• 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:
    Catalyst components which comprise the reaction product of a Ti compound and a Mg dihalide and which are in the form of spherical particles having an average diameter of 1 to 100 microns, a surface area of 300 to 500 m2/g, and a porosity of 0.3 to 0.4 cc/g are disclosed, as are catalysts also in the form of spherical particles prepared therefrom and useful in the polymerization of ethylene and of alpha-olefins CH2=CHR in which R is alkyl radical having from 1 to 6 carbon atoms, and the polymerization of the alpha-olefins therewith.
    公开号:SU1080731A3
    申请号:SU792803961
    申请日:1979-08-21
    公开日:1984-03-15
    发明作者:Феррарис Марио；Розати Франческо；Пароди Сандро；Джианетти Энзо；Мотрони Джузеппе；Альбиззати Энрико
    申请人:Монтэдисон С.П.А. (Фирма)；
    IPC主号:
    专利说明:

    vj
    The invention relates to methods for the preparation of a catalytic component for stereoregular polymerization of olefins. A known method for producing a catalytic component for the polymerization or copolymerization of olefins by co-grinding a titanium compound of the general formula MPT, ... where M is an alkali metal or NRn group, in which the quaternary nitrogen atom has valencies saturated with hydrogen atoms and / or hydrocarbon radicals R, such as al1 | yl, aryl, arylalkyl and cycloalkyl, or the indicated nitrogen atom is part of a heterocyclic ring; X. is a group HR2 in which hydrogen atoms and / or Li hydrocarbon radicals, such as alkyl, aryl, aryl alkyl and cycloalkyl, or one of the radii may be halogen, n is the valence of titanium m 1, 2 or 3, p is 0, 1, 2 or 3 with carrier — anhydrous magnesium halide having a specific surface of particles greater than 3 m / g and / or an extended glow in place of the characteristic diffraction line of its X-ray spectrum 13. The disadvantages of this method include the relatively low activity of the obtained component, which leads to a decrease in the isotactic coefficient of the polymer and the deterioration of the properties of the polymer (fluidity). The closest to the invention is a method for producing a catalytic component for stereoregular polymerization of oi-olefins by reacting titanium tetrachloride with an adduct carrier, taken in the form of spherical particles and containing magnesium chloride and an electron-donor compound, obtained by dehydration, heating it at 80 -125 ° C for 4-8 hours before the formation of MgCl4. (0.45-2) H2 in the presence of an electron-donating compound — a ketone, a simple C2 ether. The catalytic component obtained according to the indicated method is is activated by particle size uncontrollability, has a surface area of 70–150 l / 70 m / g and a pore radius of 70–150, which does not allow obtaining a polymer with good morphological characteristics, namely, the polymer obtained in the presence of a catalytic component according to this method has The relative low isotactic ratio (less than 90%), poor fluidity (s), unregulated and very scattered is the particle size of the polymer powder from less than 44 to more than 710 microns. . The purpose of the invention is to obtain a catalytic component in the form of spherical particles having an average diameter of 32-40.4 A, a surface area of 329-410 m / g and a porosity of 0.30, 4 cm / g. This goal is achieved by the fact that according to the method for producing a catalytic component for stereoregular polymerization of ot olefins by reacting four titanium chloride, in the presence of an aromatic ester, with an adduct containing magnesium chloride and an electron-donating compound, and taken as spherical particles, an adduct of MgCl-nROH is used where n is 1.5-5.0, R is C-C5f-alkyl obtained by mixing magnesium chloride with aliphatic alcohol in the presence of a dispersing liquid, such as ep, vaseline oil, silicone oil, a mixture of vaseline and silicone oils, taken in a 1: 1 volume ratio, melting the resulting adduct, emulsifying the adduct mixture and dispersing liquid in a turbulent mode, followed by cooling the M emulsion and separating solid spherical particles having an area the surface is 844 m, the porosity is 0.61 cm / g and 78-98.3% of particles with a size of 10-30 microns, and the interaction is carried out in the presence of an aromatic ester. The proposed method allows to obtain a catalytic component in the form of spherical particles having an average diameter of 32-40.4 A, area: surfaces of 329-410 and porosity of 0.3-0.4 cm / g, which allows to obtain a polymer with improved morphological characteristics, namely, the polymer obtained in the presence of the catalytic component according to the invention, has a high isotactic coefficient (more than 90%), good fluidity (less than 16 s), a spherical shape and a narrow particle size distribution (L96 wt.%) falls on particles with a size one time ka). According to the invention, the MgCl1-nROH compound of the composition, where n 1.5-5.0, R — C, —C.