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Preparation method for multiphase polyolefin

A technology of polyolefins and olefins, which is applied in the field of preparation of polyolefins and polymers. It can solve the problems of particle adhesion, affecting the stable and safe operation of the device, and difficulty in taking into account rigidity and toughness at the same time, so as to avoid particle stickiness, good fluidity, and high Effect of stiffness-toughness balance properties

Inactive Publication Date: 2013-10-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing heterogeneous polyolefins, which overcomes the difficulty of simultaneously taking into account the rigidity and toughness of heterogeneous polyolefins prepared by conventional multi-stage polymerization processes, and also solves the problem of using continuous copolymerization to prepare heterogeneous polyolefins with high ethylene-propylene rubber content. Problems such as sticking, agglomeration, and sticking to the kettle that affect the smooth and safe operation of the device

Method used

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  • Preparation method for multiphase polyolefin

Examples

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Effect test

Embodiment 1

[0047] The preparation of embodiment 1 spherical polypropylene particle matrix

[0048] (1) Prepolymerization

[0049] A Propylene prepolymerization

[0050] Before the experiment, the reactor was replaced with nitrogen at least three times, and vacuum-dried at 100 °C for 2 h, and then filled with propylene gas to make the pressure slightly higher than normal pressure, while the temperature dropped to 20 °C. Add n-heptane successively, cocatalyst Al(C 2 h 5 ) 3 , external electron donor (C 6 h 5 ) 2 Si(OCH 3 ) 2 , and 0.05g of the main catalyst. The molar ratio of aluminum in the cocatalyst to titanium in the main catalyst is 100, and the molar ratio of the external electron donor to titanium is 5. The main components of the main catalyst are: TiCl 4 , MgCl 2 , and diisobutyl phthalate, which are spherical particles with a particle size of 20-150 microns, and their titanium content is 1.5-3.0% (wt). The reaction conditions for the prepolymerization are: pressure 0...

Embodiment 2

[0057] The preparation of embodiment 2 spherical polypropylene particle matrix

[0058] Prepolymerization was carried out in the same operating process and reaction conditions as in the step A propylene prepolymerization of Example 1.

[0059] After the pre-polymerization of propylene was completed, the propylene gas was filled to 0.6 MPa, the temperature was raised to 60° C., and the reaction was terminated after stirring for 0.5 hours to obtain 50 g of the product. The obtained polypropylene is regular spherical particles with an average particle diameter of 0.5mm.

Embodiment 3

[0060] The preparation of embodiment 3 heterophasic polyolefins

[0061] Prepolymerization and main polymerization were carried out in the same operating process and reaction conditions as the propylene prepolymerization in Step A of Example 1.

[0062] After the main polymerization of propylene was terminated for 1 hour, the pressure in the kettle was reduced to -0.09 MPa (gauge pressure), and the solvent was extracted under reduced pressure and maintained for 10 minutes. Set the main polymerization time of propylene to 15 minutes and the copolymerization time of ethylene-propylene to 5 minutes respectively through the control cabinet, and set the main polymerization of propylene first. Open the inlet valve at the bottom of the tank, ASPP starts: propylene gas (hydrogen gas mole percentage is 1%) is continuously fed from the bottom of the reactor through one of the valves, and unreacted monomers are continuously discharged through the tail gas valve to keep the pressure in th...

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Abstract

The invention discloses a preparation method for a multiphase polyolefin, belongs to the field of macromolecule, and specifically relates to the field of polyolefin preparation. The preparation method for a multiphase polyolefin comprises the following steps: (1) preparation of a polyolefin particle matrix; and (2) atmosphere switching polymerization process (ASPP). The preparation method helps to realize minute-grade continuous switching between two or among more than two different atmospheres, and realize that the gas continuously enters into or is expelled from a reactor, thereby operation is simplified and the method is beneficial to continuous industrial process; in the method, the content of an in-situ compatilizer ethylene-propylene block polymer is increased, thus the compatibility of two phases is effectively increased, and the prepared impact polypropylene copolymer has higher rigid-tough balance performance; the method helps to effectively avoid the phenomenon of tacky particles during continuous ethylene propylene copolymerization, and is helpful for continuous stable production in industrialized apparatuses; and the method helps to prepare the wide-range polyolefin material with regular spherical particles, and the bonding phenomena among particles and kettles cannot be generated.

Description

Technical field: [0001] The invention belongs to the field of macromolecules, and specifically relates to the field of preparing polyolefins. Background technique [0002] Polypropylene is one of the most widely used synthetic resins. It has the advantages of high tensile strength and good heat resistance, but it has poor cold resistance and insufficient low temperature toughness. In order to toughen polypropylene, since the 1990s, some companies have used a multi-stage polymerization process to synthesize heterogeneous polyolefins based on high-efficiency spherical supported Ziegler-Natta catalysts. The production cost is low and the performance is better than conventional mechanical blending methods. At present, the representative technologies of heterogeneous polyolefins are: Spheripol and Catalloy of Basell Company (US4521566; DE430429). The polymerization process includes three to four stages of sequentially connected polymerization reaction stages, namely, propylene p...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F10/06C08F10/08C08F10/14C08F110/06C08F210/16C08F293/00C08F2/34C08L23/12C08L23/16C08L53/00
Inventor 冯连芳田洲胡庆云顾雪萍范志强梅利笪文忠
Owner CHINA PETROLEUM & CHEM CORP
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