Catalyst system for polymerization of an olefin
09944731 ยท 2018-04-17
Assignee
Inventors
- Martin Alexander Zuideveld (Kelmis, BE)
- Aurora Alexandra Batinas-Geurts (BK Sittard, NL)
- Gennadii Dimitrievich Bukatov (Novosibirsk, RU)
- Sergei Andreevich Sergeev (Novosibirsk, RU)
- Vladimir Aleksandrovich Zakharov (Novosibirsk, RU)
Cpc classification
C08F4/6557
CHEMISTRY; METALLURGY
C08F4/6557
CHEMISTRY; METALLURGY
C08F2500/03
CHEMISTRY; METALLURGY
C08F4/651
CHEMISTRY; METALLURGY
C08F2500/03
CHEMISTRY; METALLURGY
C08F4/651
CHEMISTRY; METALLURGY
International classification
Abstract
A process for the preparation of a procatalyst suitable for preparing a catalyst composition for olefin polymerization, the procatalyst obtained or obtainable by the process; and a catalyst composition for olefin polymerization comprising the procatalyst. In particular a benzamide can be used as an activator in the preparation of a supported Ziegler-Natta type procatalyst useful for a process for the preparation of polyolefins. The Polyolefins and polypropylene homopolymers are also disclosed.
Claims
1. A process for the preparation of a procatalyst for preparing a catalyst composition for olefin polymerization, said process comprising: providing a magnesium-based support, contacting said magnesium-based support with a Ziegler-Natta type catalytic species, an internal donor, and an activator, to yield a procatalyst, wherein the activator is a benzamide according to formula X: ##STR00009## wherein R.sup.70 and R.sup.71 are each independently selected from hydrogen or an alkyl, and R.sup.72, R.sup.73, R.sup.74, R.sup.75, and R.sup.76 are each independently selected from hydrogen, a heteroatom or a hydrocarbyl group; and wherein the internal donor is selected from the group consisting of 1,3-diethers represented by the Formula VII, ##STR00010## wherein R.sup.51 and R.sup.52 are each independently selected from a hydrogen or a hydrocarbyl group selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups, and one or more combinations thereof and wherein R.sup.53 and R.sup.54 are each independently selected from a hydrocarbyl group.
2. The process according to claim 1, comprising: A) providing said procatalyst obtained via a process comprising: i) contacting a compound R.sub.z.sup.4MgX.sub.2-z.sup.4 with an alkoxy- or aryloxy-containing silane compound to give a first intermediate reaction product, being a solid Mg(OR.sup.1).sub.xX.sub.2-x.sup.1, wherein: R.sup.4 is the same as R.sup.1 being a linear, branched or cyclic hydrocarbyl group independently selected from alkyl, alkenyl, aryl, aralkyl or alkylaryl groups, and one or more combinations thereof; wherein said hydrocarbyl group is substituted or unsubstituted, optionally comprises one or more heteroatoms and has from 1 to 20 carbon atoms; X.sup.4 and X.sup.1 are each independently selected from fluoride (F.sup.), chloride (Cl.sup.), bromide (Br.sup.) or iodide (I.sup.); z is in a range of larger than 0 and smaller than 2, being 0<z<2; ii) contacting the solid Mg(OR.sup.1).sub.xX.sup.1.sub.2-x obtained in step i) with at least one activating compound of formula M.sup.1(OR.sup.2).sub.v-w(OR.sup.3)w or M.sub.2(OR.sup.2).sub.v-w(R.sup.3).sub.w, to obtain a second intermediate product; wherein: M.sup.1 is a metal selected from Ti, Zr, Hf, Al or Si; M.sup.2 is a metal being Si; v is the valency of M.sup.1 or M.sup.2; R.sup.2 and R.sup.3 are each a linear, branched or cyclic hydrocarbyl group independently selected from alkyl, alkenyl, aryl, aralkyl or alkylaryl groups, and one or more combinations thereof; wherein said hydrocarbyl group is substituted or unsubstituted, optionally comprises one or more heteroatoms, and has from 1 to 20 carbon atoms; and iii) contacting the first or second intermediate reaction product, obtained respectively in step i) or ii), with a halogen-containing Ti-compound, an activator according to Formula X and an internal electron donor according to Formula VII to obtain said procatalyst.