-alkyl is obtained by mixing magnesium chloride with an aliphatic alcohol. in the presence of dispersing liquid selected from: w9eline and silicone oils, a mixture of petroleum jelly and silicone oils, taken in a 1: 1 volume ratio, melting the resulting adduct, emulsifying the mixture of adduct and dispersing liquid in a turbulent mode, followed by cooling the emulsion. separation of solid spherical particles with the subsequent interaction of the carrier adduct with titanium tetrachloride in the presence of an aromatic ester. The reaction with the titanium compound is carried out either by adding solid adduct to the undiluted T1SC held at or by conducting the reaction in a carbon-hydrogen diluent medium at a relatively low temperature, for example, lower than 40 ° C. The solid reaction product separated from the reaction mixture is then reacted with a liquid titanium compound, preferably tetrachloride titanium, at 80-135 C. The solid reaction product is separated from the excess titanium compound at a temperature at which undesirable Titanium compounds that are extracted with TiCl4 remain dissolved in the reaction medium and are removed with it. In the case when TiCl is used as the reaction medium, the solid product is isolated at temperatures exceeding. However, it is possible to work at more low temperatures, provided that Tici is used in quantities sufficient to dissolve undesired titanium compounds. It is also convenient to repeat the treatment with TiCl either once or several times. The solid is removed from the reaction mixture and then washed with an inert hydrocarbon solvent (hexane, heptane, etc., in order to remove the last unreacted titanium compound .... The components of the catalyst according to the invention, when reacting with organometallic compounds or with a metal belonging to group II and III of the periodic system, form a catalyst that is particularly active in the polymerization of olefins. the use of these catalysts, the polymers are in the form of spherical particles with high flowability, have a flow index below 16 s, and often 12–15 s (the index is measured according to method A). The polymerization can be carried out in the liquid phase or in the presence of either in the absence of an inert hydrocarbon solvent (for example, hexane, heptane, etc.), or in the gas phase. The polymerization temperature is within 40-15ac, preferably 50-90 sec. It is even more preferable to polymerize propylene or its mixtures with minor amounts of ethylene, for example, below 25%, with stereospecific catalysts. Example 1.49 g of anhydrous lory magnesium, 78.1 g of anhydrous ethyl alcohol and 1.155 ml of liquid paraffin produced by the company Montedison spA under the brand name ROS OB / 30 are loaded in an inert gas atmosphere and at room temperature and normal pressure into a two-liter autoclave equipped with a turbine agitator and tube for unloading. The reaction mass is heated to 120 ° C with stirring and an adduct of magnesium chloride with 3 mol of ethyl alcohol is obtained, which melts and remains mixed with the dispersion (liquid paraffin). After that, the pressure in the autoclave is adjusted to 10 kg / cm by introducing an inert gas-nitrogen. The discharge tube is connected through a valve to a tube having an inner diameter of 1 mm and a length of 3 meters, the tube having an external heating and heated to 120 ° C. After that, open the faucet and let the mixture flow through the tube. The linear flow rate of the mixture in the tube is about 4.5 m / s. At the outlet of the tube, the dispersion is placed in a five-liter flask equipped with a stirrer containing 2.5 liters of anhydrous heptane, with external cooling and maintained at an initial temperature of -40 s. The final temperature after collecting the emulsion flowing from the autoclave is. The solid product consisting of spheroidal particles and forming the dispersed phase of the emulsion is separated by decanting and filtering and washed with heptane. All these operations are performed in an inert gas atmosphere. After drying, carried out in vacuum at 1 mm Hg. Art. within 3h at room temperature, obtain 102 g of a solid product in the form of spherical particles of the formula MgCl 2.77 CdNuOH, which, after sieving, gives the following results relating to particle sizes: 74-105 microns 0.4% 50-74 microns 5.5% Smaller 50 microns of 94.1% 11.7 g of the fraction of the described adduct with particles less than 50 microns are suspended in 80 ml of anhydrous H-heptane in a 500-ml tube equipped with a porous diaphragm and a stirrer. While maintaining the temperature within 200 ml, a 0.85 M solution in triethylaluminum heptane is introduced for 1 hour with stirring into the indicated tube. After that, the mixture is heated for 2 hours, then filtered and washed with five portions of n-heptane in 120 ml each at 80 ° C, and stirring is carried out for 20 minutes each time. The magnesium chloride obtained in this way, after drying at 45 ° C in vacuum, has a specific 5 surface area of 844 and a porosity of 0.61 cm / g.
