 Method of producing polypropylene
专利摘要:
Catalysts for the polymerization of alpha-olefins which comprise the reaction product of: a) an Al-alkyl compound; b) a silicon compound containing at least one Si-OR or Si-OCOR or Si-NR2 bond, R being a hydrocarbyl radical; c) a solid comprising as essential support, a Mg dihalide in active form and supported therein a Ti halide or a halo-Ti-alcoholate and a particular type of electron donor compound. 公开号:SU1457813A3 申请号:SU813389099 申请日:1981-08-07 公开日:1989-02-07 发明作者:Пароди Сандро；Ноччи Роберто；Джьяннини Умберто；Барбе Энрико；Сната Умберто 申请人:Монтэдисон С П.А. (Фирма)； IPC主号:
专利说明:
dt is propylene. The solid catalytic component is prepared as follows: 26.43 g of ethyl alcohol at room temperature is added dropwise under nitrogen to 25 g of anhydrous MgClj (water content less than 0.5%, oi.-crystalline structure, crystal diameter 380 A) weighted in 300 cm of technical n-gentan. The temperature is brought to 80 ° C and the reaction is continued for 1 hour. Finally, the solvent is removed by distillation at 50 ° C and reduced pressure by the scientific research institute, resulting in 50 g of solid product. 25 g of solid product is processed by stirring during with 21.0 cm of TiCl2 at 2 hours and while stirring, 51 cm of heptane are added dropwise to the suspension. After 15 minutes of stirring, the mixture is repeatedly washed, and the washing is carried out each time in 130 cm of heptane, four times at 80 ° C and the remaining times at room temperature, until the traces of TiCl disappear and after that they are dried at 50 ° C under vacuum. The catalyst component thus obtained shows the X-ray spectrum of the powdered product, in which the actual diffraction line found in the spectrum of MgCl1, having a specific surface area of 1, has a relatively low brightness and broadening to form a halo. Then hydrogen at a pressure of 0.2 atm is supplied, the entire reaction mixture is quickly heated to 70 ° C, at the same time additionally feeding from propylene to a total pressure of 7 atm. This pressure is kept constant throughout the entire polymerization time by feeding the monomer. After 4 hours, the polymerization is stopped, the polymer is recovered by filtration, then it is dried. The entire amount of polymer dissolved in the filtrate is recovered, weighed, and added to the polymer soluble in boiling n-heptane to calculate the isotacticity index (.1.1). Example 2. The process is carried out analogously to example 1, but using the solid component of catalyst prepared as follows. Anhydrous MgCli, phenyltriz toxicant at molar ratio Mg / Si. five equal to 6, and TiCl, taken in a molar ratio to phenyltriethoxysilane 1: 1, are crushed together in a vibrating mill having a total volume of 1 l and containing 3 kg of stainless steel balls with a diameter of 16 mm. Grinding is carried out using a filling factor of 100 g / l total volume (vacuum). - at a temperature inside the mill of 25 ° C and at a grinding time of 72 hours, The grinding of the mill with the material to be ground, the grinding process and the discharging of the jointly ground product from the mill is carried out in a nitrogen atmosphere. 100 g of co-milled product is contacted with 100 ml of 1,2-0 dichloroethane for 2 hours. After this period, 1,2-dichloroethane is removed by filtration at 80 ° C, the remaining solid product is again washed with n-heptane with at room temperature until the disappearance of chlorine ions from the filtrate, then, is kept in a heptane suspension. The catalyst components thus prepared show the X-ray spectrum of the powdered product, in which the diffraction line itself, found in the spectrum of MgClI, having a specific surface of 1 m / g, has a relatively low brightness and broadening to form a halo. Example 3. 62 g of MgCl and 12.5 g of TiCl are introduced into the mill and ground together for 60 hours at room temperature. The titanium content is 3.9 wt.%, 10 g of the co-milled product is contacted with 100 ml of 1,2-dichloroethane at 80 ° C for 2 hours. The solid product is recovered by filtration and then washed with heptane at the indicated temperature until the chlorine ions disappear from the filtrate. The x-ray spectrum is similar to the x-ray spectrum of the catalyst component according to example 1. The resulting solid catalyst component is used in the polymerization of propylene under polymerization conditions analogous to example 1. Example 4. 40 g of MgCl2 are ground in a mill for 200 hours at room temperature. 0 five five 0 five 10 g of the ground product is treated with 150 ml of TiCl2 for 2 hours at. After hot filtration, treatment with titanium tetrachloride is repeated. After washing with heptone and sugi, the dry solid is used under the same polymerization conditions as in Example 1. The solid component of the catalyst shows an x-ray spectrum of the powder product similar to that of the catalyst component of example 1. Example 5 (comparative). 