HBPE (hyperbranched polyethylene) functionalized with terminal hydroxyl groups and preparation method thereof

A technology of hyperbranched polyethylene and functionalization, which is applied in the field of hyperbranched polyethylene functionalized with terminal hydroxyl groups and its preparation, can solve the problems of HBPE performance degradation, no practical value, low polymerization activity, etc., and achieve various performances and good practicality Value, high polymerization activity effect

Active Publication Date: 2015-09-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first method requires the use of noble metal palladium, the polymerization activity is very low, the synthesis cost is too high, and the polar groups are all at the end of the branch chain
The second method also uses the precious metal palladium, which has no practical value, and this method can only introduce chlorine atoms at the end of the chain of HBPE, and other polymer chains can only be introduced into HBPE through atom transfer radical polymerization and other methods.
The third method is complex, and in the graft modification process, it is often accompanied by many side reactions, such as chain scission reactions of polymer chains, resulting in a decrease in the performance of HBPE

Method used

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  • HBPE (hyperbranched polyethylene) functionalized with terminal hydroxyl groups and preparation method thereof
  • HBPE (hyperbranched polyethylene) functionalized with terminal hydroxyl groups and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Polymerization of ethylene under normal pressure is carried out under anhydrous and oxygen-free conditions. At 60°C and an ethylene pressure of 0.1 MPa, inject 40 mL of toluene into a 100 mL Schlenk bottle, and then inject 2.0 mmol of diethylaluminum chloride (control the Al / Ni ratio to 200) and 2.0 mmol of diethyl zinc (control Zn / Ni ratio is 200). Dissolve 10 μmol of procatalyst 4b (R is isopropyl) in 10 mL of toluene and inject it. The concentration of 4b in the polymerization system is 100 μmol / L. After half an hour of polymerization, feed oxygen into the polymer solution for oxidation, the reaction time is 2 hours, then reduce and precipitate with acidified ethanol, filter the polymer, wash with methanol or acetone several times, and dry in vacuum at 50°C After reaching a constant weight, 2.10 g of polymer was weighed. The catalyst activity is 0.54×10 6 g[mol(Ni)h] -1 , the number average molecular weight of the polymerization product is 4.5kg / mol, and the poly...

Embodiment 2

[0026] The cocatalyst monochlorodiethylaluminum was replaced by sesquiethylaluminum chloride, and other conditions and polymer treatment methods were the same as in Example 1 to obtain 2.60 grams of polymer. The catalyst activity is 0.67×10 6 g[mol(Ni)h] -1 , the number average molecular weight of the polymerization product is 3.5kg / mol, and the polydispersity coefficient is 1.51. 1 The degree of branching of the polymer was determined to be 125 / 1000 carbon atoms by H-NMR, and the glass transition temperature was -66°C. 93.72% of the polymer chains were terminated with hydroxyl groups.

Embodiment 3

[0028] The cocatalyst monochlorodiethylaluminum was replaced by dichloroethylaluminum, and other conditions and polymer treatment methods were the same as in Example 1 to obtain 2.24 grams of polymer. The catalyst activity is 0.58×10 6 g[mol(Ni)h] -1 , the number average molecular weight of the polymerization product is 4.0kg / mol, and the polydispersity coefficient is 1.53. 1 The degree of branching of the polymer as determined by H-NMR is 117 / 1000 carbon atoms, and the glass transition temperature is -65°C. 91.66% of the polymer chains were terminated with hydroxyl groups.

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Abstract

The invention relates to HBPE (hyperbranched polyethylene), and aims to provide HBPE functionalized with terminal hydroxyl groups and a preparation method thereof. According to the preparation of the HBPE functionalized with terminal hydroxyl groups, ethylidene acenaphthene (alpha-diimine) nickel catalyst is adopted as a main catalyst, aluminum alkyl is adopted as a cocatalyst, and diethyl zinc is adopted as a chain transfer agent; ethylene is catalyzed to be homopolymerized; the homopolymerized ethylene is subjected to ligand chain transfer polymerization to obtain diethyl zinc-terminated HBPE. The catalysts in the preparation require no precious metal, so that the synthesis cost of the HBPE is greatly reduced; diethyl zinc is adopted as the chain transfer agent, and the HBPE is prepared from the method of ligand chain transfer polymerization, so that the HBPE is high in polymerization activity and simple in technology; the method of obtaining terminal hydroxyl groups is simple and low in cost, and has good practical value; the hydroxyl in terminal hydroxyl groups HBPE is high in reaction activity, and a plurality of polymer chains with different properties can be introduced into the HBPE through condensation reaction, coupling reaction, click chemistry reaction, and the like, to prepare polymers with various properties and different functions.

Description

technical field [0001] The invention relates to hyperbranched polyethylene, in particular to a hyperbranched polyethylene functionalized with terminal hydroxyl groups and a preparation method thereof. Background technique [0002] Polyethylene (PE) is the variety with the largest output among general-purpose synthetic resins. It has high cost performance and is widely used in various fields such as industry and agriculture, medical and health care, scientific research and daily life. Polyethylene mainly includes high-density polyethylene (HDPE), low-density polyethylene (LDPE), linear low-density polyethylene (LLDPE) and some products with special properties. In 1995, the combination of (α-diimine) nickel / palladium late transition metal catalyst and MAO, discovered by Brookhart et al. in 1995, catalyzed the homopolymerization of ethylene. Depending on the ligand structure and polymerization conditions, hyperbranched polyethylene (HBPE) with different microstructures and pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F8/04C08F8/06C08F4/70
Inventor 傅智盛何峰范志强
Owner ZHEJIANG UNIV
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