3. The process according to claim 1, wherein the hydrocarbyl groups R.sup.53 and R.sup.54 each have from 1 to 10 carbon atoms.
4. The process according to claim 1, wherein the internal donor is selected from the group consisting of 1,3-dimethoxypropane, 1,3-diethoxypropane, 1,3-dibutoxypropane, 1-methoxy-3-ethoxypropane, 1-methoxy-3-butoxypropane, 1-methoxy-3-cyclohexoxypropane, 2,2-dimethyl-1,3-dimethoxypropane, 2,2-diethyl-1,3-dimethoxypropane, 2,2-di-n-butyl-1,3-dimethoxypropane, 2,2-diisobutyl-1,3-dimethoxypropane, 2-ethyl-2-n-butyl-1,3-dimethoxypropane, 2-n-propyl-2-cyclopentyl-1,3-dimethoxypropane, 2,2-dimethyl-1,3-diethoxypropane, 2-n-propyl-2-cyclohexyl-1,3-diethoxypropane, 2-(2-ethylhexyl)-1,3-dimethoxypropane, 2-isopropyl-1,3-dimethoxypropane, 2-n-butyl-1,3-dimethoxypropane, 2-sec-butyl-1,3-dimethoxypropane, 2-cyclohexyl-1,3-dimethoxypropane, 2-phenyl-1,3-diethoxypropane, 2-cumyl-1,3-diethoxypropane, 2-(2-phenyllethyl)-1,3-dimethoxypropane, 2-(2-cyclohexylethyl)-1,3-dimethoxypropane, 2-(p-chlorophenyl)-1,3-dimethoxypropane, 2-(diphenylmethyl)-1,3-dimethoxypropane, 2-(1-naphthyl)-1,3-dimethoxypropane, 2-(fluorophenyl)-1,3-dimethoxypropane, 2-(1-decahydronaphthyl)-1,3-dimethoxypropane, 2-(p-t-butylphenyl)-1,3-dimethoxypropane, 2,2-dicyclohexyl-1,3-dimethoxypropane, 2,2-di-npropyl-1,3-dimethoxypropane, 2-methyl-2-n-propyl-1,3-dimethoxypropane, 2-methyl-2-benzyl-1,3-dimethoxypropane, 2-methyl-2-ethyl-1,3-dimethoxypropane, 2-methyl-2-phenyl-1,3-dimethoxypropane, 2-methyl-2-cyclohexyl-1,3-dimethoxypropane, 2,2-bis(pchlorophenyl)-1,3-dimethoxypropane, 2,2-bis(2-cyclohexylethyl)-1,3-dimethoxypropane, 2-methyl-2-isobutyl-1,3-dimethoxypropane, 2-methyl-2-(2-ethylhexyl)-1,3-dimethoxy propane, 2-methyl-2-isopropyl-1,3-dimethoxypropane, 2,2-diphenyl-1,3-dimethoxypropane, 2,2-dibenzyl-1,3-dimethoxypropane, 2,2-bis(cyclohexylmethyl)-1,3-dimethoxypropane, 2,2-diisobutyl-1,3-diethoxypropane, 2,2-diisobutyl-1,3-di-n-butoxypropane, 2-isobutyl-2-isopropyl-1,3-dimethoxypropane, 2,2-di-sec-butyl-1,3-dimethoxypropane, 2,2-di-t-butyl-1,3-dimethoxypropane, 2,2-dineopentyl-1,3-dimethoxypropane, 2-isopropyl-2-isopentyl-1,3-dimethoxypropane, 2-phenyl-2-benzyl-1,3-dimethoxypropane, 2-cyclohexyl-2-cyclohexylmethyl-1,3-dimethoxypropane, 2-isopropyl-2-(3,7-dimethyloctyl) 1,3-dimethoxypropane, 2,2-diisopropyl-1,3-dimethoxypropane, 2-isopropyl-2-cyclohexylmethyl-1,3-dimethoxypropane, 2,2-diisopentyl-1,3-dimethoxypropane, 2-isopropyl-2-cyclohexyl-1,3-dimethoxypropane, 2-isopropyl-2-cyclopentyl-1,3-dimethoxypropane, 2,2-dicylopentyl-1,3-dimethoxypropane, 2-n-heptyl-2-n-pentyl-1,3-dimethoxypropane, 9,9-bis(methoxymethyl)fluorene, 1,3-dicyclohexyl-2,2-bis(methoxymethyl)propane, 3,3-bis(methoxymethyl)-2,5-dimethylhexane, or any combination of the foregoing, for example wherein the internal donor is selected from the group of 1,3-dicyclohexyl-2,2-bis(methoxymethyl)propane, 3,3-bis(methoxymethyl)-2,5-dimethylhexane, 2,2-dicyclopentyl-1,3-dimethoxypropane and any combinations thereof.
