Method for preparing polyolefin through metal-catalyzed ring-opening metathesis polymerization

A technology of ring-opening metathesis polymerization and metal catalysis, applied in chemical instruments and methods, chemical/physical processes, chemical/physical/physicochemical processes, etc., can solve the problems of poor controllability of the polymerization process, weakening Poiseuille flow, increasing Fluid turbulence and other problems can be achieved to reduce the molecular weight distribution index of the product, shorten the mixing time, and realize the effect of reaction time

Pending Publication Date: 2022-03-18
NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, spheres are placed in the microreactor as an internal component to increase the disturbance of the fluid, weaken th

Method used

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  • Method for preparing polyolefin through metal-catalyzed ring-opening metathesis polymerization
  • Method for preparing polyolefin through metal-catalyzed ring-opening metathesis polymerization
  • Method for preparing polyolefin through metal-catalyzed ring-opening metathesis polymerization

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Fill glass beads with a diameter of 2mm into a glass reaction tube with an inner diameter of 4.00mm, so that the retention volume is 4.00mL; use a microchannel tube with an inner diameter of 1mm and a length of 400mm to connect the syringe and the T-type mixer (the retention volume is 0.31 mL), the T-type mixer is connected to the microreactor of the internal member, and a microchannel tube with an inner diameter of 1 mm and a length of 636 mm is used to connect the receiving device (the retention volume is 0.5 mL). Flush the pipes with tetrahydrofuran solvent that has been re-evaporated and dried. Add 2.5mmol (235.4mg) norbornene and 10mL tetrahydrofuran to two 50mL Schlenk round-bottomed flasks after high-temperature baking to make monomer solution A; and 50μmol (42.44mg) Grubbs second-generation catalyst and 10mL tetrahydrofuran Catalyst solution B, after shaking and mixing, move it into two syringes A and B in the material sampling device respectively. Set the inje...

Embodiment 2

[0043]Fill the quartz beads with a diameter of 1mm into the PTFE reaction tube with an inner diameter of 4.00mm, so that the retention volume is 4.00mL; use a microchannel tube with an inner diameter of 1mm and a length of 400mm to connect the syringe and the T-type mixer (the retention volume is 0.31 mL), the T-type mixer is connected to the microreactor of the internal member, and a microchannel tube with an inner diameter of 1 mm and a length of 636 mm is used to connect the receiving device (the retention volume is 0.5 mL). Flush the pipes with tetrahydrofuran solvent that has been re-evaporated and dried. Add 2.5mmol (235.4mg) norbornene and 10mL tetrahydrofuran to two 50mL Schlenk round-bottomed flasks after high-temperature baking to make monomer solution A; and 50μmol (42.44mg) Grubbs second-generation catalyst and 10mL tetrahydrofuran Catalyst solution B, after shaking and mixing, move it into two syringes A and B in the material sampling device respectively. Set the...

Embodiment 3

[0045] Fill ceramic beads with a diameter of 1mm into a rubber reaction tube with an inner diameter of 4.00mm, so that the retention volume is 40.0mL; use a microchannel tube with an inner diameter of 1mm and a length of 400mm to connect the syringe and the T-type mixer (the retention volume is 0.31 mL), the T-type mixer is connected to the microreactor of the internal member, and a microchannel tube with an inner diameter of 1 mm and a length of 636 mm is used to connect the receiving device (the retention volume is 0.5 mL). Flush the pipes with tetrahydrofuran solvent that has been re-evaporated and dried. Add 12.5mmol (1177.0mg) norbornene and 50mL tetrahydrofuran into two 50mL Schlenk round-bottomed flasks after high-temperature baking respectively to make monomer solution A; Form catalyst solution B, shake and mix well, and then move into two syringes A and B in the material sampling device respectively. Set the injection flow rate of the sampling device A and B to 4mL / m...

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Abstract

The invention discloses a method for preparing polyolefin by metal-catalyzed ring-opening metathesis polymerization, which comprises the following steps: (1) dissolving norbornene monomers in a solvent to prepare a monomer solution A; (2) dissolving a Grubbs catalyst in a solvent to prepare a catalyst solution B; and (3) in a microchannel reaction device, simultaneously pumping the monomer solution A and the catalyst solution B into a microreactor provided with a spherical internal component, reacting, collecting a reaction solution, separating and purifying to obtain polyolefin. According to the invention, the sphere is placed in the microreactor as an internal component, so that Poiseuille flow in the pipeline is effectively improved, the mass and heat transfer efficiency is improved, the polymerization rate is increased, the space-time control of the reaction in the pipeline is enhanced, and the high-molecular-weight narrow-distribution polyolefin is efficiently prepared. Meanwhile, a brand new thought is provided for polymerization reaction process control, and the method has important industrial application value.

Description

technical field [0001] The invention belongs to the technical field of polyolefin preparation, in particular to a method for preparing polyolefin by metal-catalyzed ring-opening metathesis polymerization. Background technique [0002] When the traditional batch reactor conducts chemical reactions, there will be limitations in mass transfer, heat transfer and reaction control, and there are many shortcomings in itself, such as potential safety hazards, environmental pollution, huge energy consumption, large footprint and process scale-up Difficulty etc. Since the 1990s, academia began to apply microfluidic technology to the field of chemistry. The continuous flow micro-reaction has the advantages of precise temperature and time control, high-efficiency mass and heat transfer, safety and stability, and no amplification effect, which can well solve the problems existing in the traditional tank reaction. This new technology shows incomparable advantages over traditional batch ...

Claims

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Application Information

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IPC IPC(8): C08G61/02C08G61/12B01J19/00
CPCC08G61/08C08G61/124B01J19/0093C08G2261/11C08G2261/1426C08G2261/143C08G2261/1424C08G2261/3241C08G2261/3324C08G2261/418
Inventor 沈磊韩文鉴陈蕾蕾陈柯睿朱宁胡欣方正段金电刘一寰季栋李玉光乔凯李亚军张锴王美文郭凯
Owner NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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