200 mg of the solid component of catalyst prepared according to Example 4 is used in the polymerization process of propylene under the same conditions as in Example 1, but using ethyl p-toluate instead of phenyltristoxysilane. Example 6 (comparative). The process is carried out analogously to example 1, but using the solid component of catalyst corresponding to example 3, The results of the polymerization in examples 1-6 are presented in the table. Example 7 (known) 2.4 g of MgCl2 are dissolved in 17 g of titanate tetrabut-butylate (T1 (0-p-C4H, / 4) by stirring in a flask at 160 ° C under nitrogen atmosphere for 4 hours. The resulting solution is cooled to room temperature and diluted with 40 cm of anhydrous n-hexane. The resulting solution is cooled to 15 ° C, 40.9 g of -SiHCl is added to it, and 10 cm of anhydrous n-hexane is added over 4 hours with stirring. At the end of this addition, the temperature reaches 60 ° C, which is then maintained for another 1 hour. The solution is cooled to room temperature while precipitating out a precipitate, which is separated, washed repeatedly with anhydrous n-hexane and finally dried in vacuum at 70 ° C to constant weight. Thus obtained 3.6 g of gray powder containing 6.4 mg of titanium. Then, in a 2000 ml autoclave made of stainless steel, equipped with a magnetic stirrer and a thermometer, which is stably heated to boil and under the S78I3. 6 Serve under nitrogen, add 1.5 g of aluminum isobutyl and 20 mg of the indicated powder (solid component g of the catalyst), then propylene is added. After that, hydrogen is supplied at 0.1 atm, all heated to 70 ° C with a constant supply of propylene to create a total pressure of 7 atm. After 4 hours, the polymerization is interrupted, and 1.8 g of polypropylene is formed having I.I. 40 at the outlet of 90 g of polymer / g of catalyst component. 15 Example 8. When working in a nitrogen atmosphere, anhydrous magnesium chloride, diphenyldimethoxysilane. With a molar ratio of magnesium to silicon of 6, and TiCl, having a molecular ratio of titanium to silicon of 1, is crushed together in a vibratory mill, the total volume of which is 1 liter and which contains 4 kg of steel balls, diameter 25 of which is 16 mm by using a filling factor of 100 g / l full volume, at a temperature inside the mill of 7.5 ° C, for 72 hours. 30 10 g of the product obtained jointly} by grinding the product is brought into contact with 100 ml of 1,2-dichloroethane at 80 ° C for 2 hours. Then the solid product is filtered off at 80 ° C and washed with n-heptane at room temperature until the chlorine ions disappear, kept in suspension of heptane. The characteristics of this product, obtained in x40 Dk X-ray, are the same as those obtained with Example 2. The thus obtained solid component of the catalyst is used g for the polymerization of propylene with conditions analogous to example 1. The polymer yield is 7000 g of polymer / g of catalyst component; I.I. 96 Q Examples 9 and 10. Example B is repeated using chlorophenyldiethoxysilane (Example 9) and ethyltriethoxysilane (Example 10) as silicon compounds. The polymer codes are 4,000 and 5,000, respectively; I.I. equal to 90.5 and 90, respectively. Example 11. Anhydrous MgClI, Aenyltriethoxysilane in a molar ratio of 5 71 In a molar ratio of 1: 1 relative to phenyltriethoxysilane, Mg / Si 6 and TiC.4 are sieve ground in a vibrating crusher with a total volume of 1 l containing 3 kg of stainless steel balls with a waist of 16 mm in diameter, Grinding is carried out using a filling factor of 00 g / l total volume (vacuum), at an internal crusher temperature of 25 ° C and a grinding time of 72 hours. The crusher is loaded with substances that need to be crushed, and unloading from the crusher of the product takes place in a nitrogen atmosphere. 10 g of the co-milled product react with 100 ml of 1,2-dichloroethane at 80 ° C for 2 hours, After This, the 1,2-dichloroethane is removed by filtration and the remaining solid is re-washed with n-hexane at room temperature until the chlorine ions are removed from the filtrate and kept in a heptane suspension. The catalytic component thus obtained shows X-ray: the horse's powder spectrum, in which the most intense diffraction line in the MgGlj spectrum, having 1 mg of surface area, is increased in relative intensity and expanded to form halogen. In a steel stainless steel autoclave with a capacity of 2000 ml, equipped with a magnetic stirrer and a thermometer, at a set temperature and nitrogen atmosphere, 5 moles of aluminum triethyl, 1.5 moles of phenyltriethoxysilane, 42 