Production of polypropylene with low volatiles

Patent metadata

Field	Value
Publication number	US-12509536-B2
Application number	US-202118001674-A
Country	US
Kind code	B2
Filing date	Jun 14, 2021
Priority date	Jun 15, 2020
Publication date	Dec 30, 2025
Grant date	Dec 30, 2025

Abstract

Process for producing a polypropylene comprising the steps of polymerizing the polypropylene in the presence of a metallocene catalyst, visbreaking said polypropylene and subsequently aerating the polypropylene at elevated temperature.

First claim

The invention claimed is:

1 . A process for producing polypropylene pellets comprising the steps in the following order:
(a) polymerizing propylene and optionally at least one α-olefin selected from ethylene, 1-butene and 1-hexene in the presence of a metallocene catalyst, obtaining thereby a polypropylene in the form of a powder, wherein the obtained polypropylene powder has a melt flow rate MFR 2 (230° C., 2.16 kg) measured according to ISO 1133 in the range of 1.0 to 100 g/10 min, (b) optionally mixing the polypropylene powder with additives, (c) visbreaking the polypropylene powder of step (a) or the mixture of step (b) with a visbreaking agent in a continuous melt-mixing device obtaining thereby a polypropylene in form of pellets, wherein the polypropylene pellets have a melt flow rate MFR 2 (230° C., 2.16 kg) measured according to ISO 1133 being higher than the melt flow rate MFR 2 (230° C., 2.16 kg) of the polypropylene powder of step (a), wherein further the visbreaking ratio (VR) is in the range of 2.0 to 25.0, wherein the visbreaking ratio (VR) is determined according to equation
VR=MFR 2(FINAL) /MFR 2(START)
wherein MFR 2(FINAL) is melt flow rate MFR 2 (230° C.; 2.16 kg) measured according to ISO 1133 of the polypropylene pellets after visbreaking, MFR 2(START) is melt flow rate MFR 2 (230° C.; 2.16 kg) measured according to ISO 1133 of the polypropylene powder before visbreaking, (d) aerating the polypropylene pellets of step (c) in an aeration vessel for 1 to 15 hours with an aeration gas having a temperature of at least 40° C. but lower than the heat deflection temperature (HDT) measured according to ISO 75 B method at a stress of 0.45 MPa of the polypropylene pellets of step (c), and (e) discharging the polypropylene pellets of step (d) from the aeration vessel.

2 . The process according to claim 1 , wherein the visbreaking agent is a peroxide or a hydroxylamine ester.

3 . The process according to claim 1 , wherein the metallocene catalyst has the formula (I):

wherein
M is Ti, Zr or Hf,
Z is an oxygen atom or a sulfur atom,
R 30 , R 31 , R 32 and R 33 may be the same or different and are a hydrogen atom, a halogen atom, an alkyl group having a carbon number of 1 to 6, an alkoxy group having a carbon number of 1 to 6, a halogen-containing alkyl group having a carbon number of 1 to 6, or an aryl group having a carbon number of 6 to 18,
Q is a carbon atom, a silicon atom or a germanium atom,
each of X 1 and X 2 is independently a halogen atom, an alkyl group having a carbon number of 1 to 6, an aryl group having a carbon number of 6 to 18, an amino group substituted with an alkyl group having a carbon number of 1 to 6, an alkoxy group having a carbon number of 1 to 6, a halogen-containing alkyl group having a carbon number of 1 to 6, or a halogen-containing aryl group having a carbon number of 6 to 18,
R 7 and R 17 may be the same or different and are a hydrogen atom, a halogen atom, an alkyl group having a carbon number of 1 to 6, an alkoxy group having a carbon number of 1 to 6, a halogen-containing alkyl group having a carbon number of 1 to 6, an aryl group having a carbon number of 6 to 18, or a halogen-containing aryl group having a carbon number of 6 to 18, and when either one of R 7 and R 17 is a hydrogen atom, the other is a substituent except for a hydrogen atom,
R 8 and R 18 may be the same or different and are a hydrogen atom, a halogen atom, an alkyl group having a carbon number of 1 to 6, an alkoxy group having a carbon number of 1 to 6, a halogen-containing alkyl group having a carbon number of 1 to 6, or a halogen-containing aryl group having a carbon number of 6 to 18,
R 2 , R 3 , R 4 , R 5 , R 6 , R 9 , R 12 , R 13 , R 14 , R 15 , R 16 and R 19 may be the same or different and are a hydrogen atom, a halogen atom, an alkyl group having a carbon number of 1 to 6, an alkoxy group having a carbon number of 1 to 6, a halogen-containing alkyl group having a carbon number of 1 to 6, an aryl group having a carbon number of 6 to 18, a halogen-containing aryl group having a carbon number of 6 to 18,
A is a divalent hydrocarbon group having a carbon number of 3 to 12 and forming a ring together with Q to which it is bonded, and may contain an unsaturated bond,
R 10 is a substituent on A and is an alkyl group having a carbon number of 1 to 6, a halogen containing alkyl group having a carbon number of 1 to 6, a trialkylsilyl group-containing alkyl group having a carbon number of 1 to 6, a silyl group containing a hydrocarbon group having a carbon number of 1 to 6, an aryl group having a carbon number of 6 to 18, or a halogen-containing aryl group having a carbon number of 6 to 18,
m represents an integer of 0 to 24, and when m is 2 or more, R 10 s may combine with each other to form a new ring structure.