5. The process according to claim 1, wherein the internal donor is 9,9-bis(methoxymethyl)fluorene.
6. The process according to claim 1, wherein in the activator according to Formula X, at least one of R.sup.70 and R.sup.71 is an alkyl group, wherein the alkyl has from 1 to 6 carbon atoms.
7. The process according to claim 1, wherein the activator is N,N-dimethylbenzamide.
8. The process according to claim 1, wherein the benzamide is present in the procatalyst, in an amount of from 0.1 to 4 wt. % as measured using HPLC.
9. A procatalyst obtained by the process according to claim 1.
10. A catalyst composition for olefin polymerization comprising a procatalyst comprising a benzamide according to formula X, ##STR00011## wherein R.sup.70 and R.sup.71 are each independently selected from hydrogen or an alkyl, and R.sup.72, R.sup.73, R.sup.74, R.sup.75, and R.sup.76 are each independently selected from hydrogen, a heteroatom or a hydrocarbyl group, and wherein the benzamide according to formula X is present in an amount of from 0.1 to 3.5 wt. %, based on the procatalyst as measured using HPLC; and further comprising an internal donor selected from 1,3-diethers represented by Formula VII ##STR00012## wherein R.sup.51 and R.sup.52 are each independently selected from a hydrogen or a hydrocarbyl group selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups, and one or more combinations thereof and wherein R.sup.53 and R.sup.54 are each independently selected from a hydrocarbyl group.
11. The catalyst composition of claim 10, wherein the catalyst is a supported Ziegler-Natta catalyst.
12. A process for the preparation of polyolefins, comprising contacting a procatalyst of claim 9 with at least one olefin, and optionally an external donor and/or optionally a co-catalyst.
13. The process of claim 1, wherein the hydrocarbyl groups R.sup.53 and R.sup.54 each have from 1 to 6 carbon atoms; and at least one of R.sup.70 and R.sup.71 is an alkyl group, wherein the alkyl has from 1 to 6 carbon atoms.
14. The process according to claim 4, wherein the activator is N,N-dimethylbenzamide.
15. The process according to claim 5, wherein the activator is N,N-dimethylbenzamide.
16. A procatalyst obtained by the process according to claim 15.
Description
EXAMPLES
Example 1
(1) A. Grignard Formation Step
(2) This step was carried out as described in Example XVI of EP 1 222 214 B1.
(3) A stainless steel reactor of 9 l volume was filled with 360 gram of magnesium powder. The reactor was brought under nitrogen. The magnesium was heated at 80 C. for 1 hour, after which a mixture of dibutyl ether (1 liter) and chlorobenzene (200 ml) was added. Then iodine (0.5 g) and n-chlorobutane (50 ml) were successively added to the reaction mixture. After the colour of the iodine had visually disappeared, the temperature was raised to 94 C. Then a mixture of dibutyl ether (1.6 liter) and chlorobenzene (400 ml) was slowly added for 1 hour, and then 4 liter of chlorobenzene was slowly added for 2.0 hours. The temperature of reaction mixture was kept in interval 98-105 C. The reaction mixture was stirred for another 6 hours at 97-102 C. Then the stirring and heating were stopped and the solid material was allowed to settle for 48 hours. By decanting the solution above the precipitate, a solution of phenylmagnesiumchloride reaction product A was obtained with a concentration of 1.3 mol Mg/l. This solution was used in the further catalyst preparation.
(4) B. Preparation of the First Intermediate Reaction Product
(5) This step was carried out as described in Example XX of EP 1 222 214 B1, except that the dosing temperature of the reactor was 35 C., the dosing time was 360 min and a propeller stirrer was used. 250 ml of dibutyl ether was introduced to a 1 liter reactor. The reactor was fitted by propeller stirrer and two baffles. The reactor was thermostated at 35 C.