    The product thus activated is suspended in 100 ml of H, -heptane, and this suspension is introduced for 1 hour and, with stirring, 7.5 ml of a heptane solution containing 1.1 g of ethyl benzoate, after which the entire mixture is heated at 80 ° C for 2 hours, filter and wash with five 15 portions of heptane, 120 ml each time with stirring for 20 minutes. Then the mixture is filtered and dried under vacuum.
    80 ml of TiCl are then added to magnesium chloride with stirring and the mixture is heated at 2 hours. The product is filtered off and the solid 25 U product is processed again with a further 100 ml of TiCl at 2 hours.
    The resulting mass is filtered, cooled before and washed with several portions of heptane, 120 ml at 30–80, s, until the complete disappearance of chloride ions in the filtrate is reached. This product was dried in vacuo at and 6.8 g of a solid catalytic component were obtained, containing 35% of 1.64% by weight of titanium and 7.3% by weight of ethyl benzoate having the following characteristics: porosity 0.391, specific surface area 393 m / g , the average radius of pores 20 Ya.40
    The solid catalytic component obtained in this way is used in the polymerization of propylene in a suspension of 5 mmol of a heptane solution of a trialkylaluminum mixture with composition d, a gas after hydrolysis,% by volume ethane 9, isobutane 49.4, H - butane 41.2, propane 0.16, isobutane 0.24, is reacted at room temperature with i 1.25 mmol of methyl para toluate diluted in 80 ml of anhydrous and desulfurized H-heptane for 5 min. 50 ml of the solution is brought into contact with 61 mg of the prepared catalytic component s in accordance with the described system. The residual milliliters-55 s are diluted with n-heptane, up to 100 ml are introduced into a 3000 tal autoclave equipped with an agitator core mixer and equipped with a thermometer, with a temperature control of 60 s at 50 s, and gaseous propylene is introduced into the laboratory.
    In the same way, the suspension of the catalytic component is introduced. Pose sealing autoclave into it- 65
    hydrogen is given until the partial pressure reaches 0.3 atm, after which the suspension is heated up with the simultaneous introduction of propylene until the total pressure reaches 7 atm. The specified pressure is kept constant throughout the polymerization process while the monomer is continuously being fed. After 4 h of polymerization. The interruption is interrupted. 220 g of polypropylene is obtained, which is isolated for processing with methanol and acetone.
    The polymerization results are shown in the table.
    Example 2.28.4 g of anhydrous magnesium chloride, 49.5 g of anhydrous kantol, 100 Mft of vaseline oil ROL OB / 30 and 100 ml of organosilicon oil (viscosity 350 cSt) are introduced in an inert gas atmosphere into a flask immersed in a bath with thermal stabilization with, when re-grinding to achieve complete dissolution of magnesium chloride.
    This forms an adduct of magnesium chloride with ethanol mixed with oil. The hot mixture is transferred under an inertial atmosphere into a 1500 ml capacity, sleep: Essenne heating jacket and containing 150 ml of razelin oil and 150 ml of organosilicon oil "The resulting mixture is kept under stirring under the action of an Ultra-Turrax T-45N agitator manufactured by Yaki End Kunkel KG Ika-Verke.
