Method for preparing polyolefin through coordination polymerization in micro-reactor

A technology of microreactor and coordination polymerization, which is applied in the field of polyolefins, can solve the problems of easy violent polymerization, failure to meet the gas-liquid phase coexistence requirements of olefin coordination polymerization, and difficult to achieve olefin polymerization, etc.

Active Publication Date: 2020-10-16
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] However, the design of the microfluidic system used in the above reaction method is simple, which cannot meet the complex gas-liquid phase coexistence requirements in the coordination polymerization of olefins, and cannot be applied to the environment of severe heat release, sudden polymerization, and high system pressure during the coordination polymerization process.
In addition, the existing technology is also difficult to achieve the specific process control of olefin polymerization for the specific residence time of the fluid in the microreactor pipeline (polymerization reaction time), unimodal or multimodal polymers, and polymers with different copolymerization compositions. need

Method used

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  • Method for preparing polyolefin through coordination polymerization in micro-reactor

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Experimental program
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Embodiment 1

[0075]In this embodiment, the first feed module 1 includes a filter 11, a mass flow meter 12 and a splitter 13, which are gas olefin monomer feed ports.

[0076] (1) Ethylene monomer enters the micro-reaction channel through the filter 11 and the mass flow meter 12 of the first feeding module 1; The high-pressure constant-flow pump enters the flow channel of the microreactor; the fluid B is composed of biscyclopentadienyl zirconium dichloride and xylene at a concentration of 2.31×10 -2 mg / mL mixed; the cocatalyst fluid C enters the microreactor flow channel through the high-pressure constant flow pump 21 of the second feed module 2 at a flow rate of 0.5mL / min; the fluid C is made of MAO and xylene at a concentration of 9.16mg / mL mixed;

[0077] (2) The material of the micro-reaction channel used is stainless steel. The tube length of a single main reaction module is 8m, the outer diameter is 3.18mm, and the inner diameter is 2mm; The time is about 30 minutes;

[0078] (3) C...

Embodiment 2

[0093] In this embodiment, the first feed module 1 includes a filter 11, a mass flow meter 12 and a splitter 13, which are gas olefin monomer feed ports.

[0094] (1) Propylene monomer enters the micro-reaction channel through the filter 11 and the mass flow meter 12 of the first feed module 1; the main catalyst fluid B passes through the high pressure of the third feed module 3 at a flow rate of 0.5mL / min The constant flow pump enters the flow channel of the microreactor; the fluid B is made of TiCl 4 / Dimethyl phthalate / MgCl 2 It is mixed with solvent white oil at a concentration of 1.25mg / mL; the cocatalyst fluid C enters the microreactor flow channel through the high-pressure constant-flow pump 21 of the second feed module 2 at a flow rate of 0.5mL / min; the fluid C It is composed of triethylaluminum, external electron donor cyclohexylmethyldimethoxysilane, and n-heptane at a concentration of 6.25mg / mL and 60mg / mL;

[0095] (2) The material of the micro-reaction flow chan...

Embodiment 3

[0100] In this embodiment, the first feed module 1 includes a filter 11, a mass flow meter 12 and a splitter 13, which are gas olefin monomer feed ports.

[0101] (1) Propylene monomer enters the micro-reaction channel through the filter 11 and the mass flow meter 12 of the first feed module 1; the main catalyst fluid B passes through the high pressure of the third feed module 3 at a flow rate of 0.5mL / min The constant flow pump enters the flow channel of the microreactor; the fluid B is made of TiCl 4 / fluorene diether / MgCl 2 Mixed with white oil with a concentration of 1.25mg / mL; the cocatalyst fluid C enters the microreactor flow channel through the high-pressure constant-flow pump 21 of the second feed module 2 at a flow rate of 0.5mL / min; the fluid C is obtained by Triethylaluminum and comonomer undecenyl alcohol are mixed with n-heptane at concentrations of 6.25mg / mL and 9.4mg / mL, respectively;

[0102] (2) The material of the micro-reaction flow channel used is stainl...

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Abstract

The invention belongs to the technical field of polyolefin, and particularly relates to a method for preparing polyolefin through coordination polymerization in a micro-reactor. The method includes: letting an olefin monomer fluid, a main catalyst fluid and a cocatalyst fluid respectively enter the micro-reactor through shunting runners; arranging a micro-reaction runner of the micro-reactor in aconstant-temperature box and carrying out polymerization reaction; and collecting the polymerization liquid to obtain the polymer. According to the preparation method, the monomer and the catalyst canbe quickly mixed, the uniformity of a local reaction environment is controlled, and the problem of polymerization reaction retention time in the prior art is solved; the prepared polymerization product realizes excellent polymer performance and realizes high flux of polymerization. The olefin monomer concentration of the main reaction runner can be timely and effectively regulated, and the molecular structure and molecular weight of the polymerization product can be controlled. The micro-reactor polymerization technology provided by the invention is low in equipment investment, small in device size and safer and more flexible to operate; and the method is suitable for continuous production, small in amplification effect and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of polyolefins, in particular to a method for preparing polyolefins by coordination polymerization in a microreactor. Background technique [0002] Polyolefins are made from very simple olefin monomers, which are not only cheap, but also have excellent properties such as low relative density, good chemical resistance, good water resistance, good mechanical strength, and good electrical insulation. Polyolefins are ubiquitous in our lives, and are widely used in films, pipes, sheets, wires and cables, packaging, electronics, electrical, automobiles, machinery, agriculture, medical and military affairs, etc. Since Ziegler and Natta won the Nobel Prize for their research on olefin coordination polymerization catalysts in 1963, the research on olefin polymerization has attracted great attention from academia and industry. In the past 50 years, the development of olefin polymerization has made commercial polyolef...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F110/06C08F210/06C08F216/04C08F110/14C08F210/14C08F212/08C08F4/642C08F4/646C08F4/645C08F2/01
CPCC08F2/01C08F110/02C08F110/06C08F110/14C08F210/06C08F210/14C08F4/642C08F4/6465C08F216/04C08F4/6457C08F212/08
Inventor 李化毅刘卫卫李倩胡友良
Owner INST OF CHEM CHINESE ACAD OF SCI
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