(6) The solution of reaction product of step A (360 ml, 0.468 mol Mg) and 180 ml of a solution of tetraethoxysilane (TES) in dibutyl ether (DBE), (55 ml of TES and 125 ml of DBE), were cooled to 10 C., and then were dosed simultaneously to a mixing device of 0.45 ml volume supplied with a stirrer and jacket. From the mixing device, the mixed components were directly introduced into the reactor. The mixing device (minimixer) was cooled to 10 C. by means of cold water circulating in the minimixer's jacket. Dosing time was 360 min. The stirring speed in the minimixer was 1000 rpm. The stirring speed in the reactor was 350 rpm at the beginning of dosing and was gradually increased up to 600 rpm at the end of dosing stage.
(7) On the dosing completion the reaction mixture was heated up to 60 C. and kept at this temperature for 1 hour. Then the stirring was stopped and the solid substance was allowed to settle. The supernatant was removed by decanting. The solid substance was washed three times using 500 ml of heptane. As a result, a pale yellow solid substance, reaction product B (the solid first intermediate reaction product; the support), was obtained, suspended in 200 ml of heptane. The average particle size of support was 22 m and span value (d.sub.90d.sub.10)/d.sub.50=0.5.
(8) C. Preparation of the Second Intermediate Reaction Product
(9) Support activation was carried out as described in Example IV of WO/2007/134851 to obtain the second intermediate reaction product.
(10) under inert nitrogen atmosphere at 20 C. a 250 ml glass flask equipped with a mechanical agitator was filled with slurry of 5 g of reaction product B dispersed in 60 ml of heptane. Subsequently a solution of 0.22 ml ethanol (EtOH/Mg=0.1) in 20 ml heptane was dosed under stirring during 1 hour. After keeping the reaction mixture at 20 C. for 30 minutes, a solution of 0.79 ml titanium tetraethoxide (TET/Mg=0.1) in 20 ml of heptane was added for 1 hour.
(11) The slurry was slowly allowed to warm up to 30 C. for 90 min and kept at that temperature for another 2 hours. Finally the supernatant liquid was decanted from the solid reaction product (the second intermediate reaction product; activated support) which was washed once with 90 ml of heptane at 30 C.
(12) D. Preparation of the Catalyst Component
(13) A 500 mL reactor was brought under nitrogen and 62.5 ml of titanium tetrachloride was added to it. The reactor was heated to 100 C. and a suspension, containing about 5.5 g of activated support in 15 ml of heptane, was added to it under stirring. Then the reaction mixture was kept at 100 C. for 10 min, and 0.71 g of benzamide (BA-2H/Mg=0.15 molar ratio) in 2 ml of chlorobenzene was added to reactor. The reaction mixture was kept at 100 C. for 10 min, and 62.5 ml of chlorobenzene was added to reactor. The reaction mixture was kept at 100 C. for 30 min, and 1.0 g of 9,9-bis-methoxymethyl-9H-fluorene (flu/Mg=0.1 molar ratio) in 3 ml of chlorobenzene was added to reactor. Temperature of reaction mixture was increased to 115 C. and the reaction mixture was kept at 115 C. for 60 min (I stage of catalyst preparation). Then the stirring was stopped and the solid substance was allowed to settle. The supernatant was removed by decanting, after which the solid product was washed with chlorobenzene (125 ml) at 100-110 C. for 20 min. Then the washing solution was removed by decanting, after which a mixture of titanium tetrachloride (62.5 ml) and chlorobenzene (62.5 ml) was added. The reaction mixture was kept at 115 C. for 30 min (II stage of catalyst preparation), after which the solid substance was allowed to settle. The supernatant was removed by decanting, and the last treatment was repeated once again (III stage of catalyst preparation). The solid substance obtained was washed five times using 150 ml of heptane at 60 C., after which the catalyst component, suspended in heptane, was obtained.