    The mixture is stirred for 3 minutes at a speed of 10,000 rpm and discharged into a two-liter container containing 100 ml of anhydrous m-heptane, which is held under stirring and cooling so that the final temperature does not exceed. MgCl2 microspheres obtained in this way
     after filtration, drying is carried out in vacuum at room temperature and subjected to sieve analysis, as a result of which a fraction with a particle size of less than 50 microns is obtained, the content of which is 78 wt.%. When activating
    According to Example 1, these microspheres form a solid catalytic component containing 1.95 wt.% titanium and 7.5 wt.% ethyl benzoate and having the following characteristics: porosity of 0.322 cm / g specific surface area 397 average pore radius 16 A.
    46.3 mg of this catalytic component is used in the polymerization of propylene under the conditions of Example 1. This gives 170 g of polypropylene. The results are shown in the table.
    Example 3. 25.25 g of MgCl2 "2.77 in the form of microspheres with a particle size below 50 microns obtained under the conditions of Example 1 are suspended in 150 ml of anhydrous i-heptane in a 500 ml Kelbe equipped with a stirrer and immersed in a stabilized bath heating maintained at. In this suspension, 21.6 ml of a 1 M solution of ethyl benzoate in heptane is dissolved and the mixture is allowed to react under stirring for 10 minutes. To the suspension, which has a temperature of 100 ml, undiluted titanium tetrachloride is added. The thermally controlled bath is removed and the suspension is heated to room temperature for 1 hour, then 150 ml of titanium tetrachloride are added and the mixture is again heated to. Thereafter, the suspensions are allowed to react for 2 hours at, then they are filtered and introduced into reaction with 200 ml of miscellaneous titanium tetrachloride in the absence of a solvent, with stirring for 2 hours at. The titanium tetrachloride is removed, the solid product is cooled to 80 ° C and then it is washed with -heptane until the chloride ions are completely removed from the filtrate, and the solid product is dried under vacuum at. The solid catalysis component obtained in this way contains 3.4% by weight of titanium and 11.5% by weight of ethylbenzotat and exhibits the following characteristics: porosity 0.30 specific surface area 372 average porous pore 1 b, 2 A. 40 mg of the catalytic component in suspension in heptane is used to polymerize propylene under the conditions of example T. This gives 225 g of polymer. The results are given in the table. Example 4. 9g MgCl, h 2.77 in the form of microspheres with a diameter of less than 50 microns, obtained under the conditions of Example 1, are introduced into a flask with a volume of 560 m under nitrogen. After that, the product is kept at a stabilized temperature; the lysed temperature is maintained and the flask is connected to a vacuum source to reduce the content of ethyl alcohol in the spheroidal adduct from 2.71. up to 2 mole. The product is suspended in 150 ml of anhydrous m-heptane, followed by treatment with a titanium compound under the conditions of Example 3, with the exception that instead of 21.6 ml only 7.5 ml of heptane 1M ethyl benzoate solution is used. A solid catalytic compound is obtained, having 1.96% by weight of titanium, 9.05% by weight of ethyl benzoate and. The following characteristics - porosity of 0.39 specific surface area: 386 average pore radius: 20.2 I. 43 g of this catalytic component in suspension in heptane is used for the polymerization of propylene in the conditions of example 1. This gives 182 g of propylene. Results are shown in the table.
    Characteristic viscosity is determined in tetralin at 135 C.
    “,
    Example 5. 12 g of MgCl2,77 in the form of microspheres with a diameter of less than 50 microns, obtained under the conditions of example 1, are suspended in 100 ml of anhydrous n-heptane in a 50 ml test tube equipped with a porous diaphragm and a stirrer. While maintaining the temperature at the level, 1QO ml of titanium tetrachloride is added dropwise to this suspension. Then the temperature is raised to
    and the mass is allowed to react for 2 hours. After filtration with the solid, it is again suspended in 200 ml of titanium tetrachloride. The resulting suspension is maintained at 130 ° C for 2 hours with stirring, then filtered again and the solid is cooled down and re-washed at 80 ° C in portions of n-heptane until chloride ions disappear in the filtrate. After drying, the solid catalytic component contains 7.4% by weight of titanium and 6.32% by weight of chlorine.