4 . The process according to claim 1 , wherein the polymerization of step (a) takes place in two reactors connected in series.

5 . The process according to claim 1 , wherein in step (c) additionally additives are added into the continuous melt-mixing device.

6 . The process according to claim 1 , wherein step (b) is omitted.

7 . The process according to claim 1 , wherein polypropylene pellets after step (e) consist of:
(a) 95.0 to 99.95 wt. % of a polypropylene, and (b) 0.05 to 5.0 wt. % of additives, based on the total amount of the polypropylene pellets.

8 . The process according to claim 1 , wherein the polypropylene pellets after step (e) have a melt flow rate MFR 2 (230° C., 2.16 kg) measured according to ISO 1133 in the range of 40 to 1500 g/10 min.

9 . The process according to claim 1 , wherein:
(a) the polypropylene pellets have a molecular weight distribution (MWD) determined by gel permeation chromatography (GPC) in the range of 1.0 to below 3.2, and (b) the polypropylene of the polypropylene pellets has 2,1 regio-defects determined by 13 C-NMR spectroscopy in the range of 0.10 to 0.90%.

10 . The process according to claim 1 , wherein the polypropylene of the polypropylene pellets has a comonomer content of not more than 5.0 wt. %.

11 . The process according to claim 1 , wherein the polypropylene of the polypropylene pellets is a monophasic polypropylene.

12 . The process according to claim 11 , wherein the monophasic polypropylene is a propylene homopolymer.

13 . The process according to claim 1 , wherein the polypropylene powder has a molecular weight distribution (MWD) determined by gel permeation chromatography (GPC) in the range of 2.0 to below 4.0,
wherein further the ratio MWD (Start)/MWD (Final) is in the range of 1.01 to 2.50, wherein MWD (Start) is the molecular weight distribution (MWD) determined by gel permeation chromatography (GPC) of the polypropylene powder before visbreaking; MWD (Final) is the molecular weight distribution (MWD) determined by gel permeation chromatography (GPC) of the polypropylene pellets after visbreaking.

14 . The process according to claim 1 , wherein the polypropylene pellets after step (e) have a VOC (volatile organic compounds) value determined according to VDA 278 October 2011 in the range of 3.0 to 50 μg/g and a FOG (low volatility or condensable organic compounds) value determined according to VDA 278 October 2011 in the range of 10 to 80 μg/g.

15 . The process according to claim 1 , wherein the aeration gas is air.

16 . T

Assignees

• Borealis Ag

Inventors

• Wang Jingbo
• Gahleitner Markus
• Bernreitner Klaus
• Leskinen Pauli
• Grestenberger Georg
• Selvasankar Ramesh Kumar

Classifications

• C08J2323/26

  modified by chemical after-treatment · CPC title

• C08L23/10

  Homopolymers or copolymers of propene · CPC title

• C08F10/06

  Propene · CPC title

• C08K5/52

  Phosphorus bound to oxygen only · CPC title

• C08K5/098

  Metal salts of carboxylic acids · CPC title