(14) E. Polymerization of Propylene
(15) Polymerization of propylene was carried out in a stainless steel reactor (with a volume of 0.7 l) in heptane (300 ml) at a temperature of 70 C., total pressure 0.7 MPa and hydrogen presence (55 ml) for 1 hour in the presence of a catalyst system comprising the catalyst component according to step D, triethylaluminium and n-propyltrimethoxysilane. The concentration of the catalyst component was 0.033 g/l; the concentration of triethylaluminium was 4.0 mmol/l; the concentration of n-propyltrimethoxysilane was 0.2 mmol/l. Data on the catalyst performance at the propylene polymerization are presented in Table 1.
Example 1a
(16) Example 1a was carried out in the same way as Example 1, but in step E no n-propyltrimethoxysilane (nPTMS) was used.
Example 2
(17) Example 2 was carried out in the same way as Example 1, but N-methylbenzamide (BA-HMe/Mg=0.15 molar ratio) was used in step D instead of benzamide (BA-2H).
Example 2a
(18) Example 2a was carried out in the same way as Example 2, but in step E no nPTMS was used in step E.
Example 3
(19) Example 3 was carried out in the same way as Example 1, but N,N-dimethylbenzamide (BA-2Me/Mg=0.15 molar ratio) was used in step D instead of benzamide (BA-2H).
Example 3a
(20) Example 3a was carried out in the same way as Example 3, but no nPTMS was used in step E.
Example 4
(21) Example 4 was carried out in the same way as Example 1, but BA-2H/Mg=0.1 molar ratio was used in step D instead of BA-2H/Mg=0.15 molar ratio.
Example 4a
(22) Example 4a was carried out in the same way as Example 4, but no nPTMS was used in step E.
Example 5
(23) Example 5 was carried out in the same way as Example 2, but BA-HMe/Mg=0.1 molar ratio was used in step D instead of BA-HMe/Mg=0.15 molar ratio.
Example 5a
(24) Example 5a was carried out in the same way as Example 5, but no nPTMS was used in step E.
Example 6
(25) Example 6 was carried out in the same way as Example 2, but BA-HMe/Mg=0.25 molar ratio was used in step D instead of BA-HMe/Mg=0.15 molar ratio.
Example 6a
(26) Example 6a was carried out in the same way as Example 6, but no nPTMS was used in step E.
Example CE-A
Comparative Experiment A
(27) Example CE-A was carried out in the same way as Example 1, but ethylbenzoate (EB/Mg=0.15 molar ratio) was used in step D instead of benzamide.
Example CE-Aa
(28) Example CE-Aa was carried out in the same way as Example CE-A, but no nPTMS was used in step E.
Example CE-B
Comparative Experiment B
(29) Example CE-B was carried out in the same way as Example 1, but in step D only 9,9-bis-methoxymethyl-9H-fluorene (flu/Mg=0.15 molar ratio) without benzamide was used as follows. A reactor was brought under nitrogen and 125 ml of titanium tetrachloride was added to it. The reactor was heated to 100 C. and a suspension, containing about 5.5 g of activated support in 15 ml of heptane, was added to it under stirring. Then the temperature of reaction mixture was increased to 110 C. for 10 min and 1.5 g of 9,9-bis-methoxymethyl-9H-fluorene (flu) (flu/Mg=0.15 molar ratio) in 3 ml of chlorobenzene was added to reactor. Temperature of reaction mixture was increased to 115 C. and the reaction mixture was kept at 115 C. for 105 min (I stage of catalyst preparation). Then the stirring was stopped and the solid substance was allowed to settle. The supernatant was removed by decanting, after which the solid product was washed with chlorobenzene (125 ml) at 100-110 C. for 20 min. Then the washing solution was removed by decanting, after which a mixture of titanium tetrachloride (62.5 ml) and chlorobenzene (62.5 ml) was added. The reaction mixture was kept at 115 C. for 30 min (II stage of catalyst preparation), after which the solid substance was allowed to settle. The supernatant was removed by decanting, and the last treatment was repeated once again (III stage of catalyst preparation). The solid substance obtained was washed five times using 150 ml of heptane at 60 C., after which the catalyst component, suspended in heptane, was obtained.
Example CE-Ba
(30) Example CE-Ba was carried out in the same way as Example CE-B, but no nPTMS was used in step E.
Example CE-C
Comparative Experiment C
(31) Example CE-C was carried out in the same way as Example CE-B, but di-n-butylphthalate (DBP) at DBP/Mg=0.15 molar ratio was used in step D instead of flu/Mg=0.15.