    8 g of a solid catalytic component prepared in this way (corresponds to 0.6 mg of titanium) and 1000 ml of anhydrous H-heptane are introduced (together with 2 ml of triisobutylaluminum or under nitrogen) in an autoclave with a volume of 3 liters made of stainless steel equipped with a root stirrer and a device to stabilize the temperature at 85 ° C, then hydrogen is added to a pressure of 4 atm and ethylene to a total pressure of 13 atm, which is kept constant throughout the test time, with the introduction of monomer.
    After 4 h, the polymerization process is interrupted and 360 g of microspheroidal polyethylene is obtained, which corresponds to a yield of 1.340000 g of polyethylene per g of titanium; intrinsic viscosity. hchz 2.12 dl / g.
    Example 6. A 1000 ml wheel is placed with 229 ml of titanium tetrachloride, which is allowed to react with 2.42 ml of ethyl benzoate at 15 ° C for 10 minutes. At the same temperature for 50 minutes, a suspension containing 17.6 g of MgCL22.47 in 25 ml of n-heptane in the form of microspheres with a particle size of less than 50 microns, prepared under the conditions of Example 1, is introduced dropwise into this reaction mass.
    After the addition is complete, the temperature is increased to 100 s, and the pea is completed after 90 minutes. The reaction product is then filtered through a porous diaphragm at the reaction temperature. 100 ml of undiluted titanium tetrachloride are added to the filtrate, after which the reaction takes place another 2 hours at 120 ° C.
    The resulting product is filtered. the solid is cooled to 80 ° C and washed with c-heptane at 80 ° C until the chloride ions disappear in the filtrate. The solid, dried by vacuum drying, contains 3.26% of titanium and 9.64% by weight. % ethyl benzoate.
    The results of the experiment on the polymerization of propylene under the conditions of example 1 are given in the table.
    Example 7. Into a 1000 ml flask, 437 ml of titanium tetrachloride were introduced and cooled to 0 ° C. At this temperature, 16.90 g of MgCl2-2.44 CjHjOH (in the form of miSurospheres with a particle size corresponding to a diameter less than 50 microns, obtained under the conditions of example C /, and 16/3 ml of a 1M heptane solution of ethyl benzoate. The mixture is allowed to react 60 hn, slowly bringing the temperature to, and for 50 min the reaction mass is heated to 100 ° C. With
    This temperature continues to lead the reaction for 90 minutes.
    The reaction product is then filtered through a porous diaphragm, 200 ml of undiluted four L-titanium are added, and the reaction takes 2 more hours.
    At the end of the reaction, the product is filtered off, cooled to and washed with I-heptane at 80 ° C until the chloride ions disappear from the filtrate. The solid product, isolated by drying in vacuum, contains 3.43% by weight of titanium and 9.50% by weight of ethyl benzoate.
    The results of the experiment on the polymerization of propylene under the conditions of example 1 are placed in the table.
    Example 8. 14 g x1.9. С2Н50Н-0.8 In the form of microspheres with a diameter of less than 50 microns, obtained in example 1, is used to synthesize a solid catalytic component according to the method described in example 1. The solid solid product contains 2.93 weight % titanium and 9.27 wt.% ethyl benzoate.
    The results of the polymerization of propylene under the conditions of example 1 are placed in the table.
    , Example 9. Example 3 is repeated, except that when preparing the catalytic component with 20 ml of a 1 M heptane solution of methyl p-toluic acid ether, instead of 21.6 ml of a 1 M heptane solution of ethyl benzoate is used. The solid catalyst component contains 3.4 wt.% Ti and 11.2 wt.% Methyl para-toluic acid ester, and also has a porosity of 0.35 specific surface of 390 MVr.