mg of the described solid catalytic component, and propylene are charged. Then, 0.1 atm of hydrogen is loaded and another is propylene, so that the total pressure reaches 7 atm. This pressure is constantly maintained throughout the polymerization by introduction into the monomer. After 4 hours, the polymerization is stopped, the polymer is isolated by filtration and dried. The amount of polymer dissolved in the filtrate is isolated, weighed and added to a polymer that is soluble in boiling heptane to determine the isotactic index. The polymer obtained has I.I. 9 and the intrinsic viscosity determined in tetralin at 35 ° C; 38 1/1 dl / g. The yield is 6500 g / g of catalyst. Example 12. Example 11 is repeated, but the polymerization of propylene is carried out at (instead of 60 ° C) using triisobutylaluminum instead of Al () ,. The amount of catalytic component used is 45 mg. The polymer obtained has I.I. 96 and intrinsic viscosity, determined in tetralins at 35 ° C, 1.0 dl / g. The yield is 5,700 g / g of catalyst. Example 13. 20 mg of the catalytic component obtained in Example 11 and 50 ml of anhydrous deaerated n-heptane are introduced together with 5 mmol A1 (C, H5-) g and 1 mmol of phenyl triethoxysilane at a pressure of dry argon in a 2-liter autoclave stainless steel, equipped with a core-type stirrer heated to 70 ° C. and containing hydrogen for a partial pressure of 0.2 atm and 500 g of anhydrous propylene. After 4 hours, the reaction is stopped., The unpolymerized propylene is removed and the polymer is extracted from the autoclave, which is then dried and weighed. The polymer obtained has I.I. 96 and an intrinsic viscosity of 1.1 dg / g, determined in tetralin at 35 ° C. The yield is 18,500 g / g of catalyst. Example 14. Example 11 is repeated, but the polymerization of propylene is carried out at 60 ° C instead of 70 ° C using triisobutylaluminum instead of AlCCj Hj). The amount of the catalytic component used is 21 mg. The resulting polymer has I.I. 95 and an intrinsic viscosity of 1.0 dl / g, determined in tetralin at 35 ° C. The yield is 16,900 g / g of catalyst. Formula of invention A method of producing polypropylene by polymerizing polypropylene in an inert hydrocarbon solvent or liquid monomer at a temperature of 60-80 ° C and a pressure of 7 atm in the presence of a catalyst containing aluminum trialkyl, a silicon compound and a solid component. containing anhydrous magnesium dichloride coated with a titanium compound, or a solid component containing anhydrous magnesium dichloride coated with its titanium and silicon compounds, oj is different because in order to increase the yield of polypropylene having an increased isotacticity index, a catalyst is used containing as a trialkylaluminum compound selected from the group consisting of triethylaluminum, triisobutylaluminum. as a silicon compound, a compound selected from the group comprising phenyltriethoxysilane, diphenyldimethoxysilane, chlorophenyldiethoxysilane, methyltriethoxysilane, with a molar ratio of trialkylalumnium to a silicon compound equal to 1: 0.3; and if the silicon compound contains in the solid component, the molar ratio of the latter to the tet- titanium rachloride is 1; 1. ft
权利要求:
Claims (1) [1] 50 Formula of the invention A method of producing polypropylene by polymerizing polypropylene in an inert hydrocarbon solvent or liquid monomer at a temperature of 60-80 C and a pressure of 7 atm in the presence of a catalyst containing trialkylaluminum, a silicon compound and a solid component containing anhydrous magnesium dichloride coated with titanium compound, or solid a component containing anhydrous magnesium dichloride with titanium and silicon compounds deposited on its compounds, which is characterized by the fact that, in order to increase the quality of the silicon compound, the compound nenie selected from the group consisting of phenyltriethoxysilane, di- fenildimetoksisilan 5, hlorfenildietoksisipan, ethyltriethoxysilane, with a molar ratio of trialkyl aluminum to silicon compound of 1: 0.3, yield of polypropylene having a higher isotacticity index of the catalyst containing as trialkylaluminum compound selected from the group consisting of triethylaluminum, triisobutylaluminum. as the titanium compound, the solid component contains titanium tetrachloride and, if the solid component contains silicon, the molar ratio of the latter to titanium tetrachloride is 1: 1.
类似技术:
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同族专利:
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引用文献:
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申请号 | 申请日 | 专利标题 IT8024141A|IT1209255B|1980-08-13|1980-08-13|CATALYSTS FOR THE POLYMERIZATION OF OLEFINE.| 相关专利
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