Example CE-D
Comparative Experiment D
(32) Example CE-D was carried out in the same way as Example CE-A, but DBP/Mg=0.1 molar ratio was used in step D instead of flu/Mg=0.1 molar ratio.
Example CE-E
Comparative Experiment E
(33) Example CE-E was carried out in the same way as Example CE-A, but in step D ethylbenzoate (EB/Mg=0.15 molar ratio) at I stage and di-n-butylphthalate (DBP/Mg=0.05 molar ratio) at III stage were used as follows.
(34) A reactor was brought under nitrogen and 125 ml of titanium tetrachloride was added to it. The reactor was heated to 100 C. and a suspension, containing about 5.5 g of activated support in 15 ml of heptane, was added to it under stirring. The reaction mixture was kept at 100 C. for 10 min. Then add 0.886 g of ethyl benzoate (EB/Mg=0.15 molar ratio). The reaction mixture was kept for 60 min (I stage of catalyst preparation). Then the stirring was stopped and the solid substance was allowed to settle. The supernatant was removed by decanting, after which the solid product was washed with chlorobenzene (125 ml) at 100 C. for 20 min. Then the washing solution was removed by decanting, after which a mixture of titanium tetrachloride (62.5 ml) and chlorobenzene (62.5 ml) was added. The reaction mixture was kept at 100 C. for 30 min (II stage of catalyst preparation). After which the stirring was stopped and the solid substance was allowed to settle. The supernatant was removed by decanting, after which a mixture of titanium tetrachloride (62.5 ml) and chlorobenzene (62.5 ml) was added. Then di-n-butylphthalate (DBP) at DBP/Mg=0.05 molar ratio) in 2 ml of chlorobenzene was added to reactor and the temperature of reaction mixture was increased to 115 C. The reaction mixture was kept at 115 C. for 30 min (III stage of catalyst preparation). After which the stirring was stopped and the solid substance was allowed to settle. The supernatant was removed by decanting, after which a mixture of titanium tetrachloride (62.5 ml) and chlorobenzene (62.5 ml) was added. The reaction mixture was kept at 115 C. for 30 min (IV stage of catalyst preparation), after which the solid substance was allowed to settle. The supernatant was removed by decanting and the solid was washed five times using 150 ml of heptane at 60 C., after which the catalyst component, suspended in heptane, was obtained.
(35) Table 1 and 2 show the test results, wherein the first column discloses the example labels The second column discloses during which stage the activator is added and the type of activator used. The third column discloses the molar ratio of the activator (BA) over the magnesium in the support (Mg). The fourth column discloses the molar ratio of the internal donor over the magnesium in the support (Mg) and the type of internal donor. The fifth, sixth and seventh column disclose the amount of internal donor, activator and titanium in wt. % with respect to the total weight of the catalyst composition. The eighth column discloses the yield of polypropylene in kg/g catalyst. The ninth column discloses the amount of atactic PP (APP) in wt. % with respect to the total weight of the polymer obtained. The tenth column discloses the amount of soluble xylene (XS) in wt. %.
(36) Abbreviations and measuring methods: PP yield, kg/g cat is the amount of polypropylene obtained per gram of catalyst component; the unit of MFR is g/10 min.
(37) Analysis of Internal Donors and Activating Compounds in TiNo Procatalyst by HPLC
(38) Extract the catalyst sample (0.1-0.2 g) with 10 ml of acetonitrile in capped flask by stirring for 1 h with a magnetic stirrer. Filter the extract via a single use syringe filter Minisart SRP 15 with PTFE-membrane (pore size of 0.45 micron).
(39) Analyze the solution byH PLC using a reverse phase C18 column (Shimadzu Pathfinder C18 column, 4.650 mm, 2.5 m particle size, 100 Angstroem pore size) and isocratic mobile phase (acetonitrile/water of 85/15 vol./vol.). The column temperature is 40 C. A UV detector (single wavelength of 254 nm) is used for detection. Injection volume is 5 l. All injections are made twice.
(40) Standard solution for calibration: 0.02-0.03 g of internal donor or activating compound in 10 ml of acetonitrile analyzed under the same conditions as the catalyst sample. Calculate the content of dibutyl phthalate as:
(41) Internal donor/activating compound content
(42)
where
(43) Saverage peak area of the sample;
(44) Sstandardaverage peak area of the standard sample;
(45) Wstandardweight of the standard sample, g;
(46) Gcatalyst weight, g.
(47) ICP-AES Measurement of Procatalyst
(48) A small amount amount of procatalyst sample was contacted for 30 minutes with a H.sub.2SO.sub.4HNO.sub.3 solution to ensure a complete reaction of the procatalyst. After that, the solution of H.sub.2SO.sub.4HNO.sub.3/procatalyst reaction products was measured by means of ICP-AES, using a ThermoFisher Scientific, iCAP6500. Ti and Mg content in wt. % of total procatalyst weight is reported.
(49) TABLE-US-00001 TABLE 1 BA/ PP Ex. ID Mg ID/Mg ID BA Ti yield APP XS MFR M.sub.w/M.sub.n 1 BA-2H 0.15 0.1 9.2 4 3.0 8.5 0.8 2.7 15.5 4.3 flu 2 BA-HMe 0.15 0.1 11.6 1.6 3.0 13.1 0.65 2.1 14.7 4.3 flu 3 BA-2Me 0.15 0.1 11.7 2.2 4.6 13.4 0.6 2.2 17.2 3.9 flu 4 BA-2H 0.1 0.1 11.7 2.3 3.2 9.8 0.55 3.7 14.4 4.3 flu 5 BA-HMe 0.1 0.1 12.9 1.8 3.2 11.1 0.6 2.2 17.7 4.5 flu 6 BA-HMe 0.25 0.1 10.7 1.9 2.7 10.9 0.6 2.5 17 4.3 flu CE-A EB 0.15 0.1 13.5 3.3 2.9 16.5 0.35 2.6 14.4 5.1 flu EB CE-B 0.15 16.5 3.4 9.2 0.8 3.5 10.7 5.1 flu CE-C 0.15 10.5 2.6 13.5 0.5 3.0 12.7 4.8 DBP CE-D EB 0.15 0.1 7.3 2.3 2.8 11.1 1.0 5.4 18.4 5.6 DBP EB CE-E EB 0.15 0.05 9.2 0.7 2.3 11.3 0.6 4.0 15.8 5.0 DBP EB
(50) TABLE-US-00002 TABLE 2 Ex. stage BA/Mg ID/Mg ID BA Ti PP yield APP XS MFR M.sub.w/M.sub.n 1a BA-2H 0.15 0.1 9.2 4 3.0 13.5 1.1 4.2 25 4.9 flu 2a BA-HMe 0.15 0.1 11.6 1.6 3.0 15.4 1.0 4.2 22 4.1 flu 3a BA-2Me 0.15 0.1 11.7 2.2 4.6 14.9 0.8 3.4 23 4.6 flu 4a BA-2H 0.1 0.1 11.7 2.3 3.2 13.2 0.8 4.1 25 4.8 flu 5a BA-HMe 0.1 0.1 12.9 1.8 3.2 16.0 0.6 3.9 19 4.4 flu 6a BA-HMe 0.25 0.1 10.7 1.9 2.7 13.8 0.9 4.3 25 4.4 flu CE-Aa EB 0.15 0.1 13.5 3.3 2.9 25.0 1.0 5.8 49.5 4.3 flu EB CE-Ba 0.15 16.5 3.4 13.5 1.2 4.3 21.8 4.6 flu
(51) Table 1 shows that the catalyst component according to the present invention, i.e. comprising a benzamide of formula X and an internal donor selected from the group consisting of 1,3-diethers represented by the Formula VII allows obtaining polypropylenes having narrow molecular weight distribution, low XS and APP content at relatively high MFR values, for instance it is possible to obtain a polypropylene homopolymer having
(52) a molecular weight distribution (M.sub.w/M.sub.n) below 5.0, for example below 4.5, preferably from 2 to 4.5, more preferably from 3 to 4.5, more preferably from 3.5 to 4.5
(53) a melt flow rate of above 14, for example in the range from 14 to 1000,
(54) a weight percentage of atactic polypropylene (APP) of less than 1.5, preferably less than 1.0
(55) a xylene soluble content (XS) of less than 4.5 wt. %.