    40 mg of the catalytic component thus obtained is then subjected to polymerization in a heptane propylene suspension in accordance with the method of Example 1.
    253 g of polypropylene are obtained, with the following properties:
    Yield, g of polymer / g Ti 188000 Isotactic coefficient 91, 8 t1J Internal viscosity, n (intrinsic), dl / g 1.9 Bulk weight, g / cm 0.43 Flowability, s14.5 Particle size distribution, wt.% : 44 / i.o 44-102 | M.0.3 102-71 Oja 96.5 710./U.3.2 Example 10. Example 9 is repeated, except that when preparing the catalytic component 20 ml of 1 M of heptane solution of ethyl ester of anisic acid is used instead of 20 ml of 1 M solution of methane
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING A CATALYTIC COMPONENT FOR STEREO REGULAR POLYMERIZATION OF ci-OLEPHINS by reacting titanium tetrachloride with an adduct carrier containing magnesium chloride and an electron-donating compound and taken in the form of spherical particles, which differs in that, in order to obtain 0 having an average diameter of 32-40.4 A, a surface area of 329-410 m 2 / g and a porosity of 0.3-0.4 cm 3 / g, an adduct of the composition MgCl ^ -nROH is used, where η = 1.5- 5.0, R - C γ-C ^ -alkyl obtained by mixing magnesium chloride I am with aliphatic alcohol'C 2 -c * in the presence of a dispersing liquid, which is used, for example, liquid paraffin, silicone oil, a mixture of liquid paraffin silicone oil taken in a 1: 1 volume ratio, melting the adduct obtained, emulsifying the mixture § adduct and dispersing fluid ~ in a turbulent mode with subsequent cooling of the emulsion and separation of solid spherical particles having a surface area of 844 m 2 / g, porosity of 0.61 cm 3 / g and 78-98.3% of particles with a size of 10-30 microns, and interaction lead in the presence of aromatic acid ester.
    SU m JC080731 or copolymerization of olefins in joint grinding of titanium compounds of the general formula MPT ^ X ^. ^, M is an alkali metal or group
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    同族专利:
    公开号 | 公开日
    AU5005479A|1980-02-28|
    FR2434180A1|1980-03-21|
    BE878347A|1980-02-21|
    JPH0327566B2|1991-04-16|
    ATA560979A|1980-11-15|
    SE446402B|1986-09-08|
    FI67867C|1985-06-10|
    NO792683L|1980-02-25|
    NO158102C|1988-07-13|
    DK158360B|1990-05-07|
    DK158360C|1990-10-01|
    FR2434180B1|1985-03-29|
    GB2029840A|1980-03-26|
    PH16241A|1983-08-11|
    AT362934B|1981-06-25|
    BR7905362A|1980-05-27|
    PT70081A|1979-09-01|
    IN152966B|1984-05-12|
    DE2933997C2|1993-04-01|
    MX152392A|1985-07-10|
    NO158102B|1988-04-05|
    CA1137069A|1982-12-07|
    IT7826908D0|1978-08-22|
    GB2029840B|1983-05-18|
    NL190331B|1993-08-16|
    SG44583G|1984-07-27|
    DE2933997A1|1980-03-06|
    NL7906259A|1980-02-26|
    DK343079A|1980-02-23|
    US4399054A|1983-08-16|
    JPS5529591A|1980-03-01|
    FI67867B|1985-02-28|
    NL190331C|1994-01-17|
    AR221246A1|1981-01-15|
    SE7906869L|1980-02-23|
    AU530535B2|1983-07-21|
    GR73629B|1984-03-26|
    ZA794332B|1980-08-27|
    ES483523A1|1980-04-16|
    IT1098272B|1985-09-07|
    CH644136A5|1984-07-13|
    FI792547A|1980-02-23|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    IT26908/78A|IT1098272B|1978-08-22|1978-08-22|COMPONENTS, CATALYSTS AND CATALYSTS FOR THE POLYMERIZATION OF ALPHA-OLEFINS|
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