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Synthesis Method of Hyperbranched Polyolefin with controllable branched chain length and controllable branching degree

A synthesis method and technology of polyolefins, applied in the field of polyolefins, can solve the problems that cannot be used to synthesize hyperbranched polyolefins, and achieve the effect of good fluidity and low viscosity

Inactive Publication Date: 2020-02-18
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, although there have been reports in the literature on the synthesis of hyperbranched structures using olefin metathesis (J.Am.Chem.Soc., 2007, 129, 12672-12673), these methods can only be used to synthesize hyperbranched polyesters, Hyperbranched polymers such as polyether and other polymer chains containing heteroatoms such as oxygen, nitrogen, and phosphorus cannot be used to synthesize hyperbranched polyolefins containing only carbon and hydrogen.
The main difficulty in synthesizing hyperbranched polyolefins through olefin metathesis is that monomers containing multiple identical terminal olefins tend to form cross-linked structures during polymerization, so it is difficult to synthesize hyperbranched polyolefins without introducing heteroatom groups. react

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  • Synthesis Method of Hyperbranched Polyolefin with controllable branched chain length and controllable branching degree
  • Synthesis Method of Hyperbranched Polyolefin with controllable branched chain length and controllable branching degree
  • Synthesis Method of Hyperbranched Polyolefin with controllable branched chain length and controllable branching degree

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Embodiment 1

[0039] This embodiment relates to a method for synthesizing hyperbranched polyolefins with controllable branching chain length and controllable degree of branching. The synthetic route is as follows: figure 1 As shown, it specifically includes the following steps:

[0040] Under the protection of argon, add cuprous iodide (0.1g, 0.53mmol), bromoform (5g, 0.020mol), and tetrahydrofuran (50mL) into a 200mL reaction flask equipped with a magnetic stirrer, and slowly drip into it under an ice bath Allyl magnesium bromide solution (75 mL, 0.075 mol). After reacting for 3 hours, saturated ammonium chloride solution was added to terminate the reaction, then saturated brine was added, and the mixture was extracted three times with ether. The resulting solution was dried with anhydrous magnesium sulfate for 30 minutes and then concentrated by rotary evaporation to obtain a crude product. The crude product was purified by a silica gel column (mobile phase was n-hexane) to obtain a pure pr...

Embodiment 2

[0046] This embodiment relates to a method for synthesizing hyperbranched polyolefins with controllable branching chain length and controllable degree of branching. The synthetic route is as follows: figure 1 As shown, it specifically includes the following steps:

[0047] Under the protection of argon, add cuprous iodide (0.1g, 0.53mmol), bromoform (5g, 0.020mol), and tetrahydrofuran (50mL) into a 200mL reaction flask equipped with a magnetic stirrer, and slowly drip into it under an ice bath 1-Butene-4-magnesium bromide solution (200 mL, 0.075 mol). After reacting for 3 hours, saturated ammonium chloride solution was added to terminate the reaction, then saturated brine was added, and the mixture was extracted three times with ether. The resulting solution was dried with anhydrous magnesium sulfate for 30 minutes and then concentrated by rotary evaporation to obtain a crude product. The crude product was purified by silica gel column (mobile phase was n-hexane) to obtain pure ...

Embodiment 3

[0052] This embodiment relates to a method for synthesizing hyperbranched polyolefins with controllable branching chain length and controllable degree of branching. The synthetic route is as follows: figure 1 As shown, it specifically includes the following steps:

[0053] Under the protection of argon, add cuprous iodide (0.1g, 0.53mmol), bromoform (5g, 0.020mol), and tetrahydrofuran (50mL) into a 200mL reaction flask equipped with a magnetic stirrer, and slowly drip into it under an ice bath 1-Butene-4-magnesium bromide solution (200 mL, 0.075 mol). After reacting for 3 hours, saturated ammonium chloride solution was added to terminate the reaction, then saturated brine was added, and the mixture was extracted three times with ether. The resulting solution was dried with anhydrous magnesium sulfate for 30 minutes and then concentrated by rotary evaporation to obtain a crude product. The crude product was purified by silica gel column (mobile phase was n-hexane) to obtain pure ...

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Abstract

The invention provides a synthesis method of hyperbranched polyolefin with controllable branched chain length and controllable branching degree. The method omprises polymerizing a monomer having threeend-group olefins under the condition of a metal-organic catalyst, the monomer having three end-group olefins being represented by formula I, wherein n is an integer. According to the invention, by changing the structure of monomers, the types of catalysts, and the addition of other copolymers such as cis-cyclooctene, and changing the monomer concentration and reaction time can control the branched structure, branching degree, molecular weight and distribution of polyolefin products. Compared with the existing process, the invention adopts a kind of monomer with a brand-new structure and a polymerization process, and can synthesize hyperbranched polyolefin with accurate and controllable branched chain length. The polyolefin material prepared according to the invention has low viscosity, good fluidity, controllable branching degree and molecular weight, and can be widely applied to the fields of coatings, lubricants, polymer processing flow improvers, adhesives, curing agents and the like.

Description

Technical field [0001] The invention relates to the technical field of polyolefins, in particular to a method for synthesizing a type of hyperbranched polyolefins with controllable branching chain length and controllable branching degree. Background technique [0002] Polyolefin is currently one of the most widely used polymer materials in the world. Since the development of polymer science, the synthesis and application of polyolefins has always been a core issue in this field. In the past nearly a century, chemists have conducted in-depth research on the synthesis of polyolefins, but the controllable synthesis of hyperbranched polyolefins is still a challenging subject. In order to solve this problem, researchers proposed "Chain-Walking Polymerization" (CWP) in 1995, which uses a palladium catalyst to catalyze the polymerization of polyethylene to achieve the synthesis of hyperbranched polyolefins [Journal of the American Chemical Society 1995 117, 6414-6415]. At present, ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/22C08F216/12C08F232/04C07C1/32C07C11/21
CPCC07C1/326C08F236/22C08F216/12C08F232/04C07C11/21
Inventor 朱新远任宁童刚生
Owner SHANGHAI JIAO TONG UNIV
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