time law; 1.5-0 is the time to crosslink 5% of the total crosslinking amount; 95% crosslinking time 95% of total crosslinking. The test results for the use of granular non-dusty composition: 50 wt.% Printex 30 carbon black and 50 wt.% Bis- (3-triethoxysilylpropyl) tetrasulfide (suggested composition), are given in Table.
    [2]
    2. Table 2 D, kgcm 0, kgf, m, k, / -10, min. Continued table. 2 The test results when using a powder mixture: 50% by weight of filler — silicic acid and 50% by weight of bis- (3-triethoxysilylpropyl) tetrasulphide (silane) (for comparison, the known composition) is given in the table.
    [3]
    3. Table 3 As can be seen from Table 2 and 3, after storage for 1 year, the granular non-dusting composition of 50 wt.% Printex 30 carbon black and 50 wt.% Bis- (3-triethoxysilylpropyl) tetrasulfide does not undergo any noticeable changes in the tested mixtures, i.e. possesses good storage stability. Powdered mixture of silicic acid - filler. and silane is characterized by a significant decrease in the final amount of crosslinking () and a decrease in the rate constants of the crosslinking reaction Q%, which means the vulcanization rate is almost doubled (t 95%). Claims of the Invention: Granulated Silicone Compound for Rubber Compounds. containing organosilicon compound and inorganic powder, which is similar to the fact that, in order to increase the stability during storage of the composition, the latter contains a compound of the general formula as a silicon organic compound. Oi-p-Rp-xSi-R-S-R R is a monovalent C-C alkyl group; 58. R2 is monovalent alkyl or. alkoxy group C-C j; R is a divalent alkyl group Su-Cd; X 2.0-6.0. and as an inorganic powdery substance - soot with a weight ratio of, respectively, 30: 70-60: 40. Sources of information taken into account in the examination 1. US Patent No. 3997356, cl. 106-288, publ. 1976.
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    同族专利:
    公开号 | 公开日
    DE2747277C2|1982-06-09|
    AU512265B2|1980-10-02|
    BR7801477A|1979-05-22|
    FR2406651A1|1979-05-18|
    MY8500419A|1985-12-31|
    GB1588060A|1981-04-15|
    CA1099855A|1981-04-28|
    NL7803190A|1979-04-24|
    DD133961A5|1979-01-31|
    NL186254C|1990-10-16|
    IT7848056D0|1978-02-15|
    JPS5468860A|1979-06-02|
    DE2747277A1|1979-04-26|
    JPS6131137B2|1986-07-18|
    SG5084G|1985-02-01|
    US4128438A|1978-12-05|
    CS204038B2|1981-03-31|
    IT1155825B|1987-01-28|
    AU3222578A|1979-07-12|
    NL186254B|1990-05-16|
    BE862381A|1978-06-27|
    FR2406651B1|1981-05-29|
    引用文献:
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    US4005170A|1973-09-14|1977-01-25|Cabot Corporation|Preparation of pelletized carbon blacks|
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    DE2536674C3|1975-08-18|1979-09-27|Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler, 6000 Frankfurt|Crosslinkable mixtures based on rubber, organosilanes and silicate fillers|DE2933346C2|1979-08-17|1982-07-01|Degussa Ag, 6000 Frankfurt|Silane / filler preparations, processes for their production and application of the same|
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    DE4119959A1|1991-06-18|1992-12-24|Degussa|METHOD FOR PRODUCING VULCANIZABLE, RUSSELED PLASTIC AND RUBBER MIXTURES|
    IT1256263B|1992-12-30|1995-11-29|Bayer Italia Spa|GRANULATES OF SLIDING DYES, CHEMICALLY RESISTANT, THEIR PREPARATION AND THEIR USE|
    US5653875A|1994-02-04|1997-08-05|Supelco, Inc.|Nucleophilic bodies bonded to siloxane and use thereof for separations from sample matrices|
    US5494955A|1994-04-08|1996-02-27|Columbian Chemicals Company|Use of silane coupling agent with carbon black to enhance the balance of reinforcement properties of rubber compounds|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2747277A|DE2747277C2|1977-10-21|1977-10-21|Granular organosilane preparation, its manufacture and use|
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