1.
    发明专利
    未知

    公开(公告)号:DE1807493A1

    公开(公告)日:1970-06-11

    申请号:DE1807493

    申请日:1968-11-07

    Applicant: BASF AG

    Abstract: 1278649 Polymerizing ethylene BADISCHE ANILIN- & SODA-FABRIK AG 6 Nov 1969 [7 Nov 1968] 54426/69 Heading C3P Ethylene homopolymers are prepared by continuous polymerization of ethylene in the presence of organic peroxide initiator and a polymerization modifier at 280‹ to 340‹ C. and 1500 to 4000 atmospheres in a tubular reactor having two successive reaction zones of about equal length, a mixture of ethylene, peroxide and modifier being introduced at the beginning of each stage, wherein (1) a mixture of ethylene, 1 to 5 mole p.p.m. of an organic hydroperoxide having a half value temperature in the range 200‹ to 260‹ C. and 1À2 to 1À7 parts by weight per 100 ethylene of a modifier having a C s value of 2À0 Î 10 -2 to 1À0 Î 10 -4 is introduced at 170‹ to 220‹ C. to the beginning of the first zone in which the reaction temperature is kept in the range 310‹ to 340‹ C., and (2) a mixture of ethylene, 5 to 20 mole p.p.m. of an organic peroxy compound having a half value temperature in the range 150‹ to 195‹ C. and 1À2 to 1À7 parts by weight per 100 ethylene of a modifier having a C s value in the above range is introduced at 160‹ to 190‹ C. to the beginning of the second zone in which the reaction temperature is kept in the range 280‹ to 300‹ C., the half value temperatures of said hydroperoxide and peroxy compound differing by at least 20‹ C. and the weight ratio of the mixtures introduced per unit time being in the range 1 : 2 to 2 : 1. Specified hydroperoxides are p-menthane, cumene and diisopropylbenzene monohydroperoxide, and 2- hydroperoxy - 2 - (isopropylphenyl) propanes and mixtures thereof. Specified peroxides are di-t-butyl peroxide, t-butyl peracetate, t-butyl perbenzoate and methyl ethyl ketone peroxide. Specified modifiers are propylene, propane, methane and cyclohexane. The products have a broad molecular weight distribution free from very high molecular weight constituents, and are useful for making laminating films and for coating paper and fabrics.

    2.
    发明专利
    未知

    公开(公告)号:DE1901264A1

    公开(公告)日:1970-04-16

    申请号:DE1901264

    申请日:1969-01-11

    Applicant: BASF AG

    Abstract: 1,268,415. Granular polymers of propylene. BADISCHE ANILIN- & SODA-FABRIK A.G. 11 Aug., 1969 [12 Aug., 1968], No. 40067/69. Heading C3P. Easily processable granules of propylene polymer are prepared by (1) polymerizing propylene by means of a Ziegler-Natta catalyst containing titanium, in the absence of solvents or diluents so that the propylene polymer immediately obtained is in the form of a powder which contains 5-30 p.p.m. by weight of titanium, has a fraction of 10-35% by weight which is soluble in boiling n-heptane and which has an intrinsic viscosity of 6 to 10; (2) exposing the polymer, without deactivation of the catalyst, to a shear velocity of 20-1000 sec. -1 at 250-350‹ C. until the intrinsic viscosity is 1.5 to 4.0 and (3) homogenizing, extruding and granulating the so treated polymer by conventional techniques. In the example, propylene is polymerized using TiCl 3 . 1 / 3 AlCl 3 and Al(C 2 H 5 ) 3 to give a polymer of particle size 0.3 3 to 2.5 mm., containing 15 p.p.m. by weight of titanium, having a fraction of 27.5% which is soluble in boiling n-heptane and having an intrinsic viscosity of 7.8. 100 parts of the polymer are mixed with 0.2 parts by weight of the stearic ester of 2,6-ditert-butyl-4-methyl-6- #-hydroxyethyl phenol and 0.2 parts by weight of potassium stearate and subjected to a shear velocity of 400 sec. -1 and homogenized, extruded and granulated at temperatures between 250‹ and 300‹ C.

    Continuous production of ethylene co polymers

    公开(公告)号:DE1809045A1

    公开(公告)日:1970-06-18

    申请号:DE1809045

    申请日:1968-11-15

    Applicant: BASF AG

    Abstract: The improvement is obtained by using a polymerisation regulator of relatively high Cs no. (1.75 x 10-2 - 4 x 10-1), close control of the addition of vinyl ester and polymerisation initiator. The method is suitable for co-polymerisation of mixtures of 100 ppw. ethylene with 0.1 - 5.5 ppw. of a vinyl ester of a C2-C20 carboxylic acid at 150 - 350 degrees C and 1,500 - 4000 atmos. The reaction takes place in 2 steps. 1st step: 100 ppw. ethylene +0.1 - 2.5 ppw. vinyl ester +2-100 mol-ppm of a free-radical polymerisation initiator +0.01 - 1 ppw regulator. 2nd. step: 1.1 - 2 times the quantity of vinyl ester per 100 ppw ethylene +2-100 mol-ppm initiator +40 - 60% by wt. of the regulator used in the 1st. step.

    7.
    发明专利
    未知

    公开(公告)号:DE1908962A1

    公开(公告)日:1970-09-03

    申请号:DE1908962

    申请日:1969-02-22

    Applicant: BASF AG

    Abstract: 1292931 Polymerizing ethylene BADISCHE ANILIN- & SODA-FABRIK AG 20 Feb 1970 [22 Feb 1969] 8189/70 Addition to 1278649 Heading C3P A process for the continuous production of polyethylene of density 0À922 to 0À926 g./c.c. by polymerization at 280‹ to 320‹ C. and 1500 to 4000 atmospheres in a tubular reactor having two successive zones of about equal length comprises (1) introducing at the beginning of the first zone at 170‹ to 200‹ C. and 1500 to 4000 atmospheres a mixture of 100 parts by weight of ethylene, 5 to 100 mole p.p.m. of oxygen, 0À1 to 1À0 part by weight of a polymerization modifier having a Cs value of 1À5 Î 10 -2 to 1À0 Î 10 -4 and 0À1 to 0À7 part by weight of a polymerization modifier having a Cs value of 2À5 Î 10 -2 to 4 Î 10 -1 , and keeping the reaction temperature in the first zone at 300‹ to 320‹ C., and (2) introducing at the beginning of the second zone at 160‹ to 190‹ C. and 1500 to 4000 atmospheres a mixture of 100 parts by weight of ethylene, 3 to 20 mole p.p.m. of an organic peroxide having a half value temperature of 150‹ to 195‹ C., 0À1 to 1À0 part by weight of a modifier of Cs value 1À5 x 10 -2 to 1À0 Î 10 -4 and 40 to 60 weight per cent of the amount used in the first zone of a modifier having a Cs value of 2À5 Î 10 -2 to 4 Î 10 -1 , and keeping the reaction temperature in the second zone at 280‹ to 305‹ C., the weight ratio of mixtures introduced per unit time into the first and second zones being 1 : 2 to 2 : 1. Specified organic peroxides are t-butyl peracetate, t-butylperbenzoate, di-tbutyl peroxide and methyl ethyl ketone. Specified low Cs value modifiers are methane, propane, propylene and cyclohexane, and high Cs value modifiers are n-butyraldehyde, cyclohexanone, propionaldehyde and methyl ethyl ketone. The products have wide molecular weight distributions and may be used for laminating films and coatings.

    8.
    发明专利
    未知

    公开(公告)号:DE1904739A1

    公开(公告)日:1970-08-20

    申请号:DE1904739

    申请日:1969-01-31

    Applicant: BASF AG

    Abstract: 1287036 Shearing polyethylene BADISCHE ANILIN- & SODA-FABRIK AG 30 Jan 1970 [31 Jan 1969] 4548/70 Heading C3P Molten high pressure polyethylene is subjected to shearing in a shearing unit at a temperature of 200‹ to 300‹ C. and a viscosity of 5 Î 10 3 to 1 Î 10 5 poises in the absence of atmospheric oxygen, wherein the shearing surfaces contacting the polyethylene melt are at a temperature at least equal to that of the polyethylene melt entering the shearing unit and shearing is effected with such speed that the product of shearing speed and residence time is 5 x 10 2 to 5 x 10 4 . The unit may be a screw extruder. The polymer may contain 0À01 to 0À5 weight per cent of residual ethylene which may react with radicals formed in the shearing zone. The products may be made into films.

    10.
    发明专利
    未知

    公开(公告)号:DE1908964A1

    公开(公告)日:1970-09-10

    申请号:DE1908964

    申请日:1969-02-22

    Applicant: BASF AG

    Abstract: 1289618 Polymerizing ethylene BADISCHE ANILIN & SODA-FABRIK AG 20 Feb 1970 [22 Feb 1969] 8187/70 Heading C3P A continuous process for polymerizing ethylene at 250‹ to 340‹ C. and 1500 to 4000 atmospheres in a tubular reactor having two successive zones of about equal length comprises (1) introducing at the beginning of the first zone at 185‹ to 220‹ C. and 1500 to 4000 atmospheres a mixture of ethylene, 1 to 5 mole parts per million of an organic hydroperoxide having a half value temperature within the range 200‹ to 260‹ C. and 0À3 to 0À7 parts by weight per 100 parts of ethylene of a polymerization modifier having a C s value of 1À0 x 10 -2 to 4À0 x 10 -1 , and keeping the reaction temperature in the first zone at 305‹ to 340‹ C., and (2) introducing at the beginning of the second zone at 140‹ to 210‹ C. and 1500 to 4000 atmospheres a mixture of ethylene, 5 to 100 mole parts per million of oxygen and from 40 to 60 weight per cent of the amount used in the first zone per 100 parts of ethylene of a modifier having a C s value in the same range, and keeping the reaction temperature in the second zone at 250‹ to 305‹ C., provided that the weight ratio of the mixtures introduced into the first and second zones per unit time is in the range 1 : 2 to 2 : 1. Specified hydroperoxides are p-menthane, cumene and diisopropylbenzene hydroperoxides and 2-hydroperoxy-isopropylphenyl propanes. Specified modifiers are acetone, n-butyraldehyde, cyclohexanone, propionaldehyde and methyl ethylketone. The products have narrow molecular weight distributions and may be used